Determination of platinum-group elements in the geological standard reference materials by isotope dilution-ICPMS

Energy Technology Data Exchange (ETDEWEB)

Mingyue, Hu; Hongliao, He [National Research Center for Geoanalysis, Beijing (China)

2005-10-15

Platinum group elements (PGEs) includes platinum, palladium, iridium, osmium, rhodium and ruthenium. It has very high economic and scientific value in the field of geoscience and environmental science. But the analysis data referred by the different lab are very disperse because of the difficulty of the determination of PGEs. It makes very difficult to fix the value of the PGEs in the standard reference materials. In the article, the values of the PGEs in the standard reference materials of ocean sediment are determined by isotope dilution technique and dependable values of these elements are provided. (authors)

Determination of platinum-group elements in the geological standard reference materials by isotope dilution-ICPMS

International Nuclear Information System (INIS)

Hu Mingyue; He Hongliao

2005-01-01

Platinum group elements (PGEs) includes platinum, palladium, iridium, osmium, rhodium and ruthenium. It has very high economic and scientific value in the field of geoscience and environmental science. But the analysis data referred by the different lab are very disperse because of the difficulty of the determination of PGEs. It makes very difficult to fix the value of the PGEs in the standard reference materials. In the article, the values of the PGEs in the standard reference materials of ocean sediment are determined by isotope dilution technique and dependable values of these elements are provided. (authors)

Survey of reference materials. V. 2: Environmentally related reference materials for trace elements, nuclides and microcontaminants

International Nuclear Information System (INIS)

1996-05-01

The present report presently contains over 250 reference materials with trace element and organic contaminant information on fuel, geological and mineral, anthropogenic disposal, soil reference and miscellaneous reference materials. Not included in the current report is information on most biological and environmental reference materials with trace element, stable isotope, radioisotope and organic contaminant information. 8 refs, tabs

New Organic Stable Isotope Reference Materials for Distribution through the USGS and the IAEA

Science.gov (United States)

Schimmelmann, Arndt; Qi, Haiping

2014-05-01

The widespread adoption of relative stable isotope-ratio measurements in organic matter by diverse scientific disciplines is at odds with the dearth of international organic stable isotopic reference materials (RMs). Only two of the few carbon (C) and nitrogen (N) organic RMs, namely L-glutamic acids USGS40 and USGS41 [1], both available from the U.S. Geological Survey (USGS) and the International Atomic Energy Agency (IAEA), provide an isotopically contrasting pair of organic RMs to enable essential 2-point calibrations for δ-scale normalization [2, 3]. The supply of hydrogen (H) organic RMs is even more limited. Numerous stable isotope laboratories have resorted to questionable practices, for example by using 'CO2, N2, and H2 reference gas pulses' for isotopic calibrations, which violates the principle of identical treatment of sample and standard (i.e., organic unknowns should be calibrated directly against chemically similar organic RMs) [4], or by using only 1 anchor instead of 2 for scale calibration. The absence of international organic RMs frequently serves as an excuse for indefensible calibrations. In 2011, the U.S. National Science Foundation (NSF) funded an initiative of 10 laboratories from 7 countries to jointly develop much needed new organic RMs for future distribution by the USGS and the IAEA. The selection of targeted RMs attempts to cover various common compound classes of broad technical and scientific interest. We had to accept compromises to approach the ideal of high chemical stability, lack of toxicity, and low price of raw materials. Hazardous gases and flammable liquids were avoided in order to facilitate international shipping of future RMs. With the exception of polyethylene and vacuum pump oil, all organic RMs are individual, chemically-pure substances, which can be used for compound-specific isotopic measurements in conjunction with liquid and gas chromatographic interfaces. The compounds listed below are under isotopic calibration by

An inter-laboratory comparison of Si isotope reference materials

NARCIS (Netherlands)

Reynolds, B.C.; Aggarwal, J.; André, L.; Baxter, B.; Beucher, C.; Brzezinski, M.A.; Engström, E.; Georg, R.B.; Land, M.; Leng, M.J.; Opfergelt, S.; Rodushkin, I.; Sloane, H.J.; Van den Boorn, S.H.J.M.; Vroon, P.Z.; Cardinal, D.

2007-01-01

Three Si isotope materials have been used for an inter-laboratory comparison exercise to ensure reproducibility between international laboratories investigating natural Si isotope variations using a variety of chemical preparation methods and mass spectrometric techniques. These proposed standard

Determination of molybdenum in plant reference material by thermal-ionization isotope-dilution mass spectrometry

International Nuclear Information System (INIS)

Saumer, M.; Gantner, E.; Reinhardt, J.; Ache, H.J.

1992-01-01

An analytical method is described for the determination of the concentration and the isotopic composition of molybdenum in plant samples using thermal ionization mass spectrometry. After microwave acid digestion and liquid-liquid extractive separation with Amberlite LA-2, the molybdenum isotopes are measured as MoO 3 - -ions in a quadrupole mass spectrometer. In all cases, the relative standard deviation of the measurements of both natural and spike molybdenum was better than 3% for all ratios measured. The concentration of molybdenum found in three different plant reference materials agreed well with the certified values. (orig.)

Lead isotopic compositions of environmental certified reference materials for an inter-laboratory comparison of lead isotope analysis

International Nuclear Information System (INIS)

Aung, Nyein Nyein; Uryu, Tsutomu; Yoshinaga, Jun

2004-01-01

Lead isotope ratios, viz. 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, of the commercially available certified reference materials (CRMs) issued in Japan are presented with an objective to provide a data set, which will be useful for the quality assurance of analytical procedures, instrumental performance and method validation of the laboratories involved in environmental lead isotope ratio analysis. The analytical method used in the present study was inductively coupled plasma quadrupole mass spectrometry (ICPQMS) presented by acid digestion and with/without chemical separation of lead from the matrix. The precision of the measurements in terms of the relative standard deviation (RSD) of triplicated analyses was 0.19% and 0.14%, for 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, respectively. The trueness of lead isotope ratio measurements of the present study was tested with a few CRMs, which have been analyzed by other analytical methods and reported in various literature. The lead isotopic ratios of 18 environmental matrix CRMs (including 6 CRMs analyzed for our method validation) are presented and the distribution of their ratios is briefly discussed. (author)

IAEA biological reference materials

International Nuclear Information System (INIS)

Parr, R.M.; Schelenz, R.; Ballestra, S.

1988-01-01

The Analytical Quality Control Services programme of the IAEA encompasses a wide variety of intercomparisons and reference materials. This paper reviews only those aspects of the subject having to do with biological reference materials. The 1988 programme foresees 13 new intercomparison exercises, one for major, minor and trace elements, five for radionuclides, and seven for stable isotopes. Twenty-two natural matrix biological reference materials are available: twelve for major, minor and trace elements, six for radionuclides, and four for chlorinated hydrocarbons. Seven new intercomparisons and reference materials are in preparation or under active consideration. Guidelines on the correct use of reference materials are being prepared for publication in 1989 in consultation with other major international producers and users of biological reference materials. The IAEA database on available reference materials is being updated and expanded in scope, and a new publication is planned for 1989. (orig.)

AQCS 1990. Intercomparison runs, reference materials

International Nuclear Information System (INIS)

1990-01-01

The purpose of the Analytical Quality Control Services (AQCS) programme provided by the International Atomic Energy Agency (Agency) is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. Such a control is necessary since results of analytical activities may be the basis upon which economic, administrative, medical or legal decisions are taken; they must, therefore, be documented to be sufficiently reliable. The Agency has instituted the AQCS-programme which for 1990 will involve distributing samples for Intercomparison Runs and Reference Materials in a way similar to that of previous years. The Agency's Analytical Quality Control Services (AQCS) programme provides mainly three types of materials: materials which can be used in analytical laboratories working in the fields of nuclear technology and isotope hydrology. These include uranium ore Reference Materials and other substances of interest for nuclear fuel technology as well as stable isotope Reference Materials for mass spectrometric determination of isotope ratios in natural waters; materials with known content of uranium, thorium and/or transuranium elements or fission products for the determination of environmental radioactivity or control of nuclear safety; materials for use in the determination of stable trace elements in environmental, biomedical and marine research. Radiochemical methods such as neutron activation or isotope dilution analysis are often used in the determination of such trace elements and constitute an important contribution of nuclear techniques to applied science. Tabs

Certified reference materials and reference methods for nuclear safeguards and security.

Science.gov (United States)

Jakopič, R; Sturm, M; Kraiem, M; Richter, S; Aregbe, Y

2013-11-01

Confidence in comparability and reliability of measurement results in nuclear material and environmental sample analysis are established via certified reference materials (CRMs), reference measurements, and inter-laboratory comparisons (ILCs). Increased needs for quality control tools in proliferation resistance, environmental sample analysis, development of measurement capabilities over the years and progress in modern analytical techniques are the main reasons for the development of new reference materials and reference methods for nuclear safeguards and security. The Institute for Reference Materials and Measurements (IRMM) prepares and certifices large quantities of the so-called "large-sized dried" (LSD) spikes for accurate measurement of the uranium and plutonium content in dissolved nuclear fuel solutions by isotope dilution mass spectrometry (IDMS) and also develops particle reference materials applied for the detection of nuclear signatures in environmental samples. IRMM is currently replacing some of its exhausted stocks of CRMs with new ones whose specifications are up-to-date and tailored for the demands of modern analytical techniques. Some of the existing materials will be re-measured to improve the uncertainties associated with their certified values, and to enable laboratories to reduce their combined measurement uncertainty. Safeguards involve the quantitative verification by independent measurements so that no nuclear material is diverted from its intended peaceful use. Safeguards authorities pay particular attention to plutonium and the uranium isotope (235)U, indicating the so-called 'enrichment', in nuclear material and in environmental samples. In addition to the verification of the major ratios, n((235)U)/n((238)U) and n((240)Pu)/n((239)Pu), the minor ratios of the less abundant uranium and plutonium isotopes contain valuable information about the origin and the 'history' of material used for commercial or possibly clandestine purposes, and

Lead Isotopic Composition in Biogenic Certified Reference Materials Determined by Different ICP-based Mass Spectrometric Techniques

Czech Academy of Sciences Publication Activity Database

Ďurišová, Jana; Ackerman, Lukáš; Strnad, L.; Chrastný, V.; Borovička, Jan

2015-01-01

Roč. 39, č. 2 (2015), s. 209-220 ISSN 1639-4488 Institutional support: RVO:67985831 Keywords : Pb isotopes * 206 Pb/ 207 Pb * 208 Pb/ 206 Pb * ICP-MS * certified reference materials * vegetation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.885, year: 2015

Platinum stable isotope analysis of geological standard reference materials by double-spike MC-ICPMS.

Science.gov (United States)

Creech, J B; Baker, J A; Handler, M R; Bizzarro, M

2014-01-10

We report a method for the chemical purification of Pt from geological materials by ion-exchange chromatography for subsequent Pt stable isotope analysis by multiple-collector inductively coupled plasma mass spectrometry (MC-ICPMS) using a 196 Pt- 198 Pt double-spike to correct for instrumental mass bias. Double-spiking of samples was carried out prior to digestion and chemical separation to correct for any mass-dependent fractionation that may occur due to incomplete recovery of Pt. Samples were digested using a NiS fire assay method, which pre-concentrates Pt into a metallic bead that is readily dissolved in acid in preparation for anion-exchange chemistry. Pt was recovered from anion-exchange resin in concentrated HNO 3 acid after elution of matrix elements, including the other platinum group elements (PGE), in dilute HCl and HNO 3 acids. The separation method has been calibrated using a precious metal standard solution doped with a range of synthetic matrices and results in Pt yields of ≥90% with purity of ≥95%. Using this chemical separation technique, we have separated Pt from 11 international geological standard reference materials comprising of PGE ores, mantle rocks, igneous rocks and one sample from the Cretaceous-Paleogene boundary layer. Pt concentrations in these samples range from ca. 5 ng g -1 to 4 μg g -1 . This analytical method has been shown to have an external reproducibility on δ 198 Pt (permil difference in the 198 Pt/ 194 Pt ratio from the IRMM-010 standard) of ±0.040 (2 sd) on Pt solution standards (Creech et al., 2013, J. Anal. At. Spectrom. 28, 853-865). The reproducibility in natural samples is evaluated by processing multiple replicates of four standard reference materials, and is conservatively taken to be ca. ±0.088 (2 sd). Pt stable isotope data for the full set of reference materials have a range of δ 198 Pt values with offsets of up to 0.4‰ from the IRMM-010 standard, which are readily resolved with this technique. These

Uncertainty evaluation in normalization of isotope delta measurement results against international reference materials.

Science.gov (United States)

Meija, Juris; Chartrand, Michelle M G

2018-01-01

Isotope delta measurements are normalized against international reference standards. Although multi-point normalization is becoming a standard practice, the existing uncertainty evaluation practices are either undocumented or are incomplete. For multi-point normalization, we present errors-in-variables regression models for explicit accounting of the measurement uncertainty of the international standards along with the uncertainty that is attributed to their assigned values. This manuscript presents framework to account for the uncertainty that arises due to a small number of replicate measurements and discusses multi-laboratory data reduction while accounting for inevitable correlations between the laboratories due to the use of identical reference materials for calibration. Both frequentist and Bayesian methods of uncertainty analysis are discussed.

Stable isotope analyses of oxygen (18O:17O:16O) and chlorine (37Cl:35Cl) in perchlorate: reference materials, calibrations, methods, and interferences

Science.gov (United States)

Böhlke, John Karl; Mroczkowski, Stanley J.; Sturchio, Neil C.; Heraty, Linnea J.; Richman, Kent W.; Sullivan, Donald B.; Griffith, Kris N.; Gu, Baohua; Hatzinger, Paul B.

2017-01-01

RationalePerchlorate (ClO4−) is a common trace constituent of water, soils, and plants; it has both natural and synthetic sources and is subject to biodegradation. The stable isotope ratios of Cl and O provide three independent quantities for ClO4− source attribution and natural attenuation studies: δ37Cl, δ18O, and δ17O (or Δ17O or 17Δ) values. Documented reference materials, calibration schemes, methods, and interferences will improve the reliability of such studies.MethodsThree large batches of KClO4 with contrasting isotopic compositions were synthesized and analyzed against VSMOW-SLAP, atmospheric O2, and international nitrate and chloride reference materials. Three analytical methods were tested for O isotopes: conversion of ClO4− to CO for continuous-flow IRMS (CO-CFIRMS), decomposition to O2 for dual-inlet IRMS (O2-DIIRMS), and decomposition to O2 with molecular-sieve trap (O2-DIIRMS+T). For Cl isotopes, KCl produced by thermal decomposition of KClO4 was reprecipitated as AgCl and converted into CH3Cl for DIIRMS.ResultsKClO4 isotopic reference materials (USGS37, USGS38, USGS39) represent a wide range of Cl and O isotopic compositions, including non-mass-dependent O isotopic variation. Isotopic fractionation and exchange can affect O isotope analyses of ClO4− depending on the decomposition method. Routine analyses can be adjusted for such effects by normalization, using reference materials prepared and analyzed as samples. Analytical errors caused by SO42−, NO3−, ReO42−, and C-bearing contaminants include isotope mixing and fractionation effects on CO and O2, plus direct interference from CO2 in the mass spectrometer. The results highlight the importance of effective purification of ClO4− from environmental samples.ConclusionsKClO4 reference materials are available for testing methods and calibrating isotopic data for ClO4− and other substances with widely varying Cl or O isotopic compositions. Current ClO4−extraction, purification

USGS42 and USGS43: Human-hair stable hydrogen and oxygen isotopic reference materials and analytical methods for forensic science and implications for published measurement results

Science.gov (United States)

Coplen, T.B.; Qi, H.

2012-01-01

Because there are no internationally distributed stable hydrogen and oxygen isotopic reference materials of human hair, the U.S. Geological Survey (USGS) has prepared two such materials, USGS42 and USGS43. These reference materials span values commonly encountered in human hair stable isotope analysis and are isotopically homogeneous at sample sizes larger than 0.2 mg. USGS42 and USGS43 human-hair isotopic reference materials are intended for calibration of δ(2)H and δ(18)O measurements of unknown human hair by quantifying (1) drift with time, (2) mass-dependent isotopic fractionation, and (3) isotope-ratio-scale contraction. While they are intended for measurements of the stable isotopes of hydrogen and oxygen, they also are suitable for measurements of the stable isotopes of carbon, nitrogen, and sulfur in human and mammalian hair. Preliminary isotopic compositions of the non-exchangeable fractions of these materials are USGS42(Tibetan hair)δ(2)H(VSMOW-SLAP) = -78.5 ± 2.3‰ (n = 62) and δ(18)O(VSMOW-SLAP) = +8.56 ± 0.10‰ (n = 18) USGS42(Indian hair)δ(2)H(VSMOW-SLAP) = -50.3 ± 2.8‰ (n = 64) and δ(18)O(VSMOW-SLAP) = +14.11 ± 0.10‰ (n = 18). Using recommended analytical protocols presented herein for δ(2)H(VSMOW-SLAP) and δ(18)O(VSMOW-SLAP) measurements, the least squares fit regression of 11 human hair reference materials is δ(2)H(VSMOW-SLAP) = 6.085δ(2)O(VSMOW-SLAP) - 136.0‰ with an R-square value of 0.95. The δ(2)H difference between the calibrated results of human hair in this investigation and a commonly accepted human-hair relationship is a remarkable 34‰. It is critical that readers pay attention to the δ(2)H(VSMOW-SLAP) and δ(18)O(VSMOW-SLAP) of isotopic reference materials in publications, and they need to adjust the δ(2)H(VSMOW-SLAP) and δ(18)O(VSMOW-SLAP) measurement results of human hair in previous publications, as needed, to ensure all results on are on the same scales.

Lead Isotopic Composition in Biogenic Certified Reference Materials Determined by Different ICP-based Mass Spectrometric Techniques

Czech Academy of Sciences Publication Activity Database

Ďurišová, J.; Ackerman, L.; Strnad, L.; Chrastný, V.; Borovička, Jan

2015-01-01

Roč. 39, č. 2 (2015), s. 209-220 ISSN 1639-4488 R&D Projects: GA ČR(CZ) GAP504/11/0484 Institutional support: RVO:61389005 Keywords : Pb isotopes * Pb-206 * Pb-207 * Pb-208 * ICP-MS * certified reference materials * vegetation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.885, year: 2015

Certification of a nickel metal reference material for neutron dosimetry (EC Nuclear Reference Material 521)

International Nuclear Information System (INIS)

Pauwels, J.

1988-01-01

Nickel metal, of 99.99 % nominal purity and natural isotopic composition, in the form of 0.1 mm thick foil and 0.5 mm diameter wire has been certified for its cobalt mass fraction. The certified value of cobalt (<0.1μg.g-1) is based on 38 results obtained by neutron activation analysis, emission spectrometry with inductively coupled plasma excitation and atomic absorption spectrometry, whereas the isotopic composition of the nickel was verified by thermal ionization mass spectrometry. The material is intended to be used as a reference material in neutron metrology

Analytical quality control service programme, intercomparison runs, certified reference materials, reference materials 1987-88

International Nuclear Information System (INIS)

1986-12-01

The purpose of the Analytical Quality Control Services (AQCS) programme provided by the IAEA, is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. The tables give details of the intercomparison samples and reference materials distributed by the IAEA in the period 1987 to 1988. 2 tabs

Uranium isotopic composition and uranium concentration in special reference material SRM A (uranium in KCl/LiCl salt matrix)

International Nuclear Information System (INIS)

Graczyk, D.G.; Essling, A.M.; Sabau, C.S.; Smith, F.P.; Bowers, D.L.; Ackerman, J.P.

1997-07-01

To help assure that analysis data of known quality will be produced in support of demonstration programs at the Fuel Conditioning Facility at Argonne National Laboratory-West (Idaho Falls, ID), a special reference material has been prepared and characterized. Designated SRM A, the material consists of individual units of LiCl/KCl eutectic salt containing a nominal concentration of 2.5 wt. % enriched uranium. Analyses were performed at Argonne National Laboratory-East (Argonne, IL) to determine the uniformity of the material and to establish reference values for the uranium concentration and uranium isotopic composition. Ten units from a batch of approximately 190 units were analyzed by the mass spectrometric isotope dilution technique to determine their uranium concentration. These measurements provided a mean value of 2.5058 ± 0.0052 wt. % U, where the uncertainty includes estimated limits to both random and systematic errors that might have affected the measurements. Evidence was found of a small, apparently random, non-uniformity in uranium content of the individual SRM A units, which exhibits a standard deviation of 0.078% of the mean uranium concentration. Isotopic analysis of the uranium from three units, by means of thermal ionization mass spectrometry with a special, internal-standard procedure, indicated that the uranium isotopy is uniform among the pellets with a composition corresponding to 0.1115 ± 0.0006 wt. % 234 U, 19.8336 ± 0.0059 wt. % 235 U, 0.1337 ± 0.0006 wt. % 236 U, and 79.9171 ± 0.0057 wt. % 238 U

235Uranium isotope abundance certified reference material for gamma spectrometry EC nuclear reference material 171 certification report

International Nuclear Information System (INIS)

De Bievre, P.; Eschbach, H.L.; Lesser, R.; Meyer, H.; Audenhove, Van J.

1986-01-01

This certification report contains the information necessary for the final certification of EC nuclear reference material 171. It is also intended to inform the user of the reference material concerned on technical/scientific details which are not given in the certificate. The report describes the reference material which consists of sets of U 3 O 8 samples with five different 235 U/U abundances, filled in cylindrical aluminium cans. The can bottom serves as window for emitted gamma radiation. The report describes how the 235 U/U abundances were characterized, how the other properties relevant for gamma measurements were determined and gives all connected results as well as those from the verification measurements. Appendix A represents the draft certificate. 32 refs

Certification of a uranium-238 dioxide reference material for neutron dosimetry (EC nuclear reference material 501)

International Nuclear Information System (INIS)

Pauwels, J.; Lievens, F.; Ingelbrecht, C.

1989-01-01

Uranium-238 oxide of 99.999% isotopic and 99.98% chemical purity was transformed into dioxide spheres of nominal 0.5 and 1.0 mm diameter by gel precipitation and subsequent calcination under carbon dioxide and under argon containing 5% hydrogen at 1 125 K. The spheres were analysed by thermal ionization mass spectrometry, including isotope dilution, by gravimetry and by potentiometric titration. On the basis of these analyses, the uranium mass fraction was certified at 879.4 ± 2.8 g.kg -1 , and the 235 U/U - and 238 U/U abundances at 10.4 ± 0.5 mg.kg -1 and 999.9896 ± 0.0005 g.kg -1 , respectively. The material is intended to be used as a reference material in neutron metrology

Preparation, characterization and certification of uranium isotope reference materials; Preparacao, Caracterizacao e certificacao de materiais de referencia isotopicos de uranio

Energy Technology Data Exchange (ETDEWEB)

Oliveira Junior, Olivio Pereira de

2006-07-01

This work describes the preparation, characterization and certification of a set of uranium isotope reference materials ranging from 0.5 to 20.0 % of {sup 235}U in mass. The most important concepts of metrology in chemical measurements were applied so that the certified quantities in these materials could be directly traceable to the International System of Units (SI). As a consequence of this approach, these materials can be used in the instruments calibration, estimation of measurement uncertainty, method validation, assessment of performance of analysts, quality control routines and interlaboratory comparison programmes. The most advanced methods and techniques in mass spectrometry, that is, gas source mass spectrometry (GSMS), thermal ionisation mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICPMS) were investigated to identify which are the dominant components in the uncertainty and to quantify its contribution to the final value of the measurement uncertainty of the isotopic ratio. The results obtained were then compared to verify which are the methods and techniques associated to the lowest measurement uncertainty values. The isotope amount ratio n({sup 235}U)/n({sup 238}U) was certified in the materials produced to expanded uncertainties ranging from 0.02 to 0.10 % and the ratios n({sup 234}U)/n({sup 238}U) and n({sup 236}U)/n({sup 238}U), to uncertainties ranging from 0.03 to 2.20 %. These values fully comply to the requirements of the isotopic characterization of nuclear fuel as well as the analysis of environmental samples for nuclear safeguards. (author)

AQCS 1989 - Intercomparison runs reference materials

International Nuclear Information System (INIS)

1989-01-01

The purpose of the Analytical Quality Control Services (AQCS) programme provided by the International Atomic Energy Agency (Agency) is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. Reference Materials available are listed by origin and by analyte giving referenced values and confidence intervals. Only materials, which have one or more properties sufficiently well established from statistical evaluation of previous interlaboratory comparison studies are included. Existing Reference Materials may be updated for previously referenced constituents or properties according to the results of the Agency's Co-ordinated Research Programmes (CRPs) in these fields or according to recently published literature values. They are supplied with a reference sheet stating relevant parameters and properties of the material and can be used as secondary standards for quality control assurance within a laboratory, for checking analytical methods and/or instrumentation or for training purposes. 4 tabs

Isotope research materials

International Nuclear Information System (INIS)

Anon.

1977-01-01

Preparation of research isotope materials is described. Topics covered include: separation of tritium from aqueous effluents by bipolar electrolysis; stable isotope targets and research materials; radioisotope targets and research materials; preparation of an 241 Am metallurgical specimen; reactor dosimeters; ceramic and cermet development; fission-fragment-generating targets of 235 UO 2 ; and wire dosimeters for Westinghouse--Bettis

On the source material of magmas - with special reference to Nd isotopic ratios of igneous rocks

International Nuclear Information System (INIS)

Shuto, Kenji

1980-01-01

In 1973, the Sm-Nd method was first used for the measurement of the absolute age of igneous rocks and meteorites. Subsequently in the following years, the research works by means of the Nd isotopic ratio in igneous rocks have been made strenuously in order to reveal the chemistry of the source materials of magma giving rise to the igneous rocks and further the evolution process of mantle and earth's crust. The fundamental items for the Sm-Nd method are explained. Then, the research results more important in the above connection are given. Finally, the ideas by the author concerning the source materials of magma are presented from the data available on the Nd isotopes in meteorites and igneous rocks. The following matters are described: the fundamentals of Sm-Nd method, the Nd content in seawater, the negative correlation between Nd and Sr isotopic ratios in igneous rocks, magma source materials and Nd isotopes, and considerations on magma source materials. (J.P.N.)

Calibrating NIST SRM 683 as A New International Reference Standard for Zn Isotopes

Science.gov (United States)

Yang, Y.; Zhang, X.; Yu, H.; Huang, F.

2017-12-01

Zinc isotopes have been widely applied in the cosmochemical, geochemical, and environmental studies (Moynier et al. 2017). Obtaining precise Zn isotopic data for inter-laboratory comparison is a prerequisite to these applications. Currently, the JMC3-0749L is the primary reference standard for Zn isotopes (Albarède 2004), but it is not commercially available now. Thus, it is necessary to calibrate a new international primary reference standard for Zn isotopic analysis. Chen et al. (2016) showed that NIST SRM 683 (a pure Zn metal nugget of 140 grams) has a δ66ZnJMC of 0.12‰, which is falling within the range of natural Zn isotopic compositions, and it may a good candidate for the next generation of international reference standard (Chen et al. 2016). In order to further examine whether NIST SRM 683 has a homogeneous Zn isotopic composition, we measured more NIST SRM 683 by double-spike methods using MC-ICPMS (Conway et al. 2013). The metal nuggets of NIST SRM 683 were intensively sampled by micro-drilling. Zinc isotope analyses for two nuggets show that they have δ66Zn of 0.14 ± 0.02‰ (2SD, N = 32) and 0.13 ± 0.02‰ (2SD, N = 33), respectively. These values are similar to those of two Zn metal nuggets (0.11 ± 0.02‰ vs. 0.12 ± 0.02‰) reported previously by Chen et al. (2016). We fully dissolved one nugget, producing pure Zn solution with identical Zn isotopic composition with the drilling samples. All results strongly support that NIST SRM 683 is homogeneous in Zn isotopic compositions which could be an ideal candidate for the next reference for Zn isotopes. Tests on more metal nuggets will be performed in a few months for further confirming the Zn isotope compositions and homogeneity. Reference: Albarède et al., 2004. 'The stable isotope geochemistry of copper and zinc', Reviews in Mineralogy and Geochemistry, 55: 409-27. Chen et al., 2016. 'Zinc Isotopic Compositions of NIST SRM 683 and Whole-Rock Reference Materials', Geostandards and

IAEA AQCS catalogue for reference materials and intercomparison exercises 1998/1999

International Nuclear Information System (INIS)

1999-01-01

Fore more than thirty years the International Atomic Energy Agency (IAEA), through its Analytical Quality Control Services (AQCS) programme, has been assisting Member States' laboratories to maintain and improve the reliability of their analyses by organizing intercomparison exercises and by preparing and distributing biological, environmental and marine reference materials. The catalogue consists principally of two parts: The list of all available IAEA reference materials grouped into five categories: reference materials for radionuclides; reference materials for trace, minor and major elements, including oxides; reference materials for stable isotopes; reference materials for organic contaminants and methyl mercury containing materials. Lists of all available IAEA reference materials sorted by analytes. In addition information on recommended half-life data and suppliers of radioactive sources is provided. Planned intercomparisons are advertised and request forms for participation in intercomparisons are included. Forms for ordering reference materials, quality control spectra for gamma-spectrometry on diskettes and AQCS related publications are also provided

Standard and reference materials for environmental science. Part 1. Technical memo

Energy Technology Data Exchange (ETDEWEB)

Cantillo, A.Y.

1995-11-01

This is the fourth edition of the catalog of reference materials suited for use in environmental science, originally compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists more than 1200 reference materials from 28 producers and contains information about their proper use, sources, availability, and analyte concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross references to CAS registry numbers, alternate names, and chemical structures of selected organic compounds.

Standard and reference materials for environmental science. Part 2. Technical memo

Energy Technology Data Exchange (ETDEWEB)

Cantillo, A.Y.

1995-11-01

This is the fourth edition of the catalog of reference materials suited for use in environmental science, originally compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists more than 1200 reference materials from 28 producers and contains information about their proper use, sources, availability, and analyte concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross references to CAS registry numbers, alternate names, and chemical structures of selected organic compounds.

Committee on Diabetes Mellitus Indices of the Japan Society of Clinical Chemistry-recommended reference measurement procedure and reference materials for glycated albumin determination.

Science.gov (United States)

Takei, Izumi; Hoshino, Tadao; Tominaga, Makoto; Ishibashi, Midori; Kuwa, Katsuhiko; Umemoto, Masao; Tani, Wataru; Okahashi, Mikiko; Yasukawa, Keiko; Kohzuma, Takuji; Sato, Asako

2016-01-01

Glycated albumin is an intermediate glycaemic control marker for which there are several measurement procedures with entirely different reference intervals. We have developed a reference measurement procedure for the purpose of standardizing glycated albumin measurements. The isotope dilution liquid chromatography/tandem mass spectrometry method was developed as a reference measurement procedure for glycated albumin. The stable isotopes of lysine and fructosyl-lysine, which serve as an internal standard, were added to albumin isolated from serum, followed by hydrogenation. After hydrolysis of albumin with hot hydrochloric acid, the liberated lysine and fructosyl-lysine were measured by liquid chromatography/tandem mass spectrometry, and their concentrations were determined from each isotope ratio. The reference materials (JCCRM611) for determining of glycated albumin were prepared from pooled patient blood samples. The isotope dilution-tandem mass spectrometry calibration curve of fructosyl-lysine and lysine showed good linearity (r = 0.999). The inter-assay and intra-assay coefficient of variation values of glycated albumin measurement were 1.2 and 1.4%, respectively. The glycated albumin values of serum in patients with diabetes assessed through the use of this method showed a good relationship with routine measurement procedures (r = 0.997). The relationship of glycated albumin values of the reference material (JCCRM611) between these two methods was the same as the relationship with the patient serum samples. The Committee on Diabetes Mellitus Indices of the Japan Society of Clinical Chemistry recommends the isotope dilution liquid chromatography/tandem mass spectrometry method as a reference measurement procedure, and JCCRM611 as a certified reference material for glycated albumin measurement. In addition, we recommend the traceability system for glycated albumin measurement. © The Author(s) 2015.

Defining an absolute reference frame for 'clumped' isotope studies of CO 2

Science.gov (United States)

Dennis, Kate J.; Affek, Hagit P.; Passey, Benjamin H.; Schrag, Daniel P.; Eiler, John M.

2011-11-01

We present a revised approach for standardizing and reporting analyses of multiply substituted isotopologues of CO 2 (i.e., 'clumped' isotopic species, especially the mass-47 isotopologues). Our approach standardizes such data to an absolute reference frame based on theoretical predictions of the abundances of multiply-substituted isotopologues in gaseous CO 2 at thermodynamic equilibrium. This reference frame is preferred over an inter-laboratory calibration of carbonates because it enables all laboratories measuring mass 47 CO 2 to use a common scale that is tied directly to theoretical predictions of clumping in CO 2, regardless of the laboratory's primary research field (carbonate thermometry or CO 2 biogeochemistry); it explicitly accounts for mass spectrometric artifacts rather than convolving (and potentially confusing) them with chemical fractionations associated with sample preparation; and it is based on a thermodynamic equilibrium that can be experimentally established in any suitably equipped laboratory using commonly available materials. By analyzing CO 2 gases that have been subjected to established laboratory procedures known to promote isotopic equilibrium (i.e., heated gases and water-equilibrated CO 2), and by reference to thermodynamic predictions of equilibrium isotopic distributions, it is possible to construct an empirical transfer function that is applicable to data with unknown clumped isotope signatures. This transfer function empirically accounts for the fragmentation and recombination reactions that occur in electron impact ionization sources and other mass spectrometric artifacts. We describe the protocol necessary to construct such a reference frame, the method for converting gases with unknown clumped isotope compositions to this reference frame, and suggest a protocol for ensuring that all reported isotopic compositions (e.g., Δ 47 values; Eiler and Schauble, 2004; Eiler, 2007) can be compared among different laboratories and

Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials.

Science.gov (United States)

Murphy, K E; Beary, E S; Rearick, M S; Vocke, R D

2000-10-01

Lead (Pb) and cadmium (Cd) have been determined in six new environmental standard reference materials (SRMs) using isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The SRMs are the following: SRM 1944, New York-New Jersey Waterway Sediment, SRMs 2583 and 2584, Trace Elements in Indoor Dust, Nominal 90 mg/kg and 10,000 mg/kg Lead, respectively, SRMs 2586 and 2587, Trace Elements in Soil Containing Lead from Paint, Nominal 500 mg/kg and 3,000 mg/kg Lead, respectively, and SRM 2782, Industrial Sludge. The capabilities of ID ICP-MS for the certification of Pb and Cd in these materials are assessed. Sample preparation and ratio measurement uncertainties have been evaluated. Reproducibility and accuracy of the established procedures are demonstrated by determination of gravimetrically prepared primary standard solutions and by comparison with isotope dilution thermal ionization mass spectrometry (ID TIMS). Material heterogeneity was readily demonstrated to be the dominant source of uncertainty in the certified values.

Feasibility Study for the Development of Plutonium Reference Materials for Age Dating in Nuclear Forensics

International Nuclear Information System (INIS)

Sturm, M.; Richter, S.; Aregbe, Y.; Wellum, R.; Altzitzoglou, T.; Verbruggen, A.; Mayer, K.; Prohaska, T.

2010-01-01

Isotopic reference materials certified for the age of nuclear material (uranium, plutonium) are needed in the fields of nuclear forensics and environmental measurements. Therefore a feasibility study for the development of plutonium reference materials for age dating has been started recently at the Institute for Reference Materials and Measurements (EC-JRC-IRMM). The ''age'' of the material is defined as the time that has passed since the last chemical separation of the mother and daughter isotopes (e.g. 241 Pu and 241 Am). Assuming that the separation has been complete and all the daughter isotopes have been removed from the original material during this last separation, the age of the material can be determined by measuring the ratio of daughter and mother radio-nuclides, e.g. 241 Am/ 241 Pu. At a given time after the last separation and depending on the half lives of the radio-nuclides involved, a certain amount of the daughter radionuclide(s) will be present. For the determination of the unknown age of a material different ''clocks'' can be used; ''clocks'' are pairs of mother and daughter radio-nuclides, such as 241 Am/ 241 Pu, 238 Pu/ 234 U, 239 Pu/ 235 U, 240 Pu/ 236 U, and possibly 242 Pu/ 238 U. For the age estimation of a real sample, such as material seized in nuclear forensics investigations or dust samples in environmental measurements, it is advisable to use more than one clock in order to ensure the reliability of the results and to exclude the possibility that the sample under question is a mixture of two or more materials. Consequently, a future reference material certified for separation date should ideally be certified for more than one ''clock'' or several reference materials for different ''clocks'' should be developed. The first step of this study is to verify the known separation dates of different plutonium materials of different ages and isotopic compositions by measuring the mother ( 238 Pu, 239 Pu, 240 Pu, 241 Pu, 242 Pu) and daughter

Catalogue of reference materials of interest to nuclear energy

International Nuclear Information System (INIS)

1974-12-01

A provisional list of available chemical, isotopic and trace elements reference materials of interest to nuclear energy has been established. Emphasis has been given to the substances containing uranium and plutonium. Certified values, sample sizes, prices and addresses of suppliers are indicated

Standard reference materials analysis for MINT Radiocarbon Laboratory

International Nuclear Information System (INIS)

Noraishah Othman; Kamisah Alias; Nasasni Nasrul

2004-01-01

As a follow-up to the setting up of the MINT Radiocarbon Dating facility. an exercise on the IAEA standard reference materials was carried out. Radiocarbon laboratories frequently used these 8 natural samples to verify their systems. The materials were either pretreated or analysed directly to determine the activity of 14 C isotopes of the five samples expressed in % Modern (pMC) terms and to make recommendations on further use of these materials. We present the results of the five materials and discuss the analyses that were undertaken. (Author)

Characterizing uranium oxide reference particles for isotopic abundances and uranium mass by single particle isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Kraiem, M.; Richter, S.; Erdmann, N.; Kühn, H.; Hedberg, M.; Aregbe, Y.

2012-01-01

Highlights: ► A method to quantify the U mass in single micron particles by ID-TIMS was developed. ► Well-characterized monodisperse U-oxide particles produced by an aerosol generator were used. ► A linear correlation between the mass of U and the volume of particle(s) was found. ► The method developed is suitable for determining the amount of U in a particulate reference material. - Abstract: Uranium and plutonium particulate test materials are becoming increasingly important as the reliability of measurement results has to be demonstrated to regulatory bodies responsible for maintaining effective nuclear safeguards. In order to address this issue, the Institute for Reference Materials and Measurements (IRMM) in collaboration with the Institute for Transuranium Elements (ITU) has initiated a study to investigate the feasibility of preparing and characterizing a uranium particle reference material for nuclear safeguards, which is finally certified for isotopic abundances and for the uranium mass per particle. Such control particles are specifically required to evaluate responses of instruments based on mass spectrometric detection (e.g. SIMS, TIMS, LA-ICPMS) and to help ensuring the reliability and comparability of measurement results worldwide. In this paper, a methodology is described which allows quantifying the uranium mass in single micron particles by isotope dilution thermal ionization mass spectrometry (ID-TIMS). This methodology is characterized by substantial improvements recently achieved at IRMM in terms of sensitivity and measurement accuracy in the field of uranium particle analysis by TIMS. The use of monodisperse uranium oxide particles prepared using an aerosol generation technique developed at ITU, which is capable of producing particles of well-characterized size and isotopic composition was exploited. The evidence of a straightforward correlation between the particle volume and the mass of uranium was demonstrated in this study

The importance of reference materials in doping-control analysis.

Science.gov (United States)

Mackay, Lindsey G; Kazlauskas, Rymantas

2011-08-01

Currently a large range of pure substance reference materials are available for calibration of doping-control methods. These materials enable traceability to the International System of Units (SI) for the results generated by World Anti-Doping Agency (WADA)-accredited laboratories. Only a small number of prohibited substances have threshold limits for which quantification is highly important. For these analytes only the highest quality reference materials that are available should be used. Many prohibited substances have no threshold limits and reference materials provide essential identity confirmation. For these reference materials the correct identity is critical and the methods used to assess identity in these cases should be critically evaluated. There is still a lack of certified matrix reference materials to support many aspects of doping analysis. However, in key areas a range of urine matrix materials have been produced for substances with threshold limits, for example 19-norandrosterone and testosterone/epitestosterone (T/E) ratio. These matrix-certified reference materials (CRMs) are an excellent independent means of checking method recovery and bias and will typically be used in method validation and then regularly as quality-control checks. They can be particularly important in the analysis of samples close to threshold limits, in which measurement accuracy becomes critical. Some reference materials for isotope ratio mass spectrometry (IRMS) analysis are available and a matrix material certified for steroid delta values is currently under production. In other new areas, for example the Athlete Biological Passport, peptide hormone testing, designer steroids, and gene doping, reference material needs still need to be thoroughly assessed and prioritised.

AQCS intercomparison runs, reference materials 1991

International Nuclear Information System (INIS)

1991-01-01

The purpose of the Analytical Quality Control Services programme provided by the IAEA is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. The determination of accuracy requires special procedures such as analysis to be carried out by as many different and independent methods, analysts and techniques as possible, control analysis with reference materials and participation in interlaboratory comparison studies. This document gives details of the specimens and samples which the IAEA intends to distribute in 1991. Tabs

Metrology for stable isotope reference materials: 13C/12C and 18O/16O isotope ratio value assignment of pure carbon dioxide gas samples on the Vienna PeeDee Belemnite-CO2 scale using dual-inlet mass spectrometry.

Science.gov (United States)

Srivastava, Abneesh; Michael Verkouteren, R

2018-05-25

Isotope ratio measurements have been conducted on a series of isotopically distinct pure CO 2 gas samples using the technique of dual-inlet isotope ratio mass spectrometry (DI-IRMS). The influence of instrumental parameters, data normalization schemes on the metrological traceability and uncertainty of the sample isotope composition have been characterized. Traceability to the Vienna PeeDee Belemnite(VPDB)-CO 2 scale was realized using the pure CO 2 isotope reference materials(IRMs) 8562, 8563, and 8564. The uncertainty analyses include contributions associated with the values of iRMs and the repeatability and reproducibility of our measurements. Our DI-IRMS measurement system is demonstrated to have high long-term stability, approaching a precision of 0.001 parts-per-thousand for the 45/44 and 46/44 ion signal ratios. The single- and two-point normalization bias for the iRMs were found to be within their published standard uncertainty values. The values of 13 C/ 12 C and 18 O/ 16 O isotope ratios are expressed relative to VPDB-CO 2 using the [Formula: see text] and [Formula: see text] notation, respectively, in parts-per-thousand (‰ or per mil). For the samples, value assignments between (-25 to +2) ‰ and (-33 to -1) ‰ with nominal combined standard uncertainties of (0.05, 0.3) ‰ for [Formula: see text] and [Formula: see text], respectively were obtained. These samples are used as laboratory reference to provide anchor points for value assignment of isotope ratios (with VPDB traceability) to pure CO 2 samples. Additionally, they serve as potential parent isotopic source material required for the development of gravimetric based iRMs of CO 2 in CO 2 -free dry air in high pressure gas cylinder packages at desired abundance levels and isotopic composition values. Graphical abstract CO 2 gas isotope ratio metrology.

Certification of biological candidates reference materials by neutron activation analysis

Science.gov (United States)

Kabanov, Denis V.; Nesterova, Yulia V.; Merkulov, Viktor G.

2018-03-01

The paper gives the results of interlaboratory certification of new biological candidate reference materials by neutron activation analysis recommended by the Institute of Nuclear Chemistry and Technology (Warsaw, Poland). The correctness and accuracy of the applied method was statistically estimated for the determination of trace elements in candidate reference materials. The procedure of irradiation in the reactor thermal fuel assembly without formation of fast neutrons was carried out. It excluded formation of interfering isotopes leading to false results. The concentration of more than 20 elements (e.g., Ba, Br, Ca, Co, Ce, Cr, Cs, Eu, Fe, Hf, La, Lu, Rb, Sb, Sc, Ta, Th, Tb, Yb, U, Zn) in candidate references of tobacco leaves and bottom sediment compared to certified reference materials were determined. It was shown that the average error of the applied method did not exceed 10%.

Standard and reference materials for marine science. Third edition. Technical memo

International Nuclear Information System (INIS)

Cantillo, A.Y.

1992-08-01

The third edition of the catalog of reference materials suited for use in marine science, originally compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists close to 2,000 reference materials from sixteen producers and contains information about their proper use, sources, availability, and analyte concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross references to CAS registry numbers, alternate names, and chemical structures of selected organic compounds. The catalog is being published independently by both NOAA and IOC/UNEP and is available from NOAA/NOS/ORCA in electronic form

Preparation and characterization of the fish reference material

International Nuclear Information System (INIS)

Ulrich, Joao Cristiano

2011-01-01

The certified reference materials (CRMs) play an important role in obtaining measurement results traceable to the International System of Units, through an unbroken chain of comparisons. Thus, the demand for new certified reference materials (CRMs) increases every day in all areas of knowledge. The availability of reference materials, mainly in Brazil is still incipient, given that the demand far exceeds the available variety of these materials. The amount of certified reference materials available in the country is insufficient to meet the need of the scientific community and demands for development of new methodologies. Among the many areas in need of reference materials, we highlight the importance for the food trade balance for these products within the country. The certification of food products, intended both for export and for domestic consumption, requires analysis methods that provide precise and accurate results to ensure product quality. This paper describes the preparation and certification of a reference material in the fish matrix in mercury and methylmercury. The study brings together since the stage of material selection, preparation, development of homogeneity and stability studies and characterization. The certification was performed by means of measurements using two analytical techniques, flow injection analysis - cold vapor atomic absorption spectrometry (FIA-CV-AAS) and isotope dilution applied to mass spectrometry (IDMS), which is a primary method. In this work the standards of the ISO 30 (ABNT 30-34) and ISO Guide 35 was used as the basis for the preparation and characterization of the material. For the calculation of uncertainties was used the GUM and Eurachem guide. As a result, was produced and certified a lot of material in relation to the concentration of mercury (Hg = 0.271 ± 0.057 mg g -1 ) and methylmercury (MeHg = 0.245 ± 0.038 mg g -1 ), and informational values of lead and arsenic. (author)

Recommended reference materials for realization of physicochemical properties density

CERN Document Server

Herington, E F G

1976-01-01

This book first presents the nomenclature and units used in the determination of densities of liquids and solids, followed by a general description of the apparatus and the methods used in the measurement of density, with particular reference to the pycnometric, hydrostatic weighing, magnetic float, and temperature flotation methods. The use of water as a density reference material is then explained, focusing on the isotopic composition of Standard Mean Ocean Water (SMOW) and the absolute density of SMOW as a function of temperature. Problems due to the effect of pressure and dissolved gases o

Determination of zinc stable isotopes in biological materials using isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Patterson, K.Y.; Veillon, Claude

1992-01-01

A method is described for using isotope dilution to determine both the amount of natural zinc and enriched isotopes of zinc in biological samples. Isotope dilution inductively coupled plasma mass spectrometry offers a way to quantify not only the natural zinc found in a sample but also the enriched isotope tracers of zinc. Accurate values for the enriched isotopes and natural zinc are obtained by adjusting the mass count rate data for measurable instrumental biases. Analytical interferences from the matrix are avoided by extracting the zinc from the sample matrix using diethylammonium diethyldithiocarbamate. The extraction technique separates the zinc from elements which form interfering molecular ions at the same nominal masses as the zinc isotopes. Accuracy of the method is verified using standard reference materials. The detection limit is 0.06 μg Zn per sample. Precision of the abundance ratios range from 0.3-0.8%. R.S.D. for natural zinc concentrations is about 200-600 μg g -1 . The accuracy and precision of the measurements make it possible to follow enriched isotopic tracers of zinc in biological samples in metabolic tracer studies. (author). 19 refs.; 1 fig., 4 tabs

Reference and intercomparison materials for stable isotopes of light elements. Proceedings of a consultants meeting held in Vienna, 1-3 December 1993

International Nuclear Information System (INIS)

1995-09-01

The stable isotope composition of elements varies in natural compounds as a consequence of the slightly different physico-chemical behaviour of isotopes. The possibility of measuring the stable isotope relative variations with high precision, using mass spectrometry, promoted the rise of new fields of research in geochemistry and hydrology and, more recently, in environmental studies. The steady growth of these investigations and of their practical applications has emphasized the need for high quality isotopic standards and intercomparison samples, with well determined isotopic composition, for the intercalibration of analytical techniques and results among laboratories. The organization of the Consultants Meeting on Stable Isotope Standards and Intercomparison Materials held in Vienna from 1 to 3 December 1993, the fifth of this type (the previous meetings took place in 1966, 1976, 1983 and 1985), called for a review and a discussion of the characteristics, quality and availability of the existing standards and intercalibration materials, and for an assessment of needs for new materials, in view of recent developments and applications. A large part of the discussions was devoted to the new materials prepared for sulphur isotope analysis and the analytical requirements for highly precise isotopic analysis of CO 2 . The papers presented at the meeting are assembled in this volume. Refs, figs and tabs

Reference and intercomparison materials for stable isotopes of light elements. Proceedings of a consultants meeting held in Vienna, 1-3 December 1993

Energy Technology Data Exchange (ETDEWEB)

NONE

1995-09-01

The stable isotope composition of elements varies in natural compounds as a consequence of the slightly different physico-chemical behaviour of isotopes. The possibility of measuring the stable isotope relative variations with high precision, using mass spectrometry, promoted the rise of new fields of research in geochemistry and hydrology and, more recently, in environmental studies. The steady growth of these investigations and of their practical applications has emphasized the need for high quality isotopic standards and intercomparison samples, with well determined isotopic composition, for the intercalibration of analytical techniques and results among laboratories. The organization of the Consultants Meeting on Stable Isotope Standards and Intercomparison Materials held in Vienna from 1 to 3 December 1993, the fifth of this type (the previous meetings took place in 1966, 1976, 1983 and 1985), called for a review and a discussion of the characteristics, quality and availability of the existing standards and intercalibration materials, and for an assessment of needs for new materials, in view of recent developments and applications. A large part of the discussions was devoted to the new materials prepared for sulphur isotope analysis and the analytical requirements for highly precise isotopic analysis of CO{sub 2}. The papers presented at the meeting are assembled in this volume. Refs, figs and tabs.

Uranium reference materials

International Nuclear Information System (INIS)

Donivan, S.; Chessmore, R.

1987-07-01

The Technical Measurements Center has prepared uranium mill tailings reference materials for use by remedial action contractors and cognizant federal and state agencies. Four materials were prepared with varying concentrations of radionuclides, using three tailings materials and a river-bottom soil diluent. All materials were ground, dried, and blended thoroughly to ensure homogeneity. The analyses on which the recommended values for nuclides in the reference materials are based were performed, using independent methods, by the UNC Geotech (UNC) Chemistry Laboratory, Grand Junction, Colorado, and by C.W. Sill (Sill), Idaho National Engineering Laboratory, Idaho Falls, Idaho. Several statistical tests were performed on the analytical data to characterize the reference materials. Results of these tests reveal that the four reference materials are homogeneous and that no large systematic bias exists between the analytical methods used by Sill and those used by TMC. The average values for radionuclides of the two data sets, representing an unbiased estimate, were used as the recommended values for concentrations of nuclides in the reference materials. The recommended concentrations of radionuclides in the four reference materials are provided. Use of these reference materials will aid in providing uniform standardization among measurements made by remedial action contractors. 11 refs., 9 tabs

Compilation of minimum and maximum isotope ratios of selected elements in naturally occurring terrestrial materials and reagents

Science.gov (United States)

Coplen, T.B.; Hopple, J.A.; Böhlke, J.K.; Peiser, H.S.; Rieder, S.E.; Krouse, H.R.; Rosman, K.J.R.; Ding, T.; Vocke, R.D.; Revesz, K.M.; Lamberty, A.; Taylor, P.; De Bievre, P.

2002-01-01

Documented variations in the isotopic compositions of some chemical elements are responsible for expanded uncertainties in the standard atomic weights published by the Commission on Atomic Weights and Isotopic Abundances of the International Union of Pure and Applied Chemistry. This report summarizes reported variations in the isotopic compositions of 20 elements that are due to physical and chemical fractionation processes (not due to radioactive decay) and their effects on the standard atomic weight uncertainties. For 11 of those elements (hydrogen, lithium, boron, carbon, nitrogen, oxygen, silicon, sulfur, chlorine, copper, and selenium), standard atomic weight uncertainties have been assigned values that are substantially larger than analytical uncertainties because of common isotope abundance variations in materials of natural terrestrial origin. For 2 elements (chromium and thallium), recently reported isotope abundance variations potentially are large enough to result in future expansion of their atomic weight uncertainties. For 7 elements (magnesium, calcium, iron, zinc, molybdenum, palladium, and tellurium), documented isotope-abundance variations in materials of natural terrestrial origin are too small to have a significant effect on their standard atomic weight uncertainties. This compilation indicates the extent to which the atomic weight of an element in a given material may differ from the standard atomic weight of the element. For most elements given above, data are graphically illustrated by a diagram in which the materials are specified in the ordinate and the compositional ranges are plotted along the abscissa in scales of (1) atomic weight, (2) mole fraction of a selected isotope, and (3) delta value of a selected isotope ratio. There are no internationally distributed isotopic reference materials for the elements zinc, selenium, molybdenum, palladium, and tellurium. Preparation of such materials will help to make isotope ratio measurements among

Hafnium isotope ratios of nine GSJ reference samples

International Nuclear Information System (INIS)

Hanyu, Takeshi; Nakai, Shun'ichi; Tatsuta, Riichiro

2005-01-01

176 Hf/ 177 Hf ratios of nine geochemical reference rocks from the Geological Survey of Japan, together with BIR-1 and BCR-2, were determined using multi-collector inductively coupled plasma mass spectrometry. Our data for BIR-1, BCR-2 and JB-1 are in agreement with those previously reported, demonstrating the appropriateness of the chemical procedure and isotopic measurement employed in this study. The reference rocks have a wide range of 176 Hf/ 177 Hf covering the field defined by various volcanic rocks, such as mid-ocean ridge basalts, ocean island basalts, and subduction related volcanic rocks. They are therefore suitable as rock standards for Hf isotope measurement of geological samples. (author)

Isotope exchange reaction on solid breeder materials

International Nuclear Information System (INIS)

Baba, A.; Nishikawa, M.; Eguchi, T.; Kawagoe, T.

2000-01-01

Lithium ceramic materials such as Li 2 O, LiAlO 2 , Li 2 ZrO 3 , Li 2 TiO 3 and Li 4 SiO 4 are considered to be as candidate for the tritium breeding material in a deuterium-tritium (D-T) fusion reactor. In the recent blanket designs, helium gas with hydrogen or deuterium is planned to be used as the blanket purge gas to reduce tritium inventory and promote tritium release from the breeding material. In addition, the rate of isotope exchange reaction between hydrogen isotopes in the purge gas and tritium on the surface of the breeding material is necessary to analyze the tritium release behavior from the breeding materials. However, the rate of isotope exchange reactions between hydrogen isotopes in the purge gas and tritium on the surface of those materials has not been quantified until recently. Recently, the present authors quantified the rate of isotope exchange reaction on Li 2 O and Li 2 ZrO 3 . The overall mass transfer coefficients representing the isotope exchange reaction between H 2 and D 2 O on breeding materials or the same between D 2 and H 2 O are experimentally obtained in this study. Comparison to isotope exchange reaction rates on various breeding materials is also performed in this study. Discussions about the effects of temperature, concentration of hydrogen in the purge gas or flow rate of the purge gas on the conversion of tritiated water to tritium gas are also performed

Biological and environmental reference materials for trace elements, nuclides and organic microcontaminants

International Nuclear Information System (INIS)

Cortes Toro, E.; Parr, R.M.; Clements, S.A.

1990-01-01

This report has been produced from a database on analytical reference materials of biological and environmental origin, which is maintained at the International Atomic Energy Agency. It is an updated version of an earlier report, published in 1985, which focussed mainly on reference materials for trace elements. In the present version of the report, reference materials for trace elements still constitute the major part of the data; however, information is also now included on a number of other selected analytes of relevance to IAEA programmes, i.e. radionuclides, stable isotopes and organic microcontaminants. The database presently contains 2,694 analyte values for 117 analytes in 116 biological and 77 environmental (non-biological) reference materials produced by 20 different suppliers. Additional information on the cost of the material, the unit size supplied, (weight or volume), and the minimum weight of material recommended for analysis is also provided (if available to the authors). It is expected that this report will help analysts to select the reference material that matches as closely as possible, with respect to matrix type and concentrations of the analytes of interest, the ''real'' samples that are to be analysed. Refs, 12 tabs

The production and certification of a plutonium equal-atom reference material: NBL CRM 128

International Nuclear Information System (INIS)

Crawford, D.W.

1990-07-01

This report describes the design, production, and certification of the New Brunswick Laboratory plutonium equal-atom certified reference material (CRM), NBL CRM 128. The primary use of this CRM is for the determination of bias corrections encountered in the operation of a mass spectrometer. This reference material is available to the US Department of Energy contractor-operated and government-operated laboratories, as well as to the international nuclear safeguards community. The absolute, or unbiased, certified value for the CRM's Pu-242/Pu-239 ratio is 1.00063 ± 0.00026 (95% confidence interval) as of October 1, 1984. This value was obtained through the quantitative blending of high-purity, chemically and isotopically characterized separated isotopes, as well as through intercomparisons of CRM samples with calibration mixtures using thermal ionization mass spectrometry. 32 tabs

Comprehensive inter-laboratory calibration of reference materials for δ18O versus VSMOW using various on-line high-temperature conversion techniques

Science.gov (United States)

Brand, Willi A.; Coplen, Tyler B.; Aerts-Bijma, Anita T.; Bohlke, John Karl; Gehre, Matthias; Geilmann, Heike; Groning, Manfred; Jansen, Henk G.; Meijer, Harro A. J.; Mroczkowski, Stanley J.; Qi, Haiping; Soergel, Karin; Stuart-Williams, Hilary; Weise, Stephan M.; Werner, Roland A.

2009-01-01

Internationally distributed organic and inorganic oxygen isotopic reference materials have been calibrated by six laboratories carrying out more than 5300 measurements using a variety of high-temperature conversion techniques (HTC) in an evaluation sponsored by the International Union of Pure and Applied Chemistry (IUPAC). To aid in the calibration of these reference materials, which span more than 125‰, an artificially enriched reference water (δ18O of +78.91‰) and two barium sulfates (one depleted and one enriched in 18O) were prepared and calibrated relative to VSMOW2 and SLAP reference waters. These materials were used to calibrate the other isotopic reference materials in this study, which yielded:Reference materialδ18O and estimated combined uncertainty IAEA-602 benzoic acid+71.28 ± 0.36‰USGS35 sodium nitrate+56.81 ± 0.31‰IAEA-NO-3 potassium nitrate+25.32 ± 0.29‰IAEA-601 benzoic acid+23.14 ± 0.19‰IAEA-SO-5 barium sulfate+12.13 ± 0.33‰NBS 127 barium sulfate+8.59 ± 0.26‰VSMOW2 water0‰IAEA-600 caffeine−3.48 ± 0.53‰IAEA-SO-6 barium sulfate−11.35 ± 0.31‰USGS34 potassium nitrate−27.78 ± 0.37‰SLAP water−55.5‰The seemingly large estimated combined uncertainties arise from differences in instrumentation and methodology and difficulty in accounting for all measurement bias. They are composed of the 3-fold standard errors directly calculated from the measurements and provision for systematic errors discussed in this paper. A primary conclusion of this study is that nitrate samples analyzed for δ18O should be analyzed with internationally distributed isotopic nitrates, and likewise for sulfates and organics. Authors reporting relative differences of oxygen-isotope ratios (δ18O) of nitrates, sulfates, or organic material should explicitly state in their reports the δ18O values of two or more internationally distributed nitrates (USGS34, IAEA-NO-3, and USGS35), sulfates (IAEA-SO-5, IAEA

Evaluation of Solid Geologic Reference Materials for Uranium-Series Measurements via LA-ICPMS

Science.gov (United States)

Matthews, K. A.; Goldstein, S. J.; Norman, D. E.; Nunn, A. J.; Murrell, M. T.

2008-12-01

Uranium-series geochemistry and geochronology have a wide range of applications in paleoclimatology, volcanology and other disciplines. To further explore these fields, the geoanalytical community has now begun to exploit recent advances in in situ, micron-scale sampling via laser ablation-ICPMS. Unfortunately, improvements in instrumentation have generally outpaced development of the appropriate geologic reference materials required for in situ U-series work. We will report results for uranium and thorium isotopic ratios and elemental concentrations measured in a suite of solid standards from the USGS (e.g., BCR-2G, BHVO-2G, GSD-1G, MACS-1, NKT-2G), as well as those from the MPI-DING series (e.g., ATHO-G, T1-G, StHs6/80-G). Specifically created for microanalysis, two of these standards are synthetic (GSD-1G, MACS-1) and the remainder are naturally-sourced glasses. They cover a range of compositions, ages (± secular equilibrium), elemental concentrations and expected isotopic ratios. The U-series isotopics of some powdered source materials have been characterized (e.g., BCR-2, BHVO-2), although there is no confirmation of the same ratios in the glass. Bulk measurement of these solid standards via TIMS and solution multicollector-ICPMS can then be used to assess the performance of LA-ICPMS techniques which require matrix-matched solid standards for correction of U-series elemental and isotopic ratios. These results from existing, widely-available reference materials will also facilitate quantification and comparison of U-series data among laboratories in the broader geoscience community.

Survey of reference materials for trace elements, nuclides and organic microcontaminants

International Nuclear Information System (INIS)

Parr, R.M.; Stone, S.F.; Bel-Amakeletch, T.; Zeisler, R.

1998-01-01

The International Atomic Energy Agency (IAEA), in co-operation with the United Nations Environment Programme (UNEP), has recently prepared a survey on internationally available analytical reference materials for trace elements, nuclides and organic contaminants in biological, environmental and related matrices. The purpose is to help analysts to select reference materials for quality assurance that match as closely as possible, with respect to matrix type and concentrations of the measurands of interest, the ''real'' samples that are to be measured. The present version of the survey, which is available in the form of two cost-free printed volumes [1], contains over 10,000 certified and information values in 650 reference materials from 27 different producers. The 455 measurands listed include trace elements, major and minor elements, organic contaminants, organometallic compounds, radionuclides and stable isotopes. Currently, the database from which the survey has been produced is being modified and extended so as to make the data available in electronic form via the Internet. (orig.)

Preparation of reference material for organochlorine pesticides in a herbal matrix.

Science.gov (United States)

Wong, Yiu Chung; Wong, Siu Kay; Kam, Tat Ting

2008-12-01

The development of reference material for four organochlorine pesticides, namely hexachlorobenzene and three isomers of hexachlorocyclohexane (alpha-hexachlorocyclohexane, beta-hexachlorocyclohexane and gamma-hexachlorocyclohexane), in a ginseng root sample is presented. Raw materials (Panax ginseng) were purchased from a local market and confirmed to contain certain levels of incurred organochlorine pesticide residues by a validated gas chromatography-mass selective detection method. A total of more than 300 bottles each containing 25 g of samples were prepared after the materials had been freeze-dried, milled and thoroughly mixed. The homogeneity and stability of samples from randomly selected bottles were verified and the reference values were characterized using a highly precise isotope dilution gas chromatography-mass spectrometry (ID-GCMS) method that was recently developed by our laboratory. The purity of standard organochlorine chemicals was determined against certified reference materials to establish the accuracy of the ID-GCMS analysis. The concentrations (+/- expanded uncertainty) of hexachlorobenzene, alpha-hexachlorocyclohexane, beta-hexachlorocyclohexane and gamma-hexachlorocyclohexane in the reference material were 0.198 +/- 0.015, 0.450 +/- 0.022, 0.213 +/- 0.011 and 0.370 +/- 0.032 mg kg(-1), respectively. A portion (70 bottles) of the samples was also used in a proficiency testing (PT) scheme for assessing the testing capabilities of field laboratories. The consensus mean values of the PT obtained from the 70 participants were on the same order but deviated by -2.7 to -14.1% from those of the assigned reference values. Because of the wide spread of participants' data (relative standard deviation ranging from 44 to 56%), the PT results were not included in the calculation of the assigned values of the reference materials. The materials served as suitable reference materials to ascertain the quality control and validation processes for the

Isotopically enriched structural materials in nuclear devices

Energy Technology Data Exchange (ETDEWEB)

Morgan, L.W.G., E-mail: Lee.Morgan@ccfe.ac.uk [CCFE, Culham Science Centre, Abingdon, Oxfordshire OX14 3DB (United Kingdom); Shimwell, J. [CCFE, Culham Science Centre, Abingdon, Oxfordshire OX14 3DB (United Kingdom); Department of Physics and Astronomy, University of Sheffield, Hicks Building, Hounsfield Road, Sheffield S3 7RH (United Kingdom); Gilbert, M.R. [CCFE, Culham Science Centre, Abingdon, Oxfordshire OX14 3DB (United Kingdom)

2015-01-15

Highlights: • C-B analysis of isotopic enrichment of structural materials is presented. • Some, previously, prohibited elements could be used as alloying elements in LAM's. • Adding enriched molybdenum and nickel, to EUROFER, could increase availability. • Isotope enrichment for EUROFER could be cost-effective. • Isotopically enriching copper, in CuCrZr, can reduce helium production by 50%. - Abstract: A large number of materials exist which have been labeled as low activation structural materials (LAM). Most often, these materials have been designed in order to substitute-out or completely remove elements that become activated and contribute significantly to shut-down activity after being irradiated by neutrons in a reactor environment. To date, one of the fundamental principles from which LAMs have been developed is that natural elemental compositions are the building blocks of LAMs. Thus, elements such as Co, Al, Ni, Mo, Nb, N and Cu that produce long-lived decay products are significantly reduced or removed from the LAM composition. These elements have an important part to play in the composition of steels and the removal/substitution can have a negative impact on materials properties such as yield stress and fracture toughness. This paper looks in more detail at whether using isotopic selection of the more mechanically desirable, but prohibited due to activation, elements can improve matters. In particular, this paper focuses on the activation of Eurofer. Carefully chosen isotopically enriched elements, which are normally considered to be on the prohibited element list, are added to EUROFER steel as potential alloying elements. The EUROFER activation results show that some prohibited elements can be used as alloying elements in LAM steels, providing the selected isotopes do not have a significant impact on waste disposal rating or shut-down dose. The economic implications of isotopically enriching elements and the potential implications for

230Th-234U Model-Ages of Some Uranium Standard Reference Materials

International Nuclear Information System (INIS)

Williams, R.W.; Gaffney, A.M.; Kristo, M.J.; Hutcheon, I.D.

2009-01-01

The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the 230 Th- 234 U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumption of the initial 230 Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U 3 O 8 ) may be assumed with confidence. We present here 230 Th- 234 U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history

Halogens determination in vegetable NBS standard reference materials

International Nuclear Information System (INIS)

Stella, R.; Genova, N.; Di Casa, M.

1977-01-01

Levels of all four halogens in Orchard Leaves, Pine Needles and Tomato Leaves NBS reference standards were determined. For fluorine a spiking isotope dilution method was used followed by HF absorption on glass beads. Instrumental nuclear activation analysis was adopted for chlorine and bromine determination. Radiochemical separation by a distillation procedure was necessary for iodine nuclear activation analysis after irradiation. Activation parameters of Cl, Br and I are reported. Results of five determinations for each halogen in Orchard Leaves, Pine Needles and Tomato Leaves NBS Standard Materials and Standard deviations of the mean are reported. (T.I.)

Nuclear measurements and reference materials annual progress report, january - december 1988

International Nuclear Information System (INIS)

1989-01-01

The 1988 progress report of the Central Bureau for Nuclear Measurements (CBNM) is presented. The major changes in the role and orientation of the Joint Research Center, of which CBNM is an institute, are included. The main tasks of CBNM, which involve the program on Nuclear Measurements and Reference Materials, are given. Technical activities concerning the GELINA electron beam and Van de Graaff accelerators are reported. The study of transition radiation at linear electron accelerators, and the development of isotope dilution mass spectrometry, for trace analysis and isotope abundance measurements in iron and gallium, are summarized. The scientific and technical support to the commission, work for third parties, and contribution to conferences are presented

A new organic reference material, l-glutamic acid, USGS41a, for δ(13) C and δ(15) N measurements - a replacement for USGS41.

Science.gov (United States)

Qi, Haiping; Coplen, Tyler B; Mroczkowski, Stanley J; Brand, Willi A; Brandes, Lauren; Geilmann, Heike; Schimmelmann, Arndt

2016-04-15

The widely used l-glutamic acid isotopic reference material USGS41, enriched in both (13) C and (15) N, is nearly exhausted. A new material, USGS41a, has been prepared as a replacement for USGS41. USGS41a was prepared by dissolving analytical grade l-glutamic acid enriched in (13) C and (15) N together with l-glutamic acid of normal isotopic composition. The δ(13) C and δ(15) N values of USGS41a were directly or indirectly normalized with the international reference materials NBS 19 calcium carbonate (δ(13) CVPDB = +1.95 mUr, where milliurey = 0.001 = 1 ‰), LSVEC lithium carbonate (δ(13) CVPDB = -46.6 mUr), and IAEA-N-1 ammonium sulfate (δ(15) NAir = +0.43 mUr) and USGS32 potassium nitrate (δ(15) N = +180 mUr exactly) by on-line combustion, continuous-flow isotope-ratio mass spectrometry, and off-line dual-inlet isotope-ratio mass spectrometry. USGS41a is isotopically homogeneous; the reproducibility of δ(13) C and δ(15) N is better than 0.07 mUr and 0.09 mUr, respectively, in 200-μg amounts. It has a δ(13) C value of +36.55 mUr relative to VPDB and a δ(15) N value of +47.55 mUr relative to N2 in air. USGS41 was found to be hydroscopic, probably due to the presence of pyroglutamic acid. Experimental results indicate that the chemical purity of USGS41a is substantially better than that of USGS41. The new isotopic reference material USGS41a can be used with USGS40 (having a δ(13) CVPDB value of -26.39 mUr and a δ(15) NAir value of -4.52 mUr) for (i) analyzing local laboratory isotopic reference materials, and (ii) quantifying drift with time, mass-dependent isotopic fractionation, and isotope-ratio-scale contraction for isotopic analysis of biological and organic materials. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

NKS-Norcmass reference material for analysis of Pu-isotopes and 237Np by mass spectrometry

International Nuclear Information System (INIS)

Ross, P.; Nygren, U.; Appelblad, P.; Skipperud, L.; Sjoegren, A.

2006-04-01

The aim of the reference material in the Norcmass-project was to produce a low-level ( 239 Pu) sample of sufficient amount to allow individual laboratories to perform several tests without risk of using up the material. Although there are several reference materials available (eg IAEA) few have 239 Pu/ 240 Pu data and almost none have 237 Np/ 239 Pu-data. Those who have (eg IAEA-384) have very high concentrations and are not useful for testing analytical methods designed for low-level measurements where a large sample mass may be required. The reference material consist of the top 10cm of 2mm sieved soil pooled together from 12 different Danish locations collected during 2003. The Soil was blended and sieved through 0.6 and finally through a 0.4 mm sieve. A total amount of 17 kg soil was produced. Several aliquots of the material was subject to analysis by alpha spectrometry and ICP-MS. The material contain 239 + 240 Pu at a concentration of 0.24 ± 0.01 mBq/g and a 240 Pu/ 239 Pu atom ratio of 0.19 ± 0.006. The ratio 237 Np/ 239 Pu was determined to 0.32 ± 0.01. (au)

A new basaltic glass microanalytical reference material for multiple techniques

Science.gov (United States)

Wilson, Steve; Koenig, Alan; Lowers, Heather

2012-01-01

The U.S. Geological Survey (USGS) has been producing reference materials since the 1950s. Over 50 materials have been developed to cover bulk rock, sediment, and soils for the geological community. These materials are used globally in geochemistry, environmental, and analytical laboratories that perform bulk chemistry and/or microanalysis for instrument calibration and quality assurance testing. To answer the growing demand for higher spatial resolution and sensitivity, there is a need to create a new generation of microanalytical reference materials suitable for a variety of techniques, such as scanning electron microscopy/X-ray spectrometry (SEM/EDS), electron probe microanalysis (EPMA), laser ablation inductively coupled mass spectrometry (LA-ICP-MS), and secondary ion mass spectrometry (SIMS). As such, the microanalytical reference material (MRM) needs to be stable under the beam, be homogeneous at scales of better than 10–25 micrometers for the major to ultra-trace element level, and contain all of the analytes (elements or isotopes) of interest. Previous development of basaltic glasses intended for LA-ICP-MS has resulted in a synthetic basaltic matrix series of glasses (USGS GS-series) and a natural basalt series of glasses (BCR-1G, BHVO-2G, and NKT-1G). These materials have been useful for the LA-ICP-MS community but were not originally intended for use by the electron or ion beam community. A material developed from start to finish with intended use in multiple microanalytical instruments would be useful for inter-laboratory and inter-instrument platform comparisons. This article summarizes the experiments undertaken to produce a basalt glass reference material suitable for distribution as a multiple-technique round robin material. The goal of the analytical work presented here is to demonstrate that the elemental homogeneity of the new glass is acceptable for its use as a reference material. Because the round robin exercise is still underway, only

Substoichiometric isotope dilution analysis of arsenic in biological and environmental standard reference materials by solvent extraction using toluene-3,4-dithiol in benzene

International Nuclear Information System (INIS)

Chutke, N.L.; Ambulkar, Ms.M.N.; Weginwar, R.G.; Garg, A.N.

1994-01-01

A radiochemical solvent extraction procedure has been developed for the determination of As(III) using 76 As tracer. It is based on the complexation of As(III) with toluene-3,4-dithiol (TDT) at pH 2 and subsequent extraction in benzene. The effect of various parameters such as pH, time of equilibration, nature of solvent, quantitative character and interferences have been studied. The method has been further developed into substoichiometric isotope dilution analysis for the determination of As at < 1μg level and employed for the analysis of several environmental and biological standard Reference Materials from NIST (USA), IAEA (Vienna) and NIES (Japan). (author) 39 refs.; 4 figs.; 4 tabs

A new organic reference material, L-glutamic acid, USGS41a, for δ13C and δ15N measurements − a replacement for USGS41

Science.gov (United States)

Qi, Haiping; Coplen, Tyler B.; Mroczkowski, Stanley J.; Brand, Willi A.; Brandes, Lauren; Geilmann, Heike; Schimmelmann, Arndt

2016-01-01

RationaleThe widely used l-glutamic acid isotopic reference material USGS41, enriched in both 13C and 15N, is nearly exhausted. A new material, USGS41a, has been prepared as a replacement for USGS41.MethodsUSGS41a was prepared by dissolving analytical grade l-glutamic acid enriched in 13C and 15N together with l-glutamic acid of normal isotopic composition. The δ13C and δ15N values of USGS41a were directly or indirectly normalized with the international reference materials NBS 19 calcium carbonate (δ13CVPDB = +1.95 mUr, where milliurey = 0.001 = 1 ‰), LSVEC lithium carbonate (δ13CVPDB = −46.6 mUr), and IAEA-N-1 ammonium sulfate (δ15NAir = +0.43 mUr) and USGS32 potassium nitrate (δ15N = +180 mUr exactly) by on-line combustion, continuous-flow isotope-ratio mass spectrometry, and off-line dual-inlet isotope-ratio mass spectrometry.ResultsUSGS41a is isotopically homogeneous; the reproducibility of δ13C and δ15N is better than 0.07 mUr and 0.09 mUr, respectively, in 200-μg amounts. It has a δ13C value of +36.55 mUr relative to VPDB and a δ15N value of +47.55 mUr relative to N2 in air. USGS41 was found to be hydroscopic, probably due to the presence of pyroglutamic acid. Experimental results indicate that the chemical purity of USGS41a is substantially better than that of USGS41.ConclusionsThe new isotopic reference material USGS41a can be used with USGS40 (having a δ13CVPDB value of −26.39 mUr and a δ15NAir value of −4.52 mUr) for (i) analyzing local laboratory isotopic reference materials, and (ii) quantifying drift with time, mass-dependent isotopic fractionation, and isotope-ratio-scale contraction for isotopic analysis of biological and organic materials. Published in 2016. This article is a U.S. Government work and is in the public domain in the USA.

230Th-234U Model-Ages of Some Uranium Standard Reference Materials

Energy Technology Data Exchange (ETDEWEB)

Williams, R W; Gaffney, A M; Kristo, M J; Hutcheon, I D

2009-05-28

The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the {sup 230}Th-{sup 234}U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumption of the initial {sup 230}Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U{sub 3}O{sub 8}) may be assumed with confidence. We present here {sup 230}Th-{sup 234}U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history.

Preparation and characterization of the fish reference material; Preparacao e caracterizacao de um material de referencia de peixe

Energy Technology Data Exchange (ETDEWEB)

Ulrich, Joao Cristiano

2011-07-01

The certified reference materials (CRMs) play an important role in obtaining measurement results traceable to the International System of Units, through an unbroken chain of comparisons. Thus, the demand for new certified reference materials (CRMs) increases every day in all areas of knowledge. The availability of reference materials, mainly in Brazil is still incipient, given that the demand far exceeds the available variety of these materials. The amount of certified reference materials available in the country is insufficient to meet the need of the scientific community and demands for development of new methodologies. Among the many areas in need of reference materials, we highlight the importance for the food trade balance for these products within the country. The certification of food products, intended both for export and for domestic consumption, requires analysis methods that provide precise and accurate results to ensure product quality. This paper describes the preparation and certification of a reference material in the fish matrix in mercury and methylmercury. The study brings together since the stage of material selection, preparation, development of homogeneity and stability studies and characterization. The certification was performed by means of measurements using two analytical techniques, flow injection analysis - cold vapor atomic absorption spectrometry (FIA-CV-AAS) and isotope dilution applied to mass spectrometry (IDMS), which is a primary method. In this work the standards of the ISO 30 (ABNT 30-34) and ISO Guide 35 was used as the basis for the preparation and characterization of the material. For the calculation of uncertainties was used the GUM and Eurachem guide. As a result, was produced and certified a lot of material in relation to the concentration of mercury (Hg = 0.271 {+-} 0.057 mg g{sup -1}) and methylmercury (MeHg = 0.245 {+-} 0.038 mg g{sup -1}), and informational values of lead and arsenic. (author)

Two new organic reference materials for δ13C and δ15N measurements and a new value for the δ13C of NBS 22 oil

Science.gov (United States)

Qi, Haiping; Coplen, Tyler B.; Geilmann, Heike; Brand, Willi A.; Böhlke, J.K.

2003-01-01

Analytical grade L-glutamic acid is chemically stable and has a C/N mole ratio of 5, which is close to that of many of natural biological materials, such as blood and animal tissue. Two L-glutamic acid reference materials with substantially different 13C and 15N abundances have been prepared for use as organic reference materials for C and N isotopic measurements. USGS40 is analytical grade L-glutamic acid and has a δ13C value of −26.24‰ relative to VPDB and a δ15N value of −4.52‰ relative to N2 in air. USGS41 was prepared by dissolving analytical grade L-glutamic acid with L-glutamic acid enriched in 13C and 15N. USGS41 has a δ13C value of +37.76‰ and a δ15N value of +47.57‰. The δ13C and δ15N values of both materials were measured against the international reference materials NBS 19 calcium carbonate (δ13C = +1.95‰), L-SVEC lithium carbonate (δ13C = −46.48‰), IAEA-N-1 ammonium sulfate (δ15N = 0.43‰), and USGS32 potassium nitrate (δ15N = 180‰) by on-line combustion continuous-flow and off-line dual-inlet isotope-ratio mass spectrometry. Both USGS40 and USGS41 are isotopically homogeneous; reproducibility of δ13C is better than 0.13‰, and that of δ15N is better than 0.13‰ in 100-μg amounts. These two isotopic reference materials can be used for (i) calibrating local laboratory reference materials, and (ii) quantifying drift with time, mass-dependent fractionations, and isotope-ratio-scale contraction in the isotopic analysis of various biological materials. Isotopic results presented in this paper yield a δ13C value for NBS 22 oil of −29.91‰, in contrast to the commonly accepted value of −29.78‰ for which off-line blank corrections probably have not been quantified satisfactorily.

Present status and future plans of the study for preparation of Pu reference materials

International Nuclear Information System (INIS)

Sumi, Mika; Kageyama, Tomio; Suzuki, Toru

2007-01-01

All accountancy analysis at the Plutonium Fuel Development Center of JAEA is performed by isotope dilution mass spectrometry with well-characterized standard materials. Though Pu reference materials has been supplied from foreign country, importing those Pu materials is gradually becoming more difficult and may be almost impossible to import them in future. Thus, in order to establish the capability and expertise for the preparation of Pu reference materials, JAEA has started collaborative work with NBL who has high skills for preparing and supplying nuclear reference materials for long periods. One of the targets of this collaboration is preparation of standard material for IDMS (LSD spike). MOX powder which has been stored in JAEA was dissolved and Purified to obtain Pu solution. A small portion of the Purified solution was transported to NBL for analysis. LSD spike will be prepared from this Pu solution and then validation analysis and performance test including stability test will be performed with NBL and JAEA. This report presents status and future plans for the collaboration work. (author)

Increasing the Accuracy in the Measurement of the Minor Isotopes of Uranium: Care in Selection of Reference Materials, Baselines and Detector Calibration

Science.gov (United States)

Poths, J.; Koepf, A.; Boulyga, S. F.

2008-12-01

The minor isotopes of uranium (U-233, U-234, U-236) are increasingly useful for tracing a variety of processes: movement of anthropogenic nuclides in the environment (ref 1), sources of uranium ores (ref 2), and nuclear material attribution (ref 3). We report on improved accuracy for U-234/238 and U-236/238 by supplementing total evaporation protocol TIMS measurement on Faraday detectors (ref 4)with multiplier measurement for the minor isotopes. Measurement of small signals on Faraday detectors alone is limited by noise floors of the amplifiers and accurate measurement of the baseline offsets. The combined detector approach improves the reproducibility to better than ±1% (relative) for the U-234/238 at natural abundance, and yields a detection limit for U-236/U-238 of <0.2 ppm. We have quantified contribution of different factors to the uncertainties associated with these peak jumping measurement on a single detector, with an aim of further improvement. The uncertainties in the certified values for U-234 and U-236 in the uranium standard NBS U005, if used for mass bias correction, dominates the uncertainty in their isotopic ratio measurements. Software limitations in baseline measurement drives the detection limit for the U-236/U-238 ratio. This is a topic for discussion with the instrument manufacturers. Finally, deviation from linearity of the response of the electron multiplier with count rate limits the accuracy and reproducibility of these minor isotope measurements. References: (1) P. Steier et al(2008) Nuc Inst Meth(B), 266, 2246-2250. (2) E. Keegan et al (2008) Appl Geochem 23, 765-777. (3) K. Mayer et al (1998) IAEA-CN-98/11, in Advances in Destructive and Non-destructive Analysis for Environmental Monitoring and Nuclear Forensics. (4) S. Richter and S. Goldberg(2003) Int J Mass Spectrom, 229, 181-197.

Reference material manufacture and certification for the AVNG

Energy Technology Data Exchange (ETDEWEB)

Hauck, Danielle K [Los Alamos National Laboratory; Thron, Jonathan [Los Alamos National Laboratory; MacArthur, Duncan W. [Los Alamos National Laboratory; Livke, Alexander [RFNC - VNIIEF; Bulatov, M [RFNC-VNIIEF; Kondratov, Sergey [RFNC-VNIIEF; Leplyavkina, M [RFNC-VNIIEF; Razinkov, Sergey [RFNC-VNIIEF; Sivachev, D [RFNC-VNIIEF; Tsybryaev, S [RFNC-VNIIEF; V' yushin, A [RFNC-VNIIEF

2010-07-09

Testing and demonstration of any radiation measurement system requires the use of appropriate radioactive sources. An attribute measurement system (A VNG) was developed and fabricated at the Russian Federal Nuclear Center, VNIIEF, Russia, under contract with LANL, USA. The A VNG detects neutron and gamma radiation signatures and compares the data analysis results with the specified threshold values for three unclassified attributes; plutonium is present or absent, plutonium mass is greater than or less than the specified threshold value and plutonium isotopic ratio ²⁴⁰Pu to ²³⁹Pu) is greater than or less then the threshold value. A set of reference materials (RMs) was specially manufactured for the A VNG with masses and isotopic ratios above and below the selected thresholds. The set of RMs was certified in compliance with the Russian metrological requirements. The RMs were used to debug and test the A VNG and to demonstrate the A VNG operation to an American delegation in June 2009. In this presentation, we will describe the various steps in the manufacture and certification of these RM sources.

Reference material manufacture and certification for the AVNG

Energy Technology Data Exchange (ETDEWEB)

Hauck, Danielle K [Los Alamos National Laboratory; Mac Arthur, Duncan [Los Alamos National Laboratory; Thron, Jonathan L [Los Alamos National Laboratory; Livke, Alexander [VNIIEF; Kondratov, Sergey [VNIIEF; Razinkov, Sergey [VNIIEF

2010-01-01

Testing and demonstration of any radiation measurement system requires the use of appropriate radioactive sources. The AVNG implementation that we describe is an attribute measurement system built by RFNC - VNIIEF in Sarov, Russia. The AVNG detects neutron and gamma radiation signatures and displays the three unclassified attributes of 'plutonium presence,' 'plutonium mass > 2 kg,' and 'plutonium isotopic ratio ({sup 240}Pu to {sup 239}Pu) < 0.1.' The AVNG was tested using a number of reference material (RM) sources with masses and isotopic ratios above and below these thresholds. The AVNG was demonstrated in June 2009 using several of these sources in addition to detector calibration sources. Since the AVNG was designed to measure multi-kg plutonium sources, the RM was manufactured specifically for use with this system. In addition, the RM was used to test the thresholds in the AVNG, so the size and composition of each RM was certified prior to use. In this presentation, we will describe the various steps in the manufacture and certification of these RM sources.

Reference material manufacture and certification for the AVNG

International Nuclear Information System (INIS)

2010-01-01

Testing and demonstration of any radiation measurement system requires the use of appropriate radioactive sources. An attribute measurement system (A VNG) was developed and fabricated at the Russian Federal Nuclear Center, VNIIEF, Russia, under contract with LANL, USA. The A VNG detects neutron and gamma radiation signatures and compares the data analysis results with the specified threshold values for three unclassified attributes; plutonium is present or absent, plutonium mass is greater than or less than the specified threshold value and plutonium isotopic ratio 240 Pu to 239 Pu) is greater than or less then the threshold value. A set of reference materials (RMs) was specially manufactured for the A VNG with masses and isotopic ratios above and below the selected thresholds. The set of RMs was certified in compliance with the Russian metrological requirements. The RMs were used to debug and test the A VNG and to demonstrate the A VNG operation to an American delegation in June 2009. In this presentation, we will describe the various steps in the manufacture and certification of these RM sources.

REFERENCE MATERIALS SYSTEM OF SCIENTIFIC METHODICAL CENTRE OF STATE SERVICE OF REFERENCE MATERIALS FOR COMPOSITION AND PROPERTIES OF SUBSTANCES AND MATERIALS URAL RESEARCH INSTITUTE FOR METROLOGY

Directory of Open Access Journals (Sweden)

E. V. Osinseva

2015-01-01

Full Text Available Since 1960s UNIIM performs research in the field of needs in reference materials of composition and properties of substances and materials (RM as well as develops it. During the research UNIIM has developed 757 types of RMs for metrological measurement assurance of factors of composition and properties of substance and materials for test laboratories of chemical, pharmaceutical, fuel, food industry, agriculture, metallurgy and ecological monitoring laboratories. List ofRMs enlarges thanks to development of UNIIM standards and transmission measurement facility from State standards of units. Taking into account the actual requirements in the field of measurements, the UNIIM's key destination is to assure the accuracy and the metrological traceability of measurements. The present-day system of RMs to be developed in UNIIM includes RMs of composition of inorganic and organic compounds and their solutions, fuels, stable isotopic materials, water, grounds, food products, biomaterials, nanomaterials, metals, alloys and other materials offerrous and non-ferrous industry, RMs of properties (thermodynamic, magnetic, physical-chemical, technical of substances and materials. The present article considers history of RMs list development which were created by UNIIM and the strategy of this direction.

Hot vacuum extraction-isotopic dilution mass spectrometry for determination of hydrogen isotopes in zircaloys

International Nuclear Information System (INIS)

Shi, Y.; Leeson, P.K.; Wilkin, D.; Britton, A.; Macleod, R.

2016-01-01

A hot vacuum extraction-isotope dilution mass spectrometry (HVE-IDMS) was studied for determination of hydrogen isotopes in zirconium metal and alloys as nuclear reactor materials. A theoretical assessment of the completeness of the extraction of hydrogen isotopes under the chosen condition was carried out based on the hydrogen and deuterium solubility data for zirconium. The optimal isotopic spiking condition for conventional IDMS was further explored for the special case IDMS where the isotope abundance of the samples is varied and non-natural. Applying the optimal conditions, the accurate IDMS determination was realized. The agreement between the measured values and the certified or prepared values of standard reference materials and homemade standard materials validate the method developed. (author)

Preparation and certification of Re-Os dating reference materials: Molybdenites HLP and JDC

Science.gov (United States)

Du, A.; Wu, S.; Sun, D.; Wang, Shaoming; Qu, W.; Markey, R.; Stain, H.; Morgan, J.; Malinovskiy, D.

2004-01-01

Two Re-Os dating reference material molybdenites were prepared. Molybdenite JDC and molybdenite HLP are from a carbonate vein-type molybdenum-(lead)- uranium deposit in the Jinduicheng-Huanglongpu area of Shaanxi province, China. The samples proved to be homogeneous, based on the coefficient of variation of analytical results and an analysis of variance test. The sampling weight was 0.1 g for JDC and 0.025 g for HLP. An isotope dilution method was used for the determination of Re and Os. Sample decomposition and preconcentration of Re and Os prior to measurement were accomplished using a variety of methods: acid digestion, alkali fusion, ion exchange and solvent extraction. Negative thermal ionisation mass spectrometry and inductively coupled plasma-mass spectrometry were used for the determination of Re and 187Os concentration and isotope ratios. The certified values include the contents of Re and Os and the model ages. For HLP, the Re content was 283.8 ?? 6.2 ??g g-1, 187Os was 659 ?? 14 ng g-1 and the Re-Os model age was 221.4 ?? 5.6 Ma. For JDC, the Re content was 17.39 ?? 0.32 ng g-1, 187Os was 25.46 ?? 0.60 ng g-1 and the Re-Os model age was 139.6 ?? 3.8 Ma. Uncertainties for both certified reference materials are stated at the 95% level of confidence. Three laboratories (from three countries: P.R. China, USA, Sweden) joined in the certification programme. These certified reference materials are primarily useful for Re-Os dating of molybdenite, sulfides, black shale, etc.

Availability of enriched isotopic material for accelerator targets

International Nuclear Information System (INIS)

Newman, E.

1982-01-01

The electromagnetic isotope enrichment facility at ORNL provides a broad spectrum of highly enriched stable isotopes to the worldwide scientific community. The continued timely availability of these materials is of vital importance in many areas of basic research and, in particular, as source material for the fabrication of accelerator targets. A brief description of the facility and its capabilities and limitations is presented

New biotite and muscovite isotopic reference materials, USGS57 and USGS58, for δ2H measurements–A replacement for NBS 30

Science.gov (United States)

Qi, Haiping; Coplen, Tyler B.; Gehre, Matthias; Vennemann, Torsten W.; Brand, Willi A.; Geilmann, Heike; Olack, Gerard; Bindeman, Ilya N.; Palandri, Jim; Huang, Li; Longstaffe, Fred J.

2017-01-01

The advent of continuous-flow isotope-ratio mass spectrometry (CF-IRMS) coupled with a high temperature conversion (HTC) system enabled faster, more cost effective, and more precise δ2H analysis of hydrogen-bearing solids. Accurate hydrogen isotopic analysis by on-line or off-line techniques requires appropriate isotopic reference materials (RMs). A strategy of two-point calibrations spanning δ2H range of the unknowns using two RMs is recommended. Unfortunately, the supply of the previously widely used isotopic RM, NBS 30 biotite, is exhausted. In addition, recent measurements have shown that the determination of δ2H values of NBS 30 biotite on the VSMOW-SLAP isotope-delta scale by on-line HTC systems with CF-IRMS may be unreliable because hydrogen in this biotite may not be converted quantitatively to molecular hydrogen. The δ2HVSMOW-SLAP values of NBS 30 biotite analyzed by on-line HTC systems can be as much as 21 mUr (or ‰) too positive compared to the accepted value of − 65.7 mUr, determined by only a few conventional off-line measurements. To ensure accurate and traceable on-line hydrogen isotope-ratio determinations in mineral samples, we here propose two isotopically homogeneous, hydrous mineral RMs with well-characterized isotope-ratio values, which are urgently needed. The U.S. Geological Survey (USGS) has prepared two such RMs, USGS57 biotite and USGS58 muscovite. The δ2H values were determined by both glassy carbon-based on-line conversion and chromium-based on-line conversion, and results were confirmed by off-line conversion. The quantitative conversion of hydrogen from the two RMs using the on-line HTC method was carefully evaluated in this study. The isotopic compositions of these new RMs with 1-σ uncertainties and mass fractions of hydrogen are:USGS57 (biotite)δ2HVSMOW-SLAP = − 91.5 ± 2.4 mUr (n = 24)Mass fraction hydrogen = 0.416 ± 0.002% (n = 4)Mass fraction water = 3.74 ± 0.02% (n = 4)USGS58 (muscovite

Quality assurance and quality control in light stable isotope laboratories: A case study of Rio Grande, Texas, water samples

Science.gov (United States)

Coplen, T.B.; Qi, H.

2009-01-01

New isotope laboratories can achieve the goal of reporting the same isotopic composition within analytical uncertainty for the same material analysed decades apart by (1) writing their own acceptance testing procedures and putting them into their mass spectrometric or laser-based isotope-ratio equipment procurement contract, (2) requiring a manufacturer to demonstrate acceptable performance using all sample ports provided with the instrumentation, (3) for each medium to be analysed, prepare two local reference materials substantially different in isotopic composition to encompass the range in isotopic composition expected in the laboratory and calibrated them with isotopic reference materials available from the International Atomic Energy Agency (IAEA) or the US National Institute of Standards and Technology (NIST), (4) using the optimum storage containers (for water samples, sealing in glass ampoules that are sterilised after sealing is satisfactory), (5) interspersing among sample unknowns local laboratory isotopic reference materials daily (internationally distributed isotopic reference materials can be ordered at three-year intervals, and can be used for elemental analyser analyses and other analyses that consume less than 1 mg of material) - this process applies to H, C, N, O, and S isotope ratios, (6) calculating isotopic compositions of unknowns by normalising isotopic data to that of local reference materials, which have been calibrated to internationally distributed isotopic reference materials, (7) reporting results on scales normalised to internationally distributed isotopic reference materials (where they are available) and providing to sample submitters the isotopic compositions of internationally distributed isotopic reference materials of the same substance had they been analysed with unknowns, (8) providing an audit trail in the laboratory for analytical results - this trail commonly will be in electronic format and might include a laboratory

Evaluation of new geological reference materials for uranium-series measurements: Chinese Geological Standard Glasses (CGSG) and macusanite obsidian.

Science.gov (United States)

Denton, J S; Murrell, M T; Goldstein, S J; Nunn, A J; Amato, R S; Hinrichs, K A

2013-10-15

Recent advances in high-resolution, rapid, in situ microanalytical techniques present numerous opportunities for the analytical community, provided accurately characterized reference materials are available. Here, we present multicollector thermal ionization mass spectrometry (MC-TIMS) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) uranium and thorium concentration and isotopic data obtained by isotope dilution for a suite of newly available Chinese Geological Standard Glasses (CGSG) designed for microanalysis. These glasses exhibit a range of compositions including basalt, syenite, andesite, and a soil. Uranium concentrations for these glasses range from ∼2 to 14 μg g(-1), Th/U weight ratios range from ∼4 to 6, (234)U/(238)U activity ratios range from 0.93 to 1.02, and (230)Th/(238)U activity ratios range from 0.98 to 1.12. Uranium and thorium concentration and isotopic data are also presented for a rhyolitic obsidian from Macusani, SE Peru (macusanite). This glass can also be used as a rhyolitic reference material, has a very low Th/U weight ratio (around 0.077), and is approximately in (238)U-(234)U-(230)Th secular equilibrium. The U-Th concentration data agree with but are significantly more precise than those previously measured. U-Th concentration and isotopic data agree within estimated errors for the two measurement techniques, providing validation of the two methods. The large (238)U-(234)U-(230)Th disequilibria for some of the glasses, along with the wide range in their chemical compositions and Th/U ratios should provide useful reference points for the U-series analytical community.

Reference materials and representative test materials: the nanotechnology case

International Nuclear Information System (INIS)

Roebben, G.; Rasmussen, K.; Kestens, V.; Linsinger, T. P. J.; Rauscher, H.; Emons, H.; Stamm, H.

2013-01-01

An increasing number of chemical, physical and biological tests are performed on manufactured nanomaterials for scientific and regulatory purposes. Existing test guidelines and measurement methods are not always directly applicable to or relevant for nanomaterials. Therefore, it is necessary to verify the use of the existing methods with nanomaterials, thereby identifying where modifications are needed, and where new methods need to be developed and validated. Efforts for verification, development and validation of methods as well as quality assurance of (routine) test results significantly benefit from the availability of suitable test and reference materials. This paper provides an overview of the existing types of reference materials and introduces a new class of test materials for which the term ‘representative test material’ is proposed. The three generic concepts of certified reference material, reference material(non-certified) and representative test material constitute a comprehensive system of benchmarks that can be used by all measurement and testing communities, regardless of their specific discipline. This paper illustrates this system with examples from the field of nanomaterials, including reference materials and representative test materials developed at the European Commission’s Joint Research Centre, in particular at the Institute for Reference Materials and Measurements (IRMM), and at the Institute for Health and Consumer Protection (IHCP).

Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material

International Nuclear Information System (INIS)

Hernandez, C.; Fernandez, M.; Quejido, A. L.

2006-01-01

Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound esposure time. Due to the complex matrix of this fly ash material, a two-steps purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs

Nuclear measurements and reference materials

International Nuclear Information System (INIS)

1988-01-01

This report summarizes the progress of the JRC programs on nuclear data, nuclear metrology, nuclear reference materials and non-nuclear reference materials. Budget restrictions and personnel difficulties were encountered during 1987. Fission properties of 235 U as a function of neutron energy and of the resonances can be successfully described on the basis of a three exit channel fission model. Double differential neutron emission cross-sections were accomplished on 7 Li and were started for the tritium production cross-section of 9 Be. Reference materials of uranium minerals and ores were prepared. Special nuclear targets were prepared. A batch of 250 g of Pu0 2 was characterized in view of certification as reference material for the elemental assay of plutonium

Stable isotopes in Lithuanian bioarcheological material

Science.gov (United States)

Skipityte, Raminta; Jankauskas, Rimantas; Remeikis, Vidmantas

2015-04-01

Investigation of bioarcheological material of ancient human populations allows us to understand the subsistence behavior associated with various adaptations to the environment. Feeding habits are essential to the survival and growth of ancient populations. Stable isotope analysis is accepted tool in paleodiet (Schutkowski et al, 1999) and paleoenvironmental (Zernitskaya et al, 2014) studies. However, stable isotopes can be useful not only in investigating human feeding habits but also in describing social and cultural structure of the past populations (Le Huray and Schutkowski, 2005). Only few stable isotope investigations have been performed before in Lithuanian region suggesting a quite uniform diet between males and females and protein intake from freshwater fish and animal protein. Previously, stable isotope analysis has only been used to study a Stone Age population however, more recently studies have been conducted on Iron Age and Late medieval samples (Jacobs et al, 2009). Anyway, there was a need for more precise examination. Stable isotope analysis were performed on human bone collagen and apatite samples in this study. Data represented various ages (from 5-7th cent. to 18th cent.). Stable carbon and nitrogen isotope analysis on medieval populations indicated that individuals in studied sites in Lithuania were almost exclusively consuming C3 plants, C3 fed terrestrial animals, and some freshwater resources. Current investigation demonstrated social differences between elites and country people and is promising in paleodietary and daily life reconstruction. Acknowledgement I thank prof. dr. G. Grupe, Director of the Anthropological and Palaeoanatomical State Collection in Munich for providing the opportunity to work in her laboratory. The part of this work was funded by DAAD. Antanaitis-Jacobs, Indre, et al. "Diet in early Lithuanian prehistory and the new stable isotope evidence." Archaeologia Baltica 12 (2009): 12-30. Le Huray, Jonathan D., and Holger

COMAR - database for certified reference materials

International Nuclear Information System (INIS)

Klich, H.; Caliste, J.P.

1988-01-01

With more than 130 producers of reference materials (RM) throughout the world, it is often difficult to find the best reference material for a specific application. The computer database COMAR has been developed to aid chemists in finding the needed reference material. (orig.)

A combustion setup to precisely reference δ13C and δ2H isotope ratios of pure CH4 to produce isotope reference gases of δ13C-CH4 in synthetic air

Directory of Open Access Journals (Sweden)

H. Schaefer

2012-09-01

Full Text Available Isotope records of atmospheric CH4 can be used to infer changes in the biogeochemistry of CH4. One factor currently limiting the quantitative interpretation of such changes are uncertainties in the isotope measurements stemming from the lack of a unique isotope reference gas, certified for δ13C-CH4 or δ2H-CH4. We present a method to produce isotope reference gases for CH4 in synthetic air that are precisely anchored to the VPDB and VSMOW scales and have δ13C-CH4 values typical for the modern and glacial atmosphere. We quantitatively combusted two pure CH4 gases from fossil and biogenic sources and determined the δ13C and δ2H values of the produced CO2 and H2O relative to the VPDB and VSMOW scales within a very small analytical uncertainty of 0.04‰ and 0.7‰, respectively. We found isotope ratios of −39.56‰ and −56.37‰ for δ13C and −170.1‰ and −317.4‰ for δ2H in the fossil and biogenic CH4, respectively. We used both CH4 types as parental gases from which we mixed two filial CH4 gases. Their δ13C was determined to be −42.21‰ and −47.25‰ representing glacial and present atmospheric δ13C-CH4. The δ2H isotope ratios of the filial CH4 gases were found to be −193.1‰ and −237.1‰, respectively. Next, we mixed aliquots of the filial CH4 gases with ultrapure N2/O2 (CH4 ≤ 2 ppb producing two isotope reference gases of synthetic air with CH4 mixing ratios near atmospheric values. We show that our method is reproducible and does not introduce isotopic fractionation for δ13C within the uncertainties of our detection limit (we cannot conclude this for δ2H because our system is currently not prepared for δ2H-CH4 measurements in air samples. The general principle of our method can be applied to produce synthetic isotope reference gases targeting δ2H-CH4 or other gas species.

On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

Science.gov (United States)

Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

2014-12-03

We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

Criticality reference benchmark calculations for burnup credit using spent fuel isotopics

International Nuclear Information System (INIS)

Bowman, S.M.

1991-04-01

To date, criticality analyses performed in support of the certification of spent fuel casks in the United States do not take credit for the reactivity reduction that results from burnup. By taking credit for the fuel burnup, commonly referred to as ''burnup credit,'' the fuel loading capacity of these casks can be increased. One of the difficulties in implementing burnup credit in criticality analyses is that there have been no critical experiments performed with spent fuel which can be used for computer code validation. In lieu of that, a reference problem set of fresh fuel critical experiments which model various conditions typical of light water reactor (LWR) transportation and storage casks has been identified and used in the validation of SCALE-4. This report documents the use of this same problem set to perform spent fuel criticality benchmark calculations by replacing the actual fresh fuel isotopics from the experiments with six different sets of calculated spent fuel isotopics. The SCALE-4 modules SAS2H and CSAS4 were used to perform the analyses. These calculations do not model actual critical experiments. The calculated k-effectives are not supposed to equal unity and will vary depending on the initial enrichment and burnup of the calculated spent fuel isotopics. 12 refs., 11 tabs

Isotope ratios of strontium and neodymium for characterizing earth mantle materials

International Nuclear Information System (INIS)

Brandt, S.B.; Lepin, V.S.; Maslovskaja, M.N.

1985-01-01

It is shown that the shares of mantle, crustal and sedimentary materials in rocks and ore deposits can be determined by isotope methods. Using Yakutian kimberlites as an example, mixing processes of mantle and crustal materials are illustrated with the aid of strontium isotopes. Due to the high sensitivity of strontium to hydrothermal effects, the combined use of neodymium and strontium isotopes is considered more appropriate to solve the problem of determining the share of mantle materials. This is demonstrated for rare earth minerals and alkaline rocks of Eastern Siberia and Mongolia. (author)

Development of Separation Materials Containing Palladium for Hydrogen Isotopes Separation

International Nuclear Information System (INIS)

Deng Xiaojun; Luo Deli; Qian Xiaojing

2010-01-01

Displacement chromatography (DC) is a ascendant technique for hydrogen isotopes separation. The performance of separation materials is a key factor to determine the separation effect of DC. At present,kinds of materials are researched, including palladium materials and non-palladium materials. It is hardly replaceable because of its excellent separation performance, although palladium is expensive. The theory of hydrogen isotopes separation using DC was introduced at a brief manner, while several palladium separation materials were expatiated in detail(Pd/K, Pd-Al 2 O 3 , Pd-Pt alloy). Development direction of separation materials for DC was forecasted elementarily. (authors)

Isotope specific arbitrary material flow meter

Science.gov (United States)

Barty, Christopher P. J.; Post, John C.; Jones, Edwin

2016-10-25

A laser-based mono-energetic gamma-ray source is used to provide non-destructive and non-intrusive, quantitative determination of the absolute amount of a specific isotope contained within pipe as part of a moving fluid or quasi-fluid material stream.

Characterization of a new candidate isotopic reference material for natural Pb using primary measurement method.

Science.gov (United States)

Nonose, Naoko; Suzuki, Toshihiro; Shin, Ki-Cheol; Miura, Tsutomu; Hioki, Akiharu

2017-06-29

A lead isotopic standard solution with natural abundance has been developed by applying a mixture of a solution of enriched 208 Pb and a solution of enriched 204 Pb ( 208 Pb- 204 Pb double spike solution) as bracketing method. The amount-of-substance ratio of 208 Pb: 204 Pb in this solution is accurately measured by applying EDTA titrimetry, which is one of the primary measurement methods, to each enriched Pb isotope solution. Also metal impurities affecting EDTA titration and minor lead isotopes contained in each enriched Pb isotope solution are quantified by ICP-SF-MS. The amount-of-substance ratio of 208 Pb: 204 Pb in the 208 Pb- 204 Pb double spike solution is 0.961959 ± 0.000056 (combined standard uncertainty; k = 1). Both the measurement of lead isotope ratios in a candidate isotopic standard solution and the correction of mass discrimination in MC-ICP-MS are carried out by coupling of a bracketing method with the 208 Pb- 204 Pb double spike solution and a thallium internal addition method, where thallium solution is added to the standard and the sample. The measured lead isotope ratios and their expanded uncertainties (k = 2) in the candidate isotopic standard solution are 18.0900 ± 0.0046 for 206 Pb: 204 Pb, 15.6278 ± 0.0036 for 207 Pb: 204 Pb, 38.0626 ± 0.0089 for 208 Pb: 204 Pb, 2.104406 ± 0.00013 for 208 Pb: 206 Pb, and 0.863888 ± 0.000036 for 207 Pb: 206 Pb. The expanded uncertainties are about one half of the stated uncertainty for NIST SRM 981, for 208 Pb: 204 Pb, 207 Pb: 204 Pb and 206 Pb: 204 Pb, or one eighth, for 208 Pb: 206 Pb and 207 Pb: 206 Pb, The combined uncertainty consists of the uncertainties due to lead isotope ratio measurements and the remaining time-drift effect of mass discrimination in MC-ICP-MS, which is not removed by the coupled correction method. In the measurement of 208 Pb: 204 Pb, 207 Pb: 204 Pb and 206 Pb: 204 Pb, the latter contribution is two or three times larger than the former. When the coupling of

Room temperature Sieving of Hydrogen Isotopes Using 2-D Materials

Energy Technology Data Exchange (ETDEWEB)

Hitchcock, D. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Colon-Mercado, H. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Krentz, T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Serkiz, S. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Velten, J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Xiao, S. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2017-09-28

Hydrogen isotope separation is critical to the DOE’s mission in environmental remediation and nuclear nonproliferation. Isotope separation is also a critical technology for the NNSA, and the ability to perform the separations at room temperature with a relatively small amount of power and space would be a major advancement for their respective missions. Recent work has shown that 2-D materials such as graphene and hexagonal boron nitride can act as an isotopic sieve at room temperature; efficiently separating hydrogen isotopes in water with reported separation ratios of 10:1 for hydrogen: deuterium separation for a single pass. The work performed here suggests that this technique has merit, and furthermore, we are investigating optimization and scale up of the required 2-D material based membranes.

A routine chromium determination in biological materials; application to various reference materials and standard reference materials

International Nuclear Information System (INIS)

Tjioe, P.S.; Goeij, J.J.M. de; Volkers, K.J.

1979-01-01

The determination limit under standard working conditions of chromium in biological materials is discussed. Neutron activation analysis and atomic spectrometry have been described for some analytical experiences with NBS SRM 1577 reference material. The chromium determination is a part of a larger multi-element scheme for the determination of 12 elements in biological materials

High accuracy determination of trace elements in NIST standard reference materials by isotope dilution ICP-MS

International Nuclear Information System (INIS)

Paulsen, P.J.; Beary, E.S.

1996-01-01

At NIST (National Institute of Standards and Technology), ICP-MS ID (inductively coupled mass spectrometry isotope dilution) has been used to certify a wide range of elements in a variety of materials with high accuracy. Both the chemical preparation and instrumental procedures are simpler than with other ID mass spectrometric techniques. The ICP-MS has picogram/ml detection limits for most elements using fixed operating parameters. Chemical separations are required only to remove an interference (from molecular ions as well as isobaric atoms), or to pre-concentrate the analyte. For example, chemical separations were required for the analysis of SRM 2711, Montana II Soil, but not for boron in peach leaves, SRM 1547.(3 refs., 3 tabs., 2 figs

Preparation of plant-specific NDA reference material

International Nuclear Information System (INIS)

Abedin-Zadeh, R.; Beetle, T.; Kuhn, E.; Terrey, D.; Turel, S.; Busca, G.; Guardini, S.

1983-01-01

The importance of having suitable and well characterized non-destructive assay (NDA) reference materials for the verification activities of the safeguards control authorities is stressed. The Euratom Inspectorate and the IAEA have initiated an extensive programme for the procurement and preparation of Joint Euratom/IAEA safeguards NDA reference materials with the active participation of the Ispra Establishment of the Euratom Joint Research Centre. The different type and nature of materials, condition of measurements, and plant characteristics and provisions had to be taken into account for plant-specific NDA reference materials. The preparation of each reference material was planned case by case and specific criteria such as limitations in different facilities, measurement capabilities, conditions, product availability and population variability are being ascertained. A procurement scheme was prepared describing step-by-step procedures detailing responsibilities, measurement conditions, destructive analysis schemes, desired characteristics and methods of data evaluation. This paper describes the principles and procedures carried out for the preparation of a reference MOX pin, low enriched uranium reference rods, low enriched uranium reference drums, reference MTR assemblies, and THTR reference pebbles. The scheme for each characterization technique is presented. (author)

NBS activities in biological reference materials

Energy Technology Data Exchange (ETDEWEB)

Rasberry, S.D.

1988-12-01

NBS activities in biological reference materials during 1986-1988 are described with a preview of plans for future certifications of reference materials. During the period, work has been completed or partially completed on about 40 reference materials of importance to health, nutrition, and environmental quality. Some of the reference materials that have been completed during the period and are described include: creatinine (SRM 914a), bovine serum albumin (SRM 927a), cholesterol in human serum (SRM's 1951-1952), aspartate aminotransferase (RM 8430), cholesterol and fat-soluble vitamins in coconut oil (SRM 1563), wheat flour (SRM 1567a), rice flour (SRM 1568a), mixed diet (RM 8431a), dinitropyrene isomers and 1-nitropyrene (SRM 1596), and complex PAH's from coal tar (SRM 1597). Oyster tissue (SRM 1566a) is being analyzed and should be available in 1988.

Reference material systems: a sourcebook for material assessment

Energy Technology Data Exchange (ETDEWEB)

Bhagat, N. (ed.)

1976-12-01

A reference set of data related to material systems and a framework for carrying out the material technologies assessment are presented. While the bulk of renewables have been considered in this report, the nonrenewable materials dealt with here include structural materials only, such as steel, aluminum, cement and concrete, and bricks. The complete data set is supposed to include material flows, energy requirements, capital and labor inputs, and environmental effects for each process that a resource must go through to become a useful material for an end use. Although effort has been made to obtain as much information as possible, considerable gaps in data, apparent throughout this report, could not be avoided. A new material technology can be evaluated by substituting that technology for appropriate elements of the reference materials system and calculating the net change in material resource, energy, capital and labor requirements, and environmental impacts. This combination of information thus serves as a means of evaluating the potential benefits to be gained by research in various material technologies.

High-Quality Medium-Resolution Gamma-Ray Spectra from Certified Reference Uranium and Plutonium Materials

International Nuclear Information System (INIS)

Zsigrai, J.; Muehleisen, A.; ); Weber, A.-L.; Funk, P.; Berlizov, A.; Mintcheva, J.

2015-01-01

The Institute of Transuranium Elements (ITU) has made an effort to record a collection of medium resolution gamma-ray spectra from well-characterized U and Pu certified reference materials CRM-171 (also known as SRM-969), CBNM-271, and Harwell PIDIE standards. The goal of this exercise was twofold: (i) to complement the international database of reference gamma-ray spectra with high-quality data for medium resolution spectrometers, and (ii) to feed Phase I of the U/Pu isotopic inter-comparison exercise that is being jointly organized by the ESARDA NDA Working Group and IAEA. Phase II of the exercise will be fed by similar spectra recorded by Institute for Radiological Protection and Nuclear Safety (IRSN). These activities are supported through a joint Member State Support Programmes (MSSP) task and aimed at delivering reliable methodologies for the determination of U/Pu isotopic composition using medium resolution gamma-spectrometers. The latter have obvious benefits for in-field applications, amongst which are better usability, portability and maintainability. As the spectra will be made available online for software developers and end users, ultimately this will also contribute to sustainability as well as the improved and validated performance of existing U/Pu isotopic codes. The spectra were recorded using the IAEA's standard Lanthanum Bromide (LaBr3(Ce)) (2.0'' x 0.5'') and Cadmium Zink Telluride (CdZnTe) (500 mm''3) detectors and acquisition electronics. Aiming to acquire the highest quality reference data, the spectra were measured for long acquisition times, ensuring very good counting statistics across potentially useful spectral intervals — up to 1 MeV for the CdZnTe and up to 2.6 MeV for the LaBr3(Ce) detectors. Great attention was also paid to ensure that the measurement geometry was stable and reproducible, and the spectra had minimum influence from background radiation and pile-up effects. The paper will briefly

Isotope dilution mass spectrometry: some present limitations and possibilities to overcome these

International Nuclear Information System (INIS)

De Bievre, P.

1981-01-01

Thermionic mass spectrometry still has great potential for more precise and accurate measurements but it is going to place tremendous requirements on (1) the chemical purity of the samples we measure, (2) the temperature of both ionization and the filaments and (3) the number of molecular species being handled in ion sources which could increase to several dozen for one type of isotopic analysis. The lack of control by mass spectrometrists over the chemical preparation of the samples for isotopic analysis is an inherent limitation to further improvement of isotope dilution mass spectrometry. A limiting factor in isotope dilution is the ability to measure the ratio. At present, uranium isotopic reference materials are 0.1% and recently one was prepared at 0.05%. As these serve to calibrate isotope ratio measurements one cannot do better than these valves. There is no way in which isotope dilution can be improved until these reference values improve. For plutonium there are not even absolute isotope ratio standards. An agreement has been established between CBNM, Geel and the National Bureau of Standards, Washington, to prepare isotope ratio reference materials jointly so that they will be common to both communities. It is recommended that common batches of reference be established and stored at several places to guarantee accessibility at all times

Saturation and isotopic replacement of deuterium in low-Z material

International Nuclear Information System (INIS)

Doyle, B.L.; Wampler, W.R.; Brice, D.K.; Picraux, S.T.

1980-01-01

The saturation and replacement of hydrogen isotopes implanted into TiC, TiB 2 , VB 2 , B 4 C, B, Si, and C has been examined experimentally and modeled theoretically. The deuterium saturation concentrations for these materials varied from .16 to .57. A new isotopic replacement model is presented which predicts isotopic trapping and exchange on the basis of the depth dependence of the implanted ions and the experimentally determined hydrogen saturation concentration. Our results indicate that, for these materials used as coatings on components in a D-T fueled tokamak, T recovery by ion induced replacement with H or D should be feasible and that T buildup will be at tolerable levels

15 CFR 230.3 - New Standard Reference Materials.

Science.gov (United States)

2010-01-01

... NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY, DEPARTMENT OF COMMERCE STANDARD REFERENCE MATERIALS STANDARD REFERENCE MATERIALS General Information § 230.3 New Standard Reference Materials. When new SRM's... scientific and trade journals. ...

Metabolic studies in man using stable isotopes

International Nuclear Information System (INIS)

Faust, H.; Jung, K.; Krumbiegel, P.

1993-01-01

In this project, stable isotope compounds and stable isotope pharmaceuticals were used (with emphasis on the application of 15 N) to study several aspects of nitrogen metabolism in man. Of the many methods available, the 15 N stable isotope tracer technique holds a special position because the methodology for application and nitrogen isotope analysis is proven and reliable. Valid routine methods using 15 N analysis by emission spectrometry have been demonstrated. Several methods for the preparation of biological material were developed during our participation in the Coordinated Research Programme. In these studies, direct procedures (i.e. use of diluted urine as a samples without chemical preparation) or rapid isolation methods were favoured. Within the scope of the Analytical Quality Control Service (AQCS) enriched stable isotope reference materials for medical and biological studies were prepared and are now available through the International Atomic Energy Agency. The materials are of special importance as the increasing application of stable isotopes as tracers in medical, biological and agricultural studies has focused interest on reliable measurements of biological material of different origin. 24 refs

Cadmium isotope fractionation of materials derived from various industrial processes

Energy Technology Data Exchange (ETDEWEB)

Martinková, Eva, E-mail: eva.cadkova@geology.cz [Czech Geological Survey, Geologická 6, 152 00 Prague 5 (Czech Republic); Chrastný, Vladislav, E-mail: chrastny@fzp.czu.cz [Faculty of Environmental Sciences, Czech University of Life Sciences Prague, Kamýcká 129, 165 21 Prague 6 (Czech Republic); Francová, Michaela, E-mail: michaela.francova@fzp.czu.cz [Faculty of Environmental Sciences, Czech University of Life Sciences Prague, Kamýcká 129, 165 21 Prague 6 (Czech Republic); Šípková, Adéla, E-mail: adela.sipkova@geology.cz [Czech Geological Survey, Geologická 6, 152 00 Prague 5 (Czech Republic); Čuřík, Jan, E-mail: jan.curik@geology.cz [Czech Geological Survey, Geologická 6, 152 00 Prague 5 (Czech Republic); Myška, Oldřich, E-mail: oldrich.myska@geology.cz [Czech Geological Survey, Geologická 6, 152 00 Prague 5 (Czech Republic); Mižič, Lukáš, E-mail: lukas.mizic@geology.cz [Czech Geological Survey, Geologická 6, 152 00 Prague 5 (Czech Republic)

2016-01-25

Highlights: • All studied industrial processes were accompanied by Cd isotope fractionation. • ϵ{sup 114/110} Cd values of the waste materials were discernible from primary sources. • Technology in use plays an important role in Cd isotope fractionation. - Abstract: Our study represents ϵ{sup 114/110} Cd {sub NIST3108} values of materials resulting from anthropogenic activities such as coal burning, smelting, refining, metal coating, and the glass industry. Additionally, primary sources (ore samples, pigment, coal) processed in the industrial premises were studied. Two sphalerites, galena, coal and pigment samples exhibited ϵ{sup 114/110} Cd{sub NIST3108} values of 1.0 ± 0.2, 0.2 ± 0.2, 1.3 ± 0.1, −2.3 ± 0.2 and −0.1 ± 0.3, respectively. In general, all studied industrial processes were accompanied by Cd isotope fractionation. Most of the industrial materials studied were clearly distinguishable from the samples used as a primary source based on ϵ{sup 114/110} Cd {sub NIST3108} values. The heaviest ϵ{sup 114/110} Cd{sub NIST3108} value of 58.6 ± 0.9 was found for slag resulting from coal combustion, and the lightest ϵ{sup 114/110} Cd{sub NIST3108} value of −23 ± 2.5 was observed for waste material after Pb refinement. It is evident that ϵ{sup 114/110} Cd {sub NIST3108} values depend on technological processes, and in case of incomplete Cd transfer from source to final waste material, every industrial activity creates differences in Cd isotope composition. Our results show that Cd isotope analysis is a promising tool to track the origins of industrial waste products.

Value assignment of nutrient concentrations in five standard reference materials and six reference materials.

Science.gov (United States)

Sharpless, K E; Gill, L M

2000-01-01

A number of food-matrix reference materials (RMs) are available from the National Institute of Standards and Technology (NIST) and from Agriculture Canada through NIST. Most of these materials were originally value-assigned for their elemental composition (major, minor, and trace elements), but no additional nutritional information was provided. Two of the materials were certified for selected organic constituents. Ten of these materials (Standard Reference Material [SRM] 1,563 Cholesterol and Fat-Soluble Vitamins in Coconut Oil [Natural and Fortified], SRM 1,566b Oyster Tissue, SRM 1,570a Spinach Leaves, SRM 1,974a Organics in Mussel Tissue (Mytilus edulis), RM 8,415 Whole Egg Powder, RM 8,418 Wheat Gluten, RM 8,432 Corn Starch, RM 8,433 Corn Bran, RM 8,435 Whole Milk Powder, and RM 8,436 Durum Wheat Flour) were recently distributed by NIST to 4 laboratories with expertise in food analysis for the measurement of proximates (solids, fat, protein, etc.), calories, and total dietary fiber, as appropriate. SRM 1846 Infant Formula was distributed as a quality control sample for the proximates and for analysis for individual fatty acids. Two of the materials (Whole Egg Powder and Whole Milk Powder) were distributed in an earlier interlaboratory comparison exercise in which they were analyzed for several vitamins. Value assignment of analyte concentrations in these 11 SRMs and RMs, based on analyses by the collaborating laboratories, is described in this paper. These materials are intended primarily for validation of analytical methods for the measurement of nutrients in foods of similar composition (based on AOAC INTERNATIONAL's fat-protein-carbohydrate triangle). They may also be used as "primary control materials" in the value assignment of in-house control materials of similar composition. The addition of proximate information for 10 existing reference materials means that RMs are now available from NIST with assigned values for proximates in 6 of the 9 sectors of

Certification of methylmercury in cod fish tissue certified reference material by species-specific isotope dilution mass spectrometric analysis

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Kuroiwa, Takayoshi; Narukawa, Tomohiro; Yarita, Takashi; Takatsu, Akiko; Okamoto, Kensaku; Chiba, Koichi [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, Tsukuba, Ibaraki (Japan)

2008-07-15

A new cod fish tissue certified reference material, NMIJ CRM 7402-a, for methylmercury analysis was certified by the National Metrological Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Cod fish was collected from the sea close to Japan. The cod muscle was powdered by freeze-pulverization and was placed into 600 glass bottles (10 g each), which were sterilized with {gamma}-ray irradiation. The certification was carried out using species-specific isotope dilution gas chromatography inductively coupled plasma mass spectrometry (SSID-GC-ICPMS), where {sup 202}Hg-enriched methylmercury (MeHg) was used as the spike compound. In order to avoid any possible analytical biases caused by nonquantitative extraction, degradation and/or formation of MeHg in sample preparations, two different extraction methods (KOH/methanol and HCl/methanol extractions) were performed, and one of these extraction methods utilized two different derivatization methods (ethylation and phenylation). A double ID method was adopted to minimize the uncertainty arising from the analyses. In order to ensure not only the reliability of the analytical results but also traceability to SI units, the standard solution of MeHg used for the reverse-ID was prepared from high-purity MeHg chloride and was carefully assayed as follows: the total mercury was determined by ID-ICPMS following aqua regia digestion, and the ratio of Hg as MeHg to the total Hg content was estimated by GC-ICPMS. The certified value given for MeHg is 0.58 {+-} 0.02 mg kg{sup -1} as Hg. (orig.)

Production of NDA Working Reference Materials for the Capability Evaluation Project

International Nuclear Information System (INIS)

Noll, P.D. Jr.; Marshall, R.S.

1998-01-01

The production of Non Destructive Assay (NDA) Working Reference Materials (WRMs) that are traceable to nationally recognized standards was undertaken to support implementation of the Idaho National Engineering and Environmental Laboratory (INEEL) Nondestructive Waste Assay Capability Evaluation Project (CEP). The WRMs produced for the CEP project consist of Increased Am/Pu mass ration (IAP) and depleted Uranium (DU) WRMs. The CEP IAP/DU WRM set provides radioactive material standards for use in combination with 55 gallon drum waste matrix surrogates for the assessment of waste NDA assay system performance. The Production of WRMs is a meticulous process that is not without certain trials and tribulations. Problems may arise at any of the various stages of WRM production which include, but are not limited to; material characterization (physical, chemical, and isotopic), material blend parameters, personnel radiation exposure, gas generation phenomenon, traceability to national standards, encapsulation, statistical evaluation of the data, and others. Presented here is an overall description of the process by which the CEP WRMs were produced and certified as well as discussions pertaining to some of the problems encountered and how they were solved

Materials technology for accelerator production of fissile isotopes

International Nuclear Information System (INIS)

Horak, J.A.

1978-02-01

The materials used for the accelerator production of fissile isotopes must enable the facility to achieve maximum fuel production at a minimum cost. Neutron production in the target would be maximized by use of thorium cooled with Pb--56 percent Bi or with sodium. The thorium should be ion-plated with approximately 1 mil of nickel or stainless steel for retention of fission products. The target container will have to be replaced at frequent intervals because of the copious quantities of neutronically produced helium and hydrogen in the container. Replacement would coincide with shutdown of the facility for the removal of the fissile material produced. If sodium is used to cool both the target and fertile blanket, a simple basket-type target container could be used. This would greatly reduce radiation effects in the target container. Type 316 stainless steel or V--20 wt percent Ti should perform satisfactorily as a target container. The fertile blanket should be 233 Th or 238 U that is coated with approximately 1 mil of nickel or stainless steel and cooled with sodium. The blanket container could be an austenitic stainless steel such as type 304 or 316; some ferritic alloys may also provide a satisfactory blanket container. 31 references

Steroid isotopic standards for gas chromatography-combustion isotope ratio mass spectrometry (GCC-IRMS).

Science.gov (United States)

Zhang, Ying; Tobias, Herbert J; Brenna, J Thomas

2009-03-01

Carbon isotope ratio (CIR) analysis of urinary steroids using gas chromatography-combustion isotope ratio mass spectrometry (GCC-IRMS) is a recognized test to detect illicit doping with synthetic testosterone. There are currently no universally used steroid isotopic standards (SIS). We adapted a protocol to prepare isotopically uniform steroids for use as a calibrant in GCC-IRMS that can be analyzed under the same conditions as used for steroids extracted from urine. Two separate SIS containing a mixture of steroids were created and coded CU/USADA 33-1 and CU/USADA 34-1, containing acetates and native steroids, respectively. CU/USADA 33-1 contains 5alpha-androstan-3beta-ol acetate (5alpha-A-AC), 5alpha-androstan-3alpha-ol-17-one acetate (androsterone acetate, A-AC), 5beta-androstan-3alpha-ol-11, 17-dione acetate (11-ketoetiocholanolone acetate, 11k-AC) and 5alpha-cholestane (Cne). CU/USADA 34-1 contains 5beta-androstan-3alpha-ol-17-one (etiocholanolone, E), 5alpha-androstan-3alpha-ol-17-one (androsterone, A), and 5beta-pregnane-3alpha, 20alpha-diol (5betaP). Each mixture was prepared and dispensed into a set of about 100 ampoules using a protocol carefully designed to minimize isotopic fractionation and contamination. A natural gas reference material, NIST RM 8559, traceable to the international standard Vienna PeeDee Belemnite (VPDB) was used to calibrate the SIS. Absolute delta(13)C(VPDB) and Deltadelta(13)C(VPDB) values from randomly selected ampoules from both SIS indicate uniformity of steroid isotopic composition within measurement reproducibility, SD(delta(13)C)<0.2 per thousand. This procedure for creation of isotopic steroid mixtures results in consistent standards with isotope ratios traceable to the relevant international reference material.

The role of certified reference materials in material control and accounting

International Nuclear Information System (INIS)

Turel, S.P.

1979-01-01

One way of providing an adequate material control and accounting system for the nuclear fuel cycle is to calculate material unaccounted for (MUF) after a physical inventory and to compare the limit of error of the MUF value (LEMUF) against prescribed criteria. To achieve a meaningful LEMUF, a programme for the continuing determination of systematic and random errors is necessary. Within this programme it is necessary to achieve traceability of all Special Nuclear Material (SNM) control and accounting measurements to an International/National Measurement System by means of Certified Reference Materials. SNM measurements for control and accounting are made internationally on a great variety of materials using many diverse measurement procedures by a large number of facilities. To achieve valid overall accountability over this great variety of measurements there must be some means of relating all these measurements and their uncertainties to each other. This is best achieved by an International/National Measurement System (IMS/NMS). To this end, all individual measurement systems must be compatible to the IMS/NMS and all measurement results must be traceable to appropriate international/national Primary Certified Reference Materials. To obtain this necessary compatibility for any given SNM measurement system, secondary certified reference materials or working reference materials are needed for every class of SNM and each type of measurement system. Ways to achieve ''traceability'' and the various types of certified reference material are defined and discussed in this paper. (author)

Hydrogen isotopes transport parameters in fusion reactor materials

International Nuclear Information System (INIS)

Serra, E.; Ogorodnikova, O.V.

1998-01-01

This work presents a review of hydrogen isotopes-materials interactions in various materials of interest for fusion reactors. The relevant parameters cover mainly diffusivity, solubility, trap concentration and energy difference between trap and solution sites. The list of materials includes the martensitic steels (MANET, Batman and F82H-mod.), beryllium, aluminium, beryllium oxide, aluminium oxide, copper, tungsten and molybdenum. Some experimental work on the parameters that describe the surface effects is also mentioned. (orig.)

Platinum stable isotope analysis of geological standard reference materials by double-spike MC-ICPMS

DEFF Research Database (Denmark)

Creech, John Benjamin; Baker, J. A.; Handler, M. R.

2014-01-01

. Double-spiking of samples was carried out prior to digestion and chemical separation to correct for any mass-dependent fractionation that may occur due to incomplete recovery of Pt. Samples were digested using a NiS fire assay method, which pre-concentrates Pt into a metallic bead that is readily...... metal standard solution doped with a range of synthetic matrices and results in Pt yields of ≥90% with purity of ≥95%. Using this chemical separation technique, we have separated Pt from 11 international geological standard reference materials comprising of PGE ores, mantle rocks, igneous rocks and one...

ISOTOPIC CHARACTERIZATION OF ORGANIC MATERIALS LEACHED FROM LEAVES IN WATER OF MUNDARING WEIR DAM

Directory of Open Access Journals (Sweden)

Markus Heryanto Langsa

2010-06-01

Full Text Available This study examined the organic constituents aquatically leached from leaf components of two tree species (wandoo eucalyptus and pinus radiate. In particular this study aimed to assess the stable isotope composition behaviour of dissolved organic carbon (DOC from the residue leaves after leaching over five months. The changes in the stable carbon and nitrogen isotope compositions of the leached leaves materials were investigated using an elemental analyzer-isotope ratio mass spectrometry (EA-irMS. The stable isotope compositions were found to vary according to microbially-mediated alteration and decomposition. The average  d13C content of the raw plant elements was consistent with the  d13C values of terrestrial plants using a C3 photosynthetic pathway. The isotope compositions of leached materials of wandoo eucalyptus fresh leaf were continually depleted in d13C over the leaching period of three months. These variations correlated well with its DOC profile. Changes in  d13C values may also relate to the differential leaching of the macromolecular precursors of the original material. Lignin, for example, has a typically low  d13C and probably contributed to the decrease of  d13C in residue of the plant materials.   Keywords: isotope composition, leached materials, C3 plant

Development and validation of an analytical method for the determination of lead isotopic composition using ICP-QMS

OpenAIRE

Rodríguez-Salazar, M. T.; Morton Bermea, O.; Hernández-Álvarez, E.; García-Arreola, M. E.; Ortuño-Arzate, M. T.

2010-01-01

This work reports a method for the precise and accurate determination of Pb isotope composition in soils and geological matrices by ICP-QMS. Three reference materials (AGV-2, SRM 2709 and JSO-1) were repeatedly measured, using ICP-QMS instruments in order to assess the quality of this analytical procedure. Mass discrimination was evaluated for Pb/Pb with Pb isotope reference material NIST SRM 981, and the correction applied to the above mentioned reference materials to achieve good accuracy o...

Error analysis of isotope dilution mass spectrometry method with internal standard

International Nuclear Information System (INIS)

Rizhinskii, M.W.; Vitinskii, M.Y.

1989-02-01

The computation algorithms of the normalized isotopic ratios and element concentration by isotope dilution mass spectrometry with internal standard are presented. A procedure based on the Monte-Carlo calculation is proposed for predicting the magnitude of the errors to be expected. The estimation of systematic and random errors is carried out in the case of the certification of uranium and plutonium reference materials as well as for the use of those reference materials in the analysis of irradiated nuclear fuels. 4 refs, 11 figs, 2 tabs

Development of new reference materials for the determination of cadmium, chromium, mercury and lead in polycarbonate

International Nuclear Information System (INIS)

Lee, Kil Jae; Lee, Yeo Jin; Choi, Young Rak; Kim, Jeong Sook; Kim, Youn Sung; Heo, Soo Bong

2013-01-01

Highlights: ► RMs for the determination of Cd, Cr, Hg and Pb in polycarbonate were developed. ► Double ID-ICP-MS technique was used for characterization of candidate RMs. ► The certified values for the elements ranged from 51.7 to 1133 mg kg −1 . ► The relative expanded uncertainties were shown to be less than 5.4%. ► New RMs were found to be suitable for the RoHS compliant tests. - Abstract: Reference materials for quantitative determination of Cd, Cr, Hg and Pb in polycarbonate were developed. Reference materials with two concentration level of elements were prepared by adding appropriate amounts of chemicals to a blank polycarbonate base material. It was shown that ten bottles with triplicate analysis are enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for four weeks and long-term stability test for twelve months. The certification of the four elements was carried out by isotope-dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS) with microwave-assisted digestion. Certification of candidate reference materials in a single laboratory was confirmed with interlaboratory comparison participated by a certain number of well-recognized testing laboratories in Korea. The certified values and expanded uncertainties (k = 2) for the candidate reference material with low level and the one with high level were (51.7 ± 2.1) mg kg −1 Cd, (103.8 ± 2.9) mg kg −1 Cd, (98.8 ± 4.5) mg kg −1 Cr, (1004 ± 49.8) mg kg −1 Cr, (107.4 ± 4.6) mg kg −1 Hg, (1133 ± 50.7) mg kg −1 Hg, (94.8 ± 3.7) mg kg −1 Pb and (988.4 ± 53.6) mg kg −1 Pb, respectively. The reference materials developed in this study demonstrated their suitability for the quality assurance in Cd, Cr, Hg and Pb analysis for the implementation of RoHS Directive.

Reference materials for microanalytical nuclear techniques

Energy Technology Data Exchange (ETDEWEB)

Injuk, Jasna; Grieken, Rene van [Department of Chemistry, Micro and Trace Analysis Centre, University of Antwerp, Wilrijk-Antwerp (Belgium)

1994-07-01

This paper discusses some issues concerning reference materials required for microanalysis including physical and chemical properties of the sample matrix and homogeneity of the chemical composition. It gives some examples of the mst common standards used. Further the paper gives background information about the Micro- and Trace Analysis Center of the University of Antwerp, Belgium and discusses recent results of the Center in microanalysis of reference materials.

A new high-quality set of singly (H-2) and doubly (H-2 and O-18) stable isotope labeled reference waters for biomedical and other isotope-labeled research

NARCIS (Netherlands)

Faghihi, V.; Verstappen-Dumoulin, B. M. A. A.; Jansen, H. G.; van Dijk, G.; Aerts-Bijma, A. T.; Kerstel, E. R. T.; Groening, M.; Meijer, H. A. J.

2015-01-01

RATIONALE: Research using water with enriched levels of the rare stable isotopes of hydrogen and/or oxygen requires well-characterized enriched reference waters. The International Atomic Energy Agency (IAEA) did have such reference waters available, but these are now exhausted. New reference waters

Preparation and certification of trace mercury in water standard reference materials

International Nuclear Information System (INIS)

Moody, J.R.; Paulsen, P.J.; Rains, T.C.; Rook, H.L.

1976-01-01

The study of mercury in natural water supplies requires a Standard Reference Material (SRM) with a certified concentration at the 1 ng/g level. NBS SRM's have been prepared with nominal mercury concentrations of 1.5 μg/g and 1.2 ng/g. Confirmation of these values was obtained by neutron activation, atomic absorption, and isotope dilution-spark source mass spectrometry (IDSSMS). Nitric acid and trace amounts of gold were added to achieve a stable mercury concentration. The precautions observed for cleaning the glass and Teflon containers, preparation of mercury solutions, and the packaging of the SRM's are given. As an example of the care needed in the analysis of mercury at these levels, specific details are presented for the chemistry required to prepare samples for the spark source mass spectrometer

Isotope materials availability and services for target production at the Oak Ridge National Laboratory

International Nuclear Information System (INIS)

Ratledge, J.E.; Dahl, T.L.; Ottinger, C.L.; Aaron, W.S.; Adair, H.L.

1987-01-01

Materials available through the Isotope Distribution Program include separated stable isotopes, byproduct radioisotopes, and research quantities of source and special nuclear materials. Isotope products are routinely available in the forms listed in the product description section of the Isotopes Products and Services Catalog distributed by the Oak Ridge National Laboratory (ORNL). Different forms can be provided in some cases, usually at additional cost. Routinely available services include cyclotron target irradiations, fabrication of special physical forms, source encapsulation, ion implantation, and special purifications. Materials and services that are not offered as part of the routine distribution program may be made available from commercial sources in the United States. Specific forms of isotopic research materials include thin films and foils for use as accelerator targets, metal or other compounds in the form of bars or wires, and metal foils. Methods of fabrication include evaporation, sputtering, rolling, electrolytic deposition, pressing, sintering, and casting. High-purity metal forms of plutonium, americium, and curium are prepared by vacuum reduction/distillation. Both fissionable and nonfissionable neutron dosimeters are prepared for determining the neutron energy spectra, flux, and fluence at various locations within a reactor. Details on what materials are available and how the materials and related services can be obtained from ORNL are described. (orig.)

Determination of trace sulfur in biodiesel and diesel standard reference materials by isotope dilution sector field inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Amais, Renata S. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP (Brazil); Long, Stephen E. [Chemical Sciences Division, National Institute of Standards and Technology, Charleston, SC (United States); Nóbrega, Joaquim A. [Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP (Brazil); Christopher, Steven J., E-mail: steven.christopher@nist.gov [Chemical Sciences Division, National Institute of Standards and Technology, Charleston, SC (United States)

2014-01-02

Graphical abstract: -- Highlights: •Sulfur mass fractions are measured below 10 mg kg{sup −1} in diesel fuel materials. •SF-ICP-MS resolves molecular interferences, including oxygen and sulfur hydrides. •A detection limit of 0.7 mg kg{sup −1} (in the fuel sample) was obtained. -- Abstract: A method is described for quantification of sulfur at low concentrations on the order of mg kg{sup −1} in biodiesel and diesel fuels using isotope dilution and sector field inductively coupled plasma mass spectrometry (ID-SF-ICP-MS). Closed vessel microwave-assisted digestion was employed using a diluted nitric acid and hydrogen peroxide decomposition medium to reduce sample dilution volumes. Medium resolution mode was employed to eliminate isobaric interferences at {sup 32}S and {sup 34}S related to polyatomic phosphorus and oxygen species, and sulfur hydride species. The method outlined yielded respective limits of detection (LOD) and limits of quantification (LOQ) of 0.7 mg kg{sup −1} S and 2.5 mg kg{sup −1} S (in the sample). The LOD was constrained by instrument background counts at {sup 32}S but was sufficient to facilitate value assignment of total S mass fraction in NIST SRM 2723b Sulfur in Diesel Fuel Oil at 9.06 ± 0.13 mg kg{sup −1}. No statistically significant difference at a 95% confidence level was observed between the measured and certified values for certified reference materials NIST SRM 2773 B100 Biodiesel (Animal-Based), CENAM DRM 272b and NIST SRM 2723a Sulfur in Diesel Fuel Oil, validating method accuracy.

Reference materials and interlaboratory comparison for actinide analysis

International Nuclear Information System (INIS)

Hanssens, Alain; Viallesoubranne, Carole; Roche, Claude; Liozon, Gerard

2008-01-01

Measurement quality is crucial for the safety of nuclear facilities and is a primary requirement for fissile material monitoring and accountancy. CETAMA (Cea Committee for the establishment of analysis methods), in collaboration with Cea and AREVA laboratories, fabricates certified reference materials and organizes interlaboratory comparison programs for plutonium and uranium assay in solution. A new plutonium metal measurement standard (MP3) is currently being prepared by Cea and is a subject of cooperative work in view of its certification and use by analysis laboratories. U and Pu interlaboratory comparisons are carried out at regular intervals on benchmark samples in coordination with working groups from French nuclear laboratories. These programs are supported by international cooperation. 'Chemical' methods (potentiometry, gravimetric analysis, etc.) generally provide the best accuracy. Coulometry is the benchmark technique for plutonium assay: its metrological qualities should be an incentive for wider use by laboratories performing precise control assays of plutonium as well as uranium. Gravimetric analysis provides excellent results for analysis of pure uranyl nitrate solutions. In view of its many advantages we encourage laboratories to employ this technique to assay pure U or Pu solutions. 'Physical' or 'physicochemical' methods are increasingly used, and their performance has improved. K-edge absorption spectrometry and isotope dilution mass spectrometry are capable of reaching measurement quality levels comparable to those of the best 'chemical' methods. (authors)

Radioactive certified reference materials

International Nuclear Information System (INIS)

Watanabe, Kazuo

2010-01-01

Outline of radioactive certified reference materials (CRM) for the analysis of nuclear materials and radioactive nuclides were described. The nuclear fuel CRMs are supplied by the three institutes: NBL in the US, CETAMA in France and IRMM in Belgium. For the RI CRMs, the Japan Radioisotope Association is engaged in activities concerning supply. The natural-matrix CRMs for the analysis of trace levels of radio-nuclides are prepared and supplied by NIST in the US and the IAEA. (author)

Nuclear material safeguards surveillance and accountancy by isotope correlation techniques

International Nuclear Information System (INIS)

Persiani, P.J.; Goleb, J.A.; Kroc, T.K.

1981-11-01

The purpose of this study is to investigate the applicability of isotope correlation techniques (ICT) to the Light Water Reactor (LWR) and the Liquid Metal Fast Breeder Reactor (LMFBR) fuel cycles for nuclear material accountancy and safeguards surveillance. The isotopic measurement of the inventory input to the reprocessing phase of the fuel cycle is the primary direct determination that an anomaly may exist in the fuel management of nuclear material. The nuclear materials accountancy gap which exists between the fabrication plant output and the input to the reprocessing plant can be minimized by using ICT at the dissolver stage of the reprocessing plant. The ICT allows a level of verification of the fabricator's fuel content specifications, the irradiation history, the fuel and blanket assemblies management and scheduling within the reactor, and the subsequent spent fuel assembly flows to the reprocessing plant. The investigation indicates that there exist relationships between isotopic concentration which have predictable, functional behavior over a range of burnup. Several cross-correlations serve to establish the initial core assembly-averaged composition. The selection of the more effective functionals will depend not only on the level of reliability of ICT for verification, but also on the capability, accuracy and difficulty of developing measurement methods. The propagation of measurement errors on the correlation functions and respective sensitivities to isotopic compositional changes have been examined and found to be consistent with current measurement methods

PLANETARY-SCALE STRONTIUM ISOTOPIC HETEROGENEITY AND THE AGE OF VOLATILE DEPLETION OF EARLY SOLAR SYSTEM MATERIALS

Energy Technology Data Exchange (ETDEWEB)

Moynier, Frederic; Podosek, Frank A. [Department of Earth and Planetary Science and McDonnell Center for Space Sciences, Washington University, St. Louis, MO 63130 (United States); Day, James M. D. [Geosciences Research Division, Scripps Institution of Oceanography, La Jolla, CA 92093-0244 (United States); Okui, Wataru; Yokoyama, Tetsuya [Department of Earth and Planetary Sciences, Tokyo Institute of Technology, Tokyo 152-8551 (Japan); Bouvier, Audrey [Department of Earth Sciences, University of Minnesota, Minneapolis, MN 55455-0231 (United States); Walker, Richard J., E-mail: moynier@levee.wustl.edu, E-mail: fap@levee.wustl.edu, E-mail: jmdday@ucsd.edu, E-mail: rjwalker@umd.edu, E-mail: okui.w.aa@m.titech.ac.jp, E-mail: tetsuya.yoko@geo.titech.ac.jp, E-mail: abouvier@umn.edu [Department of Geology, University of Maryland, College Park, MD 20742 (United States)

2012-10-10

Isotopic anomalies in planetary materials reflect both early solar nebular heterogeneity inherited from presolar stellar sources and processes that generated non-mass-dependent isotopic fractionations. The characterization of isotopic variations in heavy elements among early solar system materials yields important insight into the stellar environment and formation of the solar system, and about initial isotopic ratios relevant to long-term chronological applications. One such heavy element, strontium, is a central element in the geosciences due to wide application of the long-lived {sup 87}Rb-{sup 87}Sr radioactive as a chronometer. We show that the stable isotopes of Sr were heterogeneously distributed at both the mineral scale and the planetary scale in the early solar system, and also that the Sr isotopic heterogeneities correlate with mass-independent oxygen isotope variations, with only CI chondrites plotting outside of this correlation. The correlation implies that most solar system material formed by mixing of at least two isotopically distinct components: a CV-chondrite-like component and an O-chondrite-like component, and possibly a distinct CI-chondrite-like component. The heterogeneous distribution of Sr isotopes may indicate that variations in initial {sup 87}Sr/{sup 86}Sr of early solar system materials reflect isotopic heterogeneity instead of having chronological significance, as interpreted previously. For example, given the differences in {sup 84}Sr/{sup 86}Sr between calcium aluminum inclusions and eucrites ({epsilon}{sup 84}Sr > 2), the difference in age between these materials would be {approx}6 Ma shorter than previously interpreted, placing the Sr chronology in agreement with other long- and short-lived isotope systems, such as U-Pb and Mn-Cr.

Standard test method for analysis of isotopic composition of uranium in nuclear-grade fuel material by quadrupole inductively coupled plasma-mass spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2000-01-01

1.1 This test method is applicable to the determination of the isotopic composition of uranium (U) in nuclear-grade fuel material. The following isotopic weight percentages are determined using a quadrupole inductively coupled plasma-mass spectrometer (Q-ICP-MS): 233U, 234U, 235U, 236U, and 238U. The analysis can be performed on various material matrices after acid dissolution and sample dilution into water or dilute nitric (HNO3) acid. These materials include: fuel product, uranium oxide, uranium oxide alloys, uranyl nitrate (UNH) crystals, and solutions. The sample preparation discussed in this test method focuses on fuel product material but may be used for uranium oxide or a uranium oxide alloy. Other preparation techniques may be used and some references are given. Purification of the uranium by anion-exchange extraction is not required for this test method, as it is required by other test methods such as radiochemistry and thermal ionization mass spectroscopy (TIMS). This test method is also described i...

Preparation and evaluation of reference materials for accountancy analysis. (1) Preparation and evaluation method

International Nuclear Information System (INIS)

Takamatsu, Mai; Kacchi, Tomokazu; Murakami, Toshiki; Ai, Hironobu; Sumi, Mika; Abe, Katsuo; Kageyama, Tomio; Nakazawa, Hiroaki

2009-01-01

Isotope dilution mass spectrometry method used for the accountancy analysis at nuclear fuel facilities requires the standard materials called LSD (Large Size Dried) spike. Generally, LSD spikes are prepared from certified reference materials (CRMs) which supplied from foreign laboratories. However, the difficulty of Pu CRM importation is increasing. It is important for safeguards to attain and continue high reliable accountancy analysis and stable securing of LSD spike is essential. Therefore, in order to conserve CRMs, several types of LSD spike were prepared under collaboration work between JAEA and JNFL, such as the amount of nuclear material in one LSD spike is decreased and others. Practical test with actual samples were performed at JNFL Rokkasho reprocessing plant, and those results were compared with the results obtained by using LSD spike which supplied from foreign laboratory. Preparation and verification analysis of LSD spikes and evaluation of uncertainty based on ISO-GUM will be presented. (author)

Preparation of a multi-isotope plutonium AMS standard and preliminary results of a first inter-lab comparison

Energy Technology Data Exchange (ETDEWEB)

Dittmann, B.-A.; Dunai, T.J. [Institute of Geology and Mineralogy, University of Cologne, Greinstr. 4-6, 50939 Cologne (Germany); Dewald, A.; Heinze, S.; Feuerstein, C. [Institute of Nuclear Physics, University of Cologne, Zülpicher Str. 77, 50937 Cologne (Germany); Strub, E. [Division of Nuclear Chemistry, University of Cologne, Zülpicher Str. 45, 50674 Cologne (Germany); Fifield, L.K.; Froehlich, M.B.; Tims, S.G.; Wallner, A. [Department of Nuclear Physics, Research School of Physics & Engineering, Australian National University, Canberra ACT 2601 (Australia); Christl, M. [Laboratory of Ion Beam Physics, ETH Zurich, Otto-Stern-Weg 5, 8093 Zurich (Switzerland)

2015-10-15

The motivation of this work is to establish a new multi-isotope plutonium standard for isotopic ratio measurements with accelerator mass spectrometry (AMS), since stocks of existing solutions are declining. To this end, certified reference materials (CRMs) of each of the individual isotopes {sup 239}Pu, {sup 240}Pu, {sup 242}Pu and {sup 244}Pu were obtained from JRC IRMM (Joint Research Center Institute for Reference Materials and Measurements). These certified reference materials (IRMM-081a, IRMM-083, IRMM-043 and IRMM-042a) were diluted with nitric acid and mixed to obtain a stock standard solution with an isotopic ratio of approximately 1.0:1.0:1.0:0.1 ({sup 239}Pu:{sup 240}Pu:{sup 242}Pu:{sup 244}Pu). From this stock solution, samples were prepared for measurement of the plutonium isotopic composition by AMS. These samples have been measured in a round-robin exercise between the AMS facilities at CologneAMS, at the ANU Canberra and ETH Zurich to verify the isotopic ratio and to demonstrate the reproducibility of the measurements. The results show good agreement both between the different AMS measurements and with the gravimetrically determined nominal ratios.

Biological reference materials and analysis of toxic elements

Energy Technology Data Exchange (ETDEWEB)

Subramanian, R; Sukumar, A

1988-12-01

Biological monitoring of toxic metal pollution in the environment requires quality control analysis with use of standard reference materials. A variety of biological tissues are increasingly used for analysis of element bioaccumulation, but the available Certified Reference Materials (CRMs) are insufficient. An attempt is made to review the studies made using biological reference materials for animal and human tissues. The need to have inter-laboratory studies and CRM in the field of biological monitoring of toxic metals is also discussed.

Novel methods for estimating 3D distributions of radioactive isotopes in materials

Energy Technology Data Exchange (ETDEWEB)

Iwamoto, Y., E-mail: y.iwamoto0805@ruri.waseda.jp [Research Institute for Science and Engineering, Waseda University, Shinjuku, Tokyo 169-8555 (Japan); Kataoka, J.; Kishimoto, A.; Nishiyama, T.; Taya, T.; Okochi, H.; Ogata, H. [Research Institute for Science and Engineering, Waseda University, Shinjuku, Tokyo 169-8555 (Japan); Yamamoto, S. [Nagoya University Graduate School of Medicine, 1-1-20, Daikominami, Higashi-ku, Nagoya-shi, Aichi 461-8673 (Japan)

2016-09-21

In recent years, various gamma-ray visualization techniques, or gamma cameras, have been proposed. These techniques are extremely effective for identifying “hot spots” or regions where radioactive isotopes are accumulated. Examples of such would be nuclear-disaster-affected areas such as Fukushima or the vicinity of nuclear reactors. However, the images acquired with a gamma camera do not include distance information between radioactive isotopes and the camera, and hence are “degenerated” in the direction of the isotopes. Moreover, depth information in the images is lost when the isotopes are embedded in materials, such as water, sand, and concrete. Here, we propose two methods of obtaining depth information of radioactive isotopes embedded in materials by comparing (1) their spectra and (2) images of incident gamma rays scattered by the materials and direct gamma rays. In the first method, the spectra of radioactive isotopes and the ratios of scattered to direct gamma rays are obtained. We verify experimentally that the ratio increases with increasing depth, as predicted by simulations. Although the method using energy spectra has been studied for a long time, an advantage of our method is the use of low-energy (50–150 keV) photons as scattered gamma rays. In the second method, the spatial extent of images obtained for direct and scattered gamma rays is compared. By performing detailed Monte Carlo simulations using Geant4, we verify that the spatial extent of the position where gamma rays are scattered increases with increasing depth. To demonstrate this, we are developing various gamma cameras to compare low-energy (scattered) gamma-ray images with fully photo-absorbed gamma-ray images. We also demonstrate that the 3D reconstruction of isotopes/hotspots is possible with our proposed methods. These methods have potential applications in the medical fields, and in severe environments such as the nuclear-disaster-affected areas in Fukushima.

Novel methods for estimating 3D distributions of radioactive isotopes in materials

Science.gov (United States)

Iwamoto, Y.; Kataoka, J.; Kishimoto, A.; Nishiyama, T.; Taya, T.; Okochi, H.; Ogata, H.; Yamamoto, S.

2016-09-01

In recent years, various gamma-ray visualization techniques, or gamma cameras, have been proposed. These techniques are extremely effective for identifying "hot spots" or regions where radioactive isotopes are accumulated. Examples of such would be nuclear-disaster-affected areas such as Fukushima or the vicinity of nuclear reactors. However, the images acquired with a gamma camera do not include distance information between radioactive isotopes and the camera, and hence are "degenerated" in the direction of the isotopes. Moreover, depth information in the images is lost when the isotopes are embedded in materials, such as water, sand, and concrete. Here, we propose two methods of obtaining depth information of radioactive isotopes embedded in materials by comparing (1) their spectra and (2) images of incident gamma rays scattered by the materials and direct gamma rays. In the first method, the spectra of radioactive isotopes and the ratios of scattered to direct gamma rays are obtained. We verify experimentally that the ratio increases with increasing depth, as predicted by simulations. Although the method using energy spectra has been studied for a long time, an advantage of our method is the use of low-energy (50-150 keV) photons as scattered gamma rays. In the second method, the spatial extent of images obtained for direct and scattered gamma rays is compared. By performing detailed Monte Carlo simulations using Geant4, we verify that the spatial extent of the position where gamma rays are scattered increases with increasing depth. To demonstrate this, we are developing various gamma cameras to compare low-energy (scattered) gamma-ray images with fully photo-absorbed gamma-ray images. We also demonstrate that the 3D reconstruction of isotopes/hotspots is possible with our proposed methods. These methods have potential applications in the medical fields, and in severe environments such as the nuclear-disaster-affected areas in Fukushima.

Reference materials and interlaboratory comparison for actinide analysis

Energy Technology Data Exchange (ETDEWEB)

Hanssens, Alain; Viallesoubranne, Carole; Roche, Claude; Liozon, Gerard [Commissariat a l' Energie Atomique, Marcoule: BP 17171, 30207 Bagnols sur Ceze (France)

2008-07-01

Measurement quality is crucial for the safety of nuclear facilities and is a primary requirement for fissile material monitoring and accountancy. CETAMA (Cea Committee for the establishment of analysis methods), in collaboration with Cea and AREVA laboratories, fabricates certified reference materials and organizes interlaboratory comparison programs for plutonium and uranium assay in solution. A new plutonium metal measurement standard (MP3) is currently being prepared by Cea and is a subject of cooperative work in view of its certification and use by analysis laboratories. U and Pu interlaboratory comparisons are carried out at regular intervals on benchmark samples in coordination with working groups from French nuclear laboratories. These programs are supported by international cooperation. 'Chemical' methods (potentiometry, gravimetric analysis, etc.) generally provide the best accuracy. Coulometry is the benchmark technique for plutonium assay: its metrological qualities should be an incentive for wider use by laboratories performing precise control assays of plutonium as well as uranium. Gravimetric analysis provides excellent results for analysis of pure uranyl nitrate solutions. In view of its many advantages we encourage laboratories to employ this technique to assay pure U or Pu solutions. 'Physical' or 'physicochemical' methods are increasingly used, and their performance has improved. K-edge absorption spectrometry and isotope dilution mass spectrometry are capable of reaching measurement quality levels comparable to those of the best 'chemical' methods. (authors)

Isotope exchange reactions on ceramic breeder materials and their effect on tritium inventory

Energy Technology Data Exchange (ETDEWEB)

Nishikawa, M; Baba, A [Kyushu Univ., Fukuoka (Japan). Faculty of Engineering; Kawamura, Y; Nishi, M

1998-03-01

Though lithium ceramic materials such as Li{sub 2}O, LiAlO{sub 2}, Li{sub 2}ZrO{sub 3}, Li{sub 2}TiO{sub 3} and Li{sub 4}SiO{sub 4} are considered as breeding materials in the blanket of a D-T fusion reactor, the release behavior of the bred tritium in these solid breeder materials has not been fully understood. The isotope exchange reaction rate between hydrogen isotopes in the purge gas and tritium on the surface of breeding materials have not been quantified yet, although helium gas with hydrogen or deuterium is planned to be used as the blanket purge gas in the recent blanket designs. The mass transfer coefficient representing the isotope exchange reaction between H{sub 2} and D{sub 2}O or that between D{sub 2} and H{sub 2}O in the ceramic breeding materials bed is experimentally obtained in this study. Effects of isotope exchange reactions on the tritium inventory in the bleeding blanket is discussed based on data obtained in this study where effects of diffusion of tritium in the grain, absorption of water in the bulk of grain, and adsorption of water on the surface of grain, together with two types of isotope exchange reactions are considered. The way to estimate the tritium inventory in a Li{sub 2}ZrO{sub 3} blanket used in this study shows a good agreement with data obtained in such in-situ experiments as MOZART, EXOTIC-5, 6 and TRINE experiments. (author)

Development of solid water-equivalent radioactive certified reference materials

International Nuclear Information System (INIS)

Finke, E.; Greupner, H.; Groche, K.; Rittwag, R.; Geske, G.

1991-01-01

This paper presents a brief description of the development of solid water-equivalent beta volume radioactive certified reference materials. These certified reference materials were prepared for the beta fission nuclides 90 Sr/ 90 Y, 137 Cs, 147 Pm and 204 Tl. Comparative measurements of liquid and solid water-equivalent beta volume radioactive certified reference materials are discussed. (author)

New reference materials improvement of methods of measurements

International Nuclear Information System (INIS)

Marchandise, H.

1985-01-01

The report summarizes the development of about 120 reference materials in a variety of fields (non ferrous metals, trace element analysis, food products, biomedical analysis, physical and technical properties of solid materials). The document also provides practical advice for trace element analyses, describes the principles followed for certifying reference materials and provides recommendations for their use

Radioactivity reference levels in ceramics tiles as building materials for different countries

International Nuclear Information System (INIS)

Ortiz, Josefina; Ballesteros, Luisa; Serradell, Vicente

2008-01-01

Measurements campaigns of ceramic tiles and raw materials used in them, shows that natural radionuclides of uranium ( 238 U) and thorium ( 232 Th) series, together with the radioactive isotope of potassium ( 40 K ), are presents. Uranium series contain radium, which decays to radon ( 222 Rn), an inert gas that can be released from materials and inhaled by individuals. Limits of 226 Ra concentrations are established by different countries in order to control Radon levels (200 Bq.m -3 in European Union). Potassium -40 and others gamma emitters of 226 Ra and 232 Th descendent, can cause an external dose. Therefore, with the purpose that individual doses due to building materials doesn't exceed a certain level recommendations or regulations have been established. A maximum value of 1 mSv.y -1 is recommended in European Union. In practice an easy way to avoid ceramic tiles provide doses to individuals over the reference level is to introduce an index, depending on activities concentrations of 226 Ra, 232 Th and 40 K, defined so that the dose limits due, exclusively, to building materials, will never be exceeded. These limits and indexes present differences between countries. In this paper indexes are compared and differences are discussed. (author)

Magnesium isotope systematics in Martian meteorites

Science.gov (United States)

Magna, Tomáš; Hu, Yan; Teng, Fang-Zhen; Mezger, Klaus

2017-09-01

Magnesium isotope compositions are reported for a suite of Martian meteorites that span the range of petrological and geochemical types recognized to date for Mars, including crustal breccia Northwest Africa (NWA) 7034. The δ26Mg values (per mil units relative to DSM-3 reference material) range from -0.32 to -0.11‰; basaltic shergottites and nakhlites lie to the heavier end of the Mg isotope range whereas olivine-phyric, olivine-orthopyroxene-phyric and lherzolitic shergottites, and chassignites have slightly lighter Mg isotope compositions, attesting to modest correlation of Mg isotopes and petrology of the samples. Slightly heavier Mg isotope compositions found for surface-related materials (NWA 7034, black glass fraction of the Tissint shergottite fall; δ26Mg > -0.17‰) indicate measurable Mg isotope difference between the Martian mantle and crust but the true extent of Mg isotope fractionation for Martian surface materials remains unconstrained. The range of δ26Mg values from -0.19 to -0.11‰ in nakhlites is most likely due to accumulation of clinopyroxene during petrogenesis rather than garnet fractionation in the source or assimilation of surface material modified at low temperatures. The rather restricted range in Mg isotope compositions between spatially and temporally distinct mantle-derived samples supports the idea of inefficient/absent major tectonic cycles on Mars, which would include plate tectonics and large-scale recycling of isotopically fractionated surface materials back into the Martian mantle. The cumulative δ26Mg value of Martian samples, which are not influenced by late-stage alteration processes and/or crust-mantle interactions, is - 0.271 ± 0.040 ‰ (2SD) and is considered to reflect δ26Mg value of the Bulk Silicate Mars. This value is robust taking into account the range of lithologies involved in this estimate. It also attests to the lack of the Mg isotope variability reported for the inner Solar System bodies at current

Correction of mass spectrometric isotope ratio measurements for isobaric isotopologues of O2, CO, CO2, N2O and SO2.

Science.gov (United States)

Kaiser, Jan; Röckmann, Thomas

2008-12-01

Gas isotope ratio mass spectrometers usually measure ion current ratios of molecules, not atoms. Often several isotopologues contribute to an ion current at a particular mass-to-charge ratio (m/z). Therefore, corrections have to be applied to derive the desired isotope ratios. These corrections are usually formulated in terms of isotope ratios (R), but this does not reflect the practice of measuring the ion current ratios of the sample relative to those of a reference material. Correspondingly, the relative ion current ratio differences (expressed as delta values) are first converted into isotopologue ratios, then into isotope ratios and finally back into elemental delta values. Here, we present a reformulation of this data reduction procedure entirely in terms of delta values and the 'absolute' isotope ratios of the reference material. This also shows that not the absolute isotope ratios of the reference material themselves, but only product and ratio combinations of them, are required for the data reduction. These combinations can be and, for carbon and oxygen have been, measured by conventional isotope ratio mass spectrometers. The frequently implied use of absolute isotope ratios measured by specially calibrated instruments is actually unnecessary. Following related work on CO2, we here derive data reduction equations for the species O2, CO, N2O and SO2. We also suggest experiments to measure the required absolute ratio combinations for N2O, SO2 and O2. As a prelude, we summarise historic and recent measurements of absolute isotope ratios in international isotope reference materials. Copyright 2008 John Wiley & Sons, Ltd.

Isotopic power materials development. Quarterly progress report for period ending March 31, 1976

International Nuclear Information System (INIS)

Schaffhauser, A.C.

1976-06-01

The second in a series of quarterly reports for Technology and Space Applications materials programs conducted by the Metals and Ceramics Division of Oak Ridge National Laboratory for the Nuclear Research and Applications Division of ERDA is presented. These quarterly reports replace the monthly and annual reports previously issued on this work. The areas of research covered include high-temperature alloys for space isotopic heat sources, physical and mechanical metallurgy of heat source containment materials, isotope Brayton system materials support, and space nuclear flight systems hardware

Isotopic-spectral determination of hydrogen, nitrogen, oxygen and carbon in semiconductor materials

International Nuclear Information System (INIS)

Dudich, G.K.; Eremeev, V.A.; Li, V.N.; Nemets, V.M.

1981-01-01

Techniques of low-temperature isotopic-spectral determination of impurities of hydrogen, nitrogen, oxygen and carbon in semiconductor materials Bi, Ge, Pb tellurides are developed. The techniques include selection into special vessel with the known volume (exchanger) of sample analyzed, dosed introduction into exchanger of rare isotope of the element determined ( 2 H, 15 N, 18 O, 13 C) in the form of isotope-containing gas, balancing of the determined element isotopes in the system sample-isotope, containing gas, spectroscopic, determination of its isotope composition in gaseous phase of the system and calculation of the amount of the element determined in the sample. The lower boundaries of the amounts determined constitute 10 -7 , 10 -7 , 10 -6 and 10 -5 mass % respectively when sample of 20 g are used [ru

Development of solid water-equivalent radioactive certified reference materials

Energy Technology Data Exchange (ETDEWEB)

Finke, E.; Greupner, H.; Groche, K.; Rittwag, R. (Office for Standardization, Metrology and Quality Control (ASMW), Berlin (Germany, F.R.)); Geske, G. (Jena Univ. (Germany, F.R.))

1991-01-01

This paper presents a brief description of the development of solid water-equivalent beta volume radioactive certified reference materials. These certified reference materials were prepared for the beta fission nuclides {sup 90}Sr/{sup 90}Y, {sup 137}Cs, {sup 147}Pm and {sup 204}Tl. Comparative measurements of liquid and solid water-equivalent beta volume radioactive certified reference materials are discussed. (author).

Development of a candidate certified reference material of cypermethrin in green tea

International Nuclear Information System (INIS)

Sin, Della W.M.; Chan, Pui-kwan; Cheung, Samuel T.C.; Wong, Yee-Lok; Wong, Siu-kay; Mok, Chuen-shing; Wong Yiuchung

2012-01-01

Highlights: ► A cypermethrin CRM in green tea was developed. ► Using two isotope dilution mass spectrometry techniques for characterization. ► Certified value of 148 μg kg −1 with expanded uncertainty of ±9.2%. ► Support quality assurance of pesticide residue analysis in tea to testing. - Abstract: This paper presents the preparation of a candidate certified reference material (CRM) of cypermethrin in green tea, GLHK-11-01a according to the requirements of ISO Guide 34 and 35. Certification of the material was performed using a newly developed isotope dilution mass spectrometry (IDMS) approach, with gas chromatography high resolution mass spectrometry (GC–HRMS) and gas chromatography–tandem mass spectrometry (GC–MS/MS). Statistical analysis (one-way ANOVA) showed excellent agreement of the analytical data sets generated from the two mass spectrometric detections. The characterization methods have also been satisfactorily applied in an Asia-Pacific Metrology Program (APMP) interlaboratory comparison study. Both the GC–HRIDMS and GC–IDMS/MS methods proved to be sufficiently reliable and accurate for certification purpose. The certified value of cypermethrin in dry mass fraction was 148 μg kg −1 and the associated expanded uncertainty was 14 μg kg −1 . The uncertainty budget was evaluated from sample in homogeneity, long-term and short-term stability and variability in the characterization procedure. GLHK-11-01a is primarily developed to support the local and wider testing community on need basis in quality assurance work and in seeking accreditation.

Preparation and certification of Sargasso seaweed reference material

Energy Technology Data Exchange (ETDEWEB)

Okamoto, Kensaku

1988-01-01

Sargasso seaweed reference material was prepared from Sargassum felvellum obtained from an unpolluted area in Japan. The sargasso samples were washed, freeze-dried, pulverized, sieved to pass a 80-mesh screen and finally homogenized. Collaborative studies on the elemental analysis of the sargasso reference material were performed using various analytical techniques. Certified values are provided for Ag, As, Ca, Cd, Co, Cu, Fe, K, Mg, Mn, Na, Pb, Rb, Sr, V and Zn, based on results of determinations by at least three independent analytical techniques. Reference values are reported for Al, Br, Cl, Cr, Cs, Hg, I, P, S, Sb, Sc, Se, Ti and U. The sargasso certified reference material contains high levels of alkali metals, alkaline earth metals, I, Br, As and U, while the concentration of trace elements may be considered to be at the lower end of the range of reported values for marine brown algae. The sargasso sample will be of practical use in marine and environmental sciences as a certified reference material having an elemental composition close to background levels.

ISOTOPE METHODS IN HOMOGENEOUS CATALYSIS.

Energy Technology Data Exchange (ETDEWEB)

BULLOCK,R.M.; BENDER,B.R.

2000-12-01

The use of isotope labels has had a fundamentally important role in the determination of mechanisms of homogeneously catalyzed reactions. Mechanistic data is valuable since it can assist in the design and rational improvement of homogeneous catalysts. There are several ways to use isotopes in mechanistic chemistry. Isotopes can be introduced into controlled experiments and followed where they go or don't go; in this way, Libby, Calvin, Taube and others used isotopes to elucidate mechanistic pathways for very different, yet important chemistries. Another important isotope method is the study of kinetic isotope effects (KIEs) and equilibrium isotope effect (EIEs). Here the mere observation of where a label winds up is no longer enough - what matters is how much slower (or faster) a labeled molecule reacts than the unlabeled material. The most careti studies essentially involve the measurement of isotope fractionation between a reference ground state and the transition state. Thus kinetic isotope effects provide unique data unavailable from other methods, since information about the transition state of a reaction is obtained. Because getting an experimental glimpse of transition states is really tantamount to understanding catalysis, kinetic isotope effects are very powerful.

Review of neutron activation analysis in the standardization and study of reference materials, including its application to radionuclide reference materials

International Nuclear Information System (INIS)

Byrne, A.R.

1993-01-01

Neutron activation analysis (NAA) plays a very important role in the certification of reference materials (RMs) and their characterization, including homogeneity testing. The features of the method are briefly reviewed, particularly aspects relating to its completely independent nuclear basis, its virtual freedom from blank problems, and its capacity for self-verification. This last aspect, arising from the essentially isotopic character of NAA, can be exploited by using different nuclear reactions and induced nuclides, and the possibility of employing two modes, one instrumental (nondestructive), the other radiochemical (destructive). This enables the derivation of essentially independent analytical information and the unique capacity of NAA for selfvalidation. The application of NAA to quantify natural or man-made radionuclides such as uranium, thorium, 237 Np, 129 I and 230 Th is discussed, including its advantages over conventional radiometric methods and its usefulness in providing independent data for nuclides where other confirmatory analyses are impossible, or are only recently becoming available through newer 'atom counting' techniques. Certain additional, prospective uses of NAA in the study of RMs and potential RMs are mentioned, including transmutation reactions, creation of endogenously radiolabelled matrices for production and study of RMs (such as dissolution and leaching tests, use as incorporated radiotracers for chemical recovery correction), and the possibility of molecular activation analysis for specification. (orig.)

Biomedical applications of mass spectrometry. Clinical uses of stable isotopes

International Nuclear Information System (INIS)

Krahmer, U.I.; McCloskey, J.A.

1978-01-01

The review covers typical or important examples of stable isotope usage in clinical fields during the period since the last triennial mass spectrometry conference in 1973. Items are included which involve uses of stable isotopes in human or clinically oriented studies, including measurements carried out on materials of human origin. 163 references. (U.K.)

Nuclear and isotopic techniques for addressing nutritional problems, with special reference to current applications in developing countries.

Science.gov (United States)

Iyengar, Venkatesh

2002-03-01

Nuclear and isotopic techniques are valuable tools in human nutritional research studies. Isotopes, both radioactive and nonradioactive, enable detailed evaluations of nutrient intake, body composition, energy expenditure, status of micronutrients, and nutrient bioavailability. In recent times, isotopic methods have been widely used in a number of coordinated research projects and technical cooperation projects of the International Atomic Energy Agency's Nutrition Programme. The doubly labeled water technique combines the use of the stable isotopes oxygen-18 and hydrogen-2 (deuterium) to measure total energy expenditure in free-living human subjects, and to investigate the magnitude and causes of both undernutrition and the emergence of obesity in developing countries. The deuterium dilution technique is a reliable tool to measure breastmilk intake and thereby infant growth and development. In collaboration with the World Health Organization's Growth Monitoring Program, this technique is being used to generate new data on growth standards for children in developing countries. This technique is also used in the measurement of body composition by the estimation of lean body mass and fat mass in individuals. Stable isotopes of iron and zinc have been successfully used to assess the nutritional impact of several nationwide food supplementation-programs conducted on pregnant and lactating women and children in both industrialized and developing countries. Isotopic techniques are especially suitable for monitoring changes in body composition, energy metabolism, and mineral status (with particular reference to osteoporosis) in the elderly. Nuclear methods have also served to develop models for a physiological reference man in Asia in support of radiological health and safety issues, for establishing elemental composition of foods, and for measurement of pollutants in the environment.

Isotopic reconstruction of ancient human migrations: A comprehensive Sr isotope reference database for France and the first case study at Tumulus de Sables, south-western France

Science.gov (United States)

Willmes, M.; Boel, C.; Grün, R.; Armstrong, R.; Chancerel, A.; Maureille, B.; Courtaud, P.

2012-04-01

Strontium isotope ratios (87Sr/86Sr) can be used for the reconstruction of human and animal migrations across geologically different terrains. Sr isotope ratios in rocks are a product of age and composition and thus vary between geologic units. From the eroding environment Sr is transported into the soils, plants and rivers of a region. Humans and animals incorporate Sr from their diet into their bones and teeth, where it substitutes for calcium. Tooth enamel contains Sr isotope signatures acquired during childhood and is most resistant to weathering and overprinting, while the dentine is often diagenetically altered towards the local Sr signature. For the reconstruction of human and animal migrations the tooth enamel 87Sr/86Sr ratio is compared to the Sr isotope signature in the vicinity of the burial site and the surrounding area. This study focuses on the establishment of a comprehensive reference map of bioavailable 87Sr/86Sr ratios for France. In a next step we will compare human and animal teeth from key archaeological sites to this reference map to investigate mobility. So far, we have analysed plant and soil samples from ~200 locations across France including the Aquitaine basin, the western and northern parts of the Paris basin, as well as three transects through the Pyrenees Mountains. The isotope data, geologic background information (BRGM 1:1M), field images, and detailed method descriptions are available through our online database iRhum (http://rses.anu.edu.au/research/ee). This database can also be used in forensic studies and food sciences. As an archaeological case study teeth from 16 adult and 8 juvenile individuals were investigated from an early Bell Beaker (2500-2000 BC) site at Le Tumulus des Sables, south-west France (Gironde). The teeth were analysed for Sr isotope ratios using laser ablation ICP-MS. Four teeth were also analysed using solution ICP-MS, which showed a significant offset to the laser ablation results. This requires further

Isotope enrichment

International Nuclear Information System (INIS)

Garbuny, M.

1979-01-01

The invention discloses a method for deriving, from a starting material including an element having a plurality of isotopes, derived material enriched in one isotope of the element. The starting material is deposited on a substrate at less than a critical submonatomic surface density, typically less than 10 16 atoms per square centimeter. The deposit is then selectively irradiated by a laser (maser or electronic oscillator) beam with monochromatic coherent radiation resonant with the one isotope causing the material including the one istope to escape from the substrate. The escaping enriched material is then collected. Where the element has two isotopes, one of which is to be collected, the deposit may be irradiated with radiation resonant with the other isotope and the residual material enriched in the one isotope may be evaporated from the substrate and collected

Validation of multi-element isotope dilution ICPMS for the analysis of basalts

Energy Technology Data Exchange (ETDEWEB)

Willbold, M.; Jochum, K.P.; Raczek, I.; Amini, M.A.; Stoll, B.; Hofmann, A.W. [Max-Planck-Institut fuer Chemie, Mainz (Germany)

2003-09-01

In this study we have validated a newly developed multi-element isotope dilution (ID) ICPMS method for the simultaneous analysis of up to 12 trace elements in geological samples. By evaluating the analytical uncertainty of individual components using certified reference materials we have quantified the overall analytical uncertainty of the multi-element ID ICPMS method at 1-2%. Individual components include sampling/weighing, purity of reagents, purity of spike solutions, calibration of spikes, determination of isotopic ratios, instrumental sources of error, correction of mass discrimination effect, values of constants, and operator bias. We have used the ID-determined trace elements for internal standardization to improve indirectly the analysis of 14 other (mainly mono-isotopic trace elements) by external calibration. The overall analytical uncertainty for those data is about 2-3%. In addition, we have analyzed USGS and MPI-DING geological reference materials (BHVO-1, BHVO-2, KL2-G, ML3B-G) to quantify the overall bias of the measurement procedure. Trace element analysis of geological reference materials yielded results that agree mostly within about 2-3% relative to the reference values. Since these results match the conclusions obtained by the investigation of the overall analytical uncertainty, we take this as a measure for the validity of multi-element ID ICPMS. (orig.)

Development of SI-traceable C-peptide certified reference material NMIJ CRM 6901-a using isotope-dilution mass spectrometry-based amino acid analyses.

Science.gov (United States)

Kinumi, Tomoya; Goto, Mari; Eyama, Sakae; Kato, Megumi; Kasama, Takeshi; Takatsu, Akiko

2012-07-01

A certified reference material (CRM) is a higher-order calibration material used to enable a traceable analysis. This paper describes the development of a C-peptide CRM (NMIJ CRM 6901-a) by the National Metrology Institute of Japan using two independent methods for amino acid analysis based on isotope-dilution mass spectrometry. C-peptide is a 31-mer peptide that is utilized for the evaluation of β-cell function in the pancreas in clinical testing. This CRM is a lyophilized synthetic peptide having the human C-peptide sequence, and contains deamidated and pyroglutamylated forms of C-peptide. By adding water (1.00 ± 0.01) g into the vial containing the CRM, the C-peptide solution in 10 mM phosphate buffer saline (pH 6.6) is reconstituted. We assigned two certified values that represent the concentrations of total C-peptide (mixture of C-peptide, deamidated C-peptide, and pyroglutamylated C-peptide) and C-peptide. The certified concentration of total C-peptide was determined by two amino acid analyses using pre-column derivatization liquid chromatography-mass spectrometry and hydrophilic chromatography-mass spectrometry following acid hydrolysis. The certified concentration of C-peptide was determined by multiplying the concentration of total C-peptide by the ratio of the relative area of C-peptide to that of the total C-peptide measured by liquid chromatography. The certified value of C-peptide (80.7 ± 5.0) mg/L represents the concentration of the specific entity of C-peptide; on the other hand, the certified value of total C-peptide, (81.7 ± 5.1) mg/L can be used for analyses that does not differentiate deamidated and pyroglutamylated C-peptide from C-peptide itself, such as amino acid analyses and immunochemical assays.

Nanoporous materials for hydrogen storage and H2/D2 isotope separation

International Nuclear Information System (INIS)

Oh, Hyunchul

2014-01-01

This thesis presents a study of hydrogen adsorption properties at RT with noble metal doped porous materials and an efficient separation of hydrogen isotopes with nanoporous materials. Most analysis is performed via thermal desorption spectra (TDS) and Sieverts-type apparatus. The result and discussion is presented in two parts; Chapter 4 focuses on metal doped nanoporous materials for hydrogen storage. Cryogenic hydrogen storage by physisorption on porous materials has the advantage of high reversibility and fast refuelling times with low heat evolution at modest pressures. At room temperature, however, the physisorption mechanism is not abEle to achieve enough capacity for practical application due to the weak van der Waals interaction, i.e., low isosteric heats for hydrogen sorption. Recently, the ''spillover'' effect has been proposed by R. Yang et al. to enhance the room temperature hydrogen storage capacity. However, the mechanism of this storage enhancement by decoration of noble metal particles inside high surface area supports is not yet fully understood and still under debate. In this chapter, noble metal (Pt / Pd) doped nanoporous materials (i.e. porous carbon, COFs) have been investigated for room temperature hydrogen storage. Their textural properties and hydrogen storage capacity are characterized by various analytic techniques (e.g. SEM, HRTEM, XRD, BET, ICP-OES, Thermal desorption spectra, Sievert's apparatus and Raman spectroscopy). Firstly, Pt-doped and un-doped templated carbons possessing almost identical textural properties were successfully synthesized via a single step wet impregnation method. This enables the study of Pt catalytic activities and hydrogen adsorption kinetics on porous carbons at ambient temperature by TDS after H 2 /D 2 gas exposure and PCT measurement, respectively. While the H 2 adsorption kinetics in the microporous structure is enhanced by Pt catalytic activities (spillover), only a small enhancement of the hydrogen

Recent development in isotope ratio mass spectrometry

International Nuclear Information System (INIS)

Platzner, I.

1992-01-01

Within the limited of this review the following topics will be briefly discussed: a) Accuracy, precision, internal relative standard deviation (RISD) and external relative standard deviation (RESD) of isotope ratio measurements. With advanced instrumentation and use of standard reference materials, high accuracy and RESD = 0.002% (or better) may be achieved; b) The advantages of modern automatic isotope ratio mass spectrometer are briefly described. Computer controlled operation and data acquisition, and multiple ion collection are the recent important improvement; c) The isotopic fractionation during the course of isotope ratio measurement is considered as a major source of errors in thermal ionization of metallic elements. The phenomenon in strontium, neodymium, uranium, lead and calcium and methods to correct the measured data are discussed; d) Applications of isotope ratio mass spectrometry in atomic weight determinations, the isotope dilution technique, isotope geology, and isotope effects in biological systems are described together with specific applications in various research and technology area. (author)

Assessment of fibrous insulation materials for the selenide isotope generator system

International Nuclear Information System (INIS)

Wei, G.C; Tennery, V.J.

1977-11-01

Fibrous insulations for use in the converter and the heat source of the radioisotope-powered, selenide element, thermoelectric generator (selenide isotope generator) are assessed. The most recent system design and material selection basis is presented. Several fibrous insulation materials which have the potential for use as load-bearing or nonload-bearing thermal insulations are reviewed, and thermophysical properties supplied by manufacturers or published in the literature are presented. Potential problems with the application of fibrous insulations in the selenide isotope generator are as follows: compatibility with graphite, the thermoelectric elements, and the isolation hot frame; devitrification, grain growth, and sintering with an accompanying degradation of insulation quality; impurity diffusion from the insulation to adjoining structures; outgassing and storage of fibrous materials. Areas in which thermophysical data or quantitative information on the insulation and structural stability is lacking are identified

Determination of carbon-14 in environmental level, solid reference materials

Energy Technology Data Exchange (ETDEWEB)

Blowers, Paul, E-mail: paul.blowers@cefas.co.uk [Cefas Lowestoft Laboratory, Pakefield Road, Lowestoft, Suffolk, NR33 0HT (United Kingdom); Caborn, Jane, E-mail: jane.a.caborn@nnl.co.uk [NNL, Springfields, Salwick, Preston, Lancashire, PR4 0XJ (United Kingdom); Dell, Tony [Veterinary Laboratories Agency, New Haw, Addlestone, Surrey, KT15 3NB (United Kingdom); Gingell, Terry [DSTL, Radiation Protection Services, Crescent Road, Alverstoke, Gosport, Hants, PO12 2DL (United Kingdom); Harms, Arvic [National Physical Laboratory, Hampton Road, Teddington, Middlesex, TW11 0LW (United Kingdom); Long, Stephanie [Radiological Protection Institute of Ireland, 3 Clonskeagh Square, Clonskeagh Road, Dublin 14, Ireland (United Kingdom); Sleep, Darren [Centre for Ecology and Hydrology, Lancaster Environment Centre, Library Avenue, Bailrigg, Lancaster, LA1 4AP (United Kingdom); Stewart, Charlie [UKAEA (Waste Management Group), Chemical Support Services, D1310/14, Dounreay, Thurso, Caithness, KW14 7TZ (United Kingdom); Walker, Jill [Radiocarbon Dating, The Old Stables, East Lockinge, Wantage, Oxon OX12 8QY (United Kingdom); Warwick, Phil E. [GAU-Radioanalytical, National Oceanography Centre Southampton, European Way, Southampton, SO14 3ZH (United Kingdom)

2011-10-15

An intercomparison exercise to determine the {sup 14}C activity concentrations in a range of solid, environmental level materials was conducted between laboratories in the UK. IAEA reference materials, C2, C6 and C7, and an in-house laboratory QA material were dispatched in 2006 to ten laboratories comprising of members of the Analyst Informal Working Group (AIWG) and one other invited party. The laboratories performed the determinations using a number of techniques, and using the results each one was evaluated in terms of levels of precision, sensitivity and limits of detection. The results of the study show that all techniques are capable of successfully analysing {sup 14}C in environmental level materials, however, a shortage of certified environmental reference materials exists. The suitability of the IAEA reference materials and other material for use as reference materials was also assessed.

Determination of carbon-14 in environmental level, solid reference materials

International Nuclear Information System (INIS)

Blowers, Paul; Caborn, Jane; Dell, Tony; Gingell, Terry; Harms, Arvic; Long, Stephanie; Sleep, Darren; Stewart, Charlie; Walker, Jill; Warwick, Phil E.

2011-01-01

An intercomparison exercise to determine the 14 C activity concentrations in a range of solid, environmental level materials was conducted between laboratories in the UK. IAEA reference materials, C2, C6 and C7, and an in-house laboratory QA material were dispatched in 2006 to ten laboratories comprising of members of the Analyst Informal Working Group (AIWG) and one other invited party. The laboratories performed the determinations using a number of techniques, and using the results each one was evaluated in terms of levels of precision, sensitivity and limits of detection. The results of the study show that all techniques are capable of successfully analysing 14 C in environmental level materials, however, a shortage of certified environmental reference materials exists. The suitability of the IAEA reference materials and other material for use as reference materials was also assessed.

Use of gamma spectrometry for analysis of three reference materials

International Nuclear Information System (INIS)

Kinova, L.

2004-01-01

All reference materials (Reference material A: weight = 49.23 g; Reference material B: weight = 36.08 g; Reference material C: weight = 26.18 g) were packed in 50 cm 3 polypropylene vials, sealed and measured consecutively three times at intervals of the average of 25 days. Low background gamma spectrometry system: HPGe detector with high energy resolution (FWHM for 1332 KeV of Co-60 is 1.9 KeV, Relative counting efficiency for the same energy is 21 %) was used. Results: All materials are of low activity and must be measured for a long time.The highest specific activity of a man-made radionuclides Cs-137 and Am-241 is in the material A. An instrumentally measurable activity of Pb-210 also can be observed in this material. Medium values are in the material B. The reference material C according to the specific activity seems to be a low natural radioactivity material with highest activity of natural nuclides Th-232 and Pa-234 (progeny of U-238). Conclusions: Gamma spectrometry is an useful tool for initial measurement of materials with low radioactivity. Such measurements give an orientation for the nuclides content and approximate activity in the material for the following radiochemical determinations

Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

International Nuclear Information System (INIS)

Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

2009-01-01

This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

An outline of reference materials for analysis techniques in China

International Nuclear Information System (INIS)

Zhang Yuanxun; Qian Yine; Zhang Yongping; Tong Yongpeng

1994-01-01

This paper provides background information on the development in the field of reference materials in China. The major considerations in development of reference materials include homogeneity, stability, handling procedures and certification. Further it discusses the plans for development in the near future specific natural-matrix reference materials containing low levels of trace elements and having high degree of homogeneity

An outline of reference materials for analysis techniques in China

Energy Technology Data Exchange (ETDEWEB)

Yuanxun, Zhang; Yine, Qian; Yongping, Zhang; Yongpeng, Tong [Shanghai Institute of Nuclear Research, Academia Sinica (China)

1994-07-01

This paper provides background information on the development in the field of reference materials in China. The major considerations in development of reference materials include homogeneity, stability, handling procedures and certification. Further it discusses the plans for development in the near future specific natural-matrix reference materials containing low levels of trace elements and having high degree of homogeneity.

Geochemical and isotopic signatures for the identification of ...

Indian Academy of Sciences (India)

In case of stable isotopes of hydrogen and oxygen in water samples, the reference material is a stan- dard ocean ..... Aquifers – Modeling, Monitoring and Management,. Morocco .... Israel: Its bearing on the water crisis in the country;. J. Hydrol.

A compilation of silicon, rare earth element and twenty-one other trace element concentrations in the natural river water reference material SLRS-5 (NRC-CNRC)

International Nuclear Information System (INIS)

Yeghicheyan, Delphine; Cloquet, Christophe; Bossy, Cecile; Bouhnik Le Coz, Martine; Douchet, Chantal; Granier, Guy; Heimburger, Alexie; Losno, Remi; Lacan, Francois; Labatut, Marie; Pradoux, Catherine; Lanzanova, Aurelie; Candaudap, Frederic; Chmeleff, Jerome; Rousseau, Tristan C.C.; Seidel, Jean-Luc; Delpoux, Sophie; Tharaud, Mickael; Sivry, Yann; Sonke, Jeroen E.

2013-01-01

The natural river water certified reference material SLRS-5 (NRC-CNRC) was routinely analysed in this study for major and trace elements by ten French laboratories. Most of the measurements were made using ICP-MS. Because no certified values are assigned by NRC-CNRC for silicon and 35 trace element concentrations (rare earth elements, Ag, B, Bi, Cs, Ga, Ge, Li, Nb, P, Rb, Rh, Re, S, Sc, Sn, Th, Ti, Tl, W, Y and Zr), or for isotopic ratios, we provide a compilation of the concentrations and related uncertainties obtained by the participating laboratories. Strontium isotopic ratios are also given. (authors)

Development and use of reference materials and quality control materials

International Nuclear Information System (INIS)

2003-04-01

Current knowledge is summarized on correct use of commercially available certified reference materials (CRMs) and reference materials (RMs). Acknowledged are also the limitations and restrictions analysts have to face if they want to apply quality control. The concept of in-house RMs or quality control materials (QCMs) is advocated to supplement the use of CRMs for quality control purposes. On hand advice on how to select, prepare, characterize and use these QCMs is given from the experts' perspective. Several scenarios are described to make this concept widely applicable to: advanced laboratories with CRMs with validated analytical techniques available, laboratories with less experience and facilities, as well as cases were labile compounds and unstable matrices are involved. Each scenario considers different approaches to overcome the lack of appropriate CRMs and advise on the preparation of QCMs, which might fit the particular purpose

Development and use of reference materials and quality control materials

Energy Technology Data Exchange (ETDEWEB)

NONE

2003-04-01

Current knowledge is summarized on correct use of commercially available certified reference materials (CRMs) and reference materials (RMs). Acknowledged are also the limitations and restrictions analysts have to face if they want to apply quality control. The concept of in-house RMs or quality control materials (QCMs) is advocated to supplement the use of CRMs for quality control purposes. On hand advice on how to select, prepare, characterize and use these QCMs is given from the experts' perspective. Several scenarios are described to make this concept widely applicable to: advanced laboratories with CRMs with validated analytical techniques available, laboratories with less experience and facilities, as well as cases were labile compounds and unstable matrices are involved. Each scenario considers different approaches to overcome the lack of appropriate CRMs and advise on the preparation of QCMs, which might fit the particular purpose.

A new certified reference material for size analysis of nanoparticles

International Nuclear Information System (INIS)

Braun, Adelina; Kestens, Vikram; Franks, Katrin; Roebben, Gert; Lamberty, Andrée; Linsinger, Thomas P. J.

2012-01-01

A certified reference material, ERM-FD100, for quality assurance and validation of various nanoparticle sizing methods, was developed by the Institute for Reference Materials and Measurements. The material was prepared from an industrially sourced colloidal silica containing nanoparticles with a nominal equivalent spherical diameter of 20 nm. The homogeneity and stability of the candidate reference material was assessed by means of dynamic light scattering and centrifugal liquid sedimentation. Certification of the candidate reference material was based on a global interlaboratory comparison in which 34 laboratories participated with various analytical methods (DLS, CLS, EM, SAXS, ELS). After scrutinising the interlaboratory comparison data, 4 different certified particle size values, specific for the corresponding analytical method, could be assigned. The good comparability of results allowed the certification of the colloidal silica material for nanoparticle size analysis.

Reference materials for micro-analytical nuclear techniques

International Nuclear Information System (INIS)

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

1994-01-01

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

Biological and environmental reference materials in CENAM.

Science.gov (United States)

Arvizu-Torres, R; Perez-Castorena, A; Salas-Tellez, J A; Mitani-Nakanishi, Y

2001-06-01

Since 1994, when the NIST/NOAA Quality Assurance Program in Chemical Measurements was discussed in Queretaro, CENAM, the National Measurement Institute (NMI) of Mexico, has become involved in the development of reference materials. In the field of biological and environmental reference materials, in particular, the NORAMET collaboration program with NIST and NRC, and the North-American Environmental Cooperation signed among three free-trade treaty organizations, have greatly helped the development of the materials metrology program in the newly established CENAM. This paper describes some particularly significant efforts of CENAM in the development of biological and environmental reference materials, on the basis of inter-comparison studies organized with local and governmental environmental agencies of Mexico. In the field of water pollution CENAM has developed a practical proficiency testing (PT) scheme for field laboratories, as a part of registration by local government in the metropolitan area, according to the Mexican Ecological Regulation. The results from these eight PTs in the last 5 years have demonstrated that this scheme has helped ensure the reliability of analytical capability of more than 50 field laboratories in three states, Mexico, D.F., and the States of Mexico and Queretaro. Similar experience has been obtained for more than 70 service units of stack emission measurements in the three states in 1998 and 1999, as a result of the design of a PT scheme for reference gas mixtures. This PT scheme has been accomplished successfully by 30 analytical laboratories who provide monitoring services and perform research on toxic substances (Hg, methylmercury, PCB, etc.) in Mexico. To support these activities, reference samples have been produced through the NIST SRMs, and efforts have been made to increase CENAM's capability in the preparation of primary reference materials in spectrometric solutions and gas mixtures. Collaboration among NMIs has also

A manual for a Laboratory Information Management System (LIMS) for light stable isotopes

Science.gov (United States)

Coplen, Tyler B.

1998-01-01

The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program is presented herein. Major benefits of this system include (i) an increase in laboratory efficiency, (ii) reduction in the use of paper, (iii) reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) decreased errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for stable isotope laboratories. Since the original publication of the manual for LIMS for Light Stable Isotopes, the isotopes 3 H, 3 He, and 14 C, and the chlorofluorocarbons (CFCs), CFC-11, CFC-12, and CFC-113, have been added to this program.

Isotope correlation verification of analytical measurements for dissolver materials

International Nuclear Information System (INIS)

Satkowski, J.

1988-01-01

An independent verification of analytical results for accountability measurements of dissolver materials can be performed using the Iosotop Correlation Technique (ICT). ICT is based on the relationships that exist between the initial and final elemental concentration and isotopic abundances of the nuclear fuel. Linear correlation functions between isotopic ratios and plutonium/uranium ratios have been developed for specific reactor fuels. The application of these correlations to already existing analytical data provides a laboratory additional confidence in the reported results. Confirmation is done by a test of consistancy with historical data. ICT is being utilized with dissolver accountability measurements at the Savannah River Plant Laboratory. The application, implementation, and operating experience of this technique are presented

REFERENCE MATERIALS IN THE SPHERE OF USE OF ATOMIC ENERGY

Directory of Open Access Journals (Sweden)

V. A. Borisov

2015-01-01

Full Text Available The article describes the chronology of development of the system of reference materials in the nuclear industry of the Russian Federation. The basic documents used in the sphere of nuclear energy are described. The nomenclature of reference materials and feature of their application in the "Rosatom" is given. The prospects of development activities in the field of reference materials are formulated.

Development of natural matrix reference materials for monitoring environmental radioactivity

International Nuclear Information System (INIS)

Holmes, A.S.; Houlgate, P.R.; Pang, S.; Brookman, B.

1992-01-01

The Department of the Environment commissioned the Laboratory of the Government Chemist to carry out a contract on natural matrix reference materials. A survey of current availability of such materials in the western world, along with the UK's need, was conducted. Four suitable matrices were identified for production and validation. Due to a number of unforeseen problems with the collection, processing and validation of the materials, the production of the four identified reference materials was not completed in the allocated period of time. In the future production of natural matrix reference materials the time required, the cost and the problems encountered should not be underestimated. Certified natural matrix reference materials are a vital part of traceability in analytical science and without them there is no absolute method of checking the validity of measurement in the field of radiochemical analysis. (author)

Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products.

Science.gov (United States)

Boulyga, Sergei F; Heilmann, Jens; Heumann, Klaus G

2005-08-01

Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different 34S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured 34S/32S isotope ratio of the isotope-diluted sample remained constant-a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 microg g(-1) ('sulfur-free' premium gasoline) to 10.4 mg g(-1) (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 microg g(-1) and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level.

Preparation and analysis of a marble reference material

International Nuclear Information System (INIS)

Carmo Freitas, M.; Moens, L.; Seabra e Barros, J.

1988-01-01

A 7 kg stone of a Carrara marble was reduced to grains smaller than 100 μm, mixed and homogenized in order to prepare a marble reference material. The homogeneity was tested for 16 elements by instrumental neutron activation analysis (INAA). Through a one-way analysis of variance based on several analyses of each of 15 bottles and within the same bottle, it was concluded that the inter-bottle heterogeneity is not greater than the intra-bottle heterogeneity. Results on the concentration of major and trace elements in the marble reference material, obtained by different laboratories and different techniques, are given. The limestone certified reference material KALKSTEIN KH was used to evaluate measurement accuracy, to intercalibrate laboratories, and to provide compatibility of measurement data. (author) 10 refs.; 12 tabs

Preparation of in-house graphite reference material for boron

International Nuclear Information System (INIS)

Kumar, Sanjukta A.; Venkatesh, K.; Swain, Kallola K.; Manisha, V.; Kamble, Granthali S.; Pandey, Shailaja P.; Remya Devi, P.S.; Ghosh, M.; Verma, R.

2016-05-01

Graphite is extensively used in nuclear technology. Boron concentration in graphite is one of the important parameters that decide its acceptability for nuclear applications. Reliable analytical methods are essential for the determination of boron in graphite at concentration about 5 mg kg -1 . Reference materials are used for validation of existing analytical methods and developing new methodologies. In view of the importance of determination of boron in graphite and unavailability of graphite reference material, an In-house graphite reference material was prepared in Analytical Chemistry Division. Graphite source material was procured, processed to obtain powder of ≤ 75 μm (200 mesh) and bottled. Procedures were developed for the determination of boron in graphite using inductively coupled plasma optical emission spectrometry (ICPOES) and inductively coupled plasma mass spectrometry (ICPMS) techniques. Homogeneity testing was carried out on the bottled units and boron content along with the combined and expanded uncertainties were established. The assigned boron concentration in the In-house graphite reference material is (7.3±0.46) mg kg -1 . (author)

Certification of a niobium metal reference material for neutron dosimetry (EC nuclear reference material 526)

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.

1990-01-01

Niobium metal, of 99.999% nominal purity, in the form of 0.02 and 0.1 mm thick foil and of 0.5 mm diameter wire, has been certified for its tantalum mass fraction. The certified value of the tantalum mass fraction is 0.3 ± 0.09 mg. Kg -1 , and is based on 70 results obtained by six independent laboratories by neutron activation analysis or inductively coupled plasma mass spectrometry. The material is intended to be used as a reference material in neutron metrology

Reference material IAEA 413: Major, minor and trace elements in algae

International Nuclear Information System (INIS)

2010-01-01

Reference materials are a basic requirement for any sort of quantitative chemical and radiochemical analysis. Laboratories need them for calibration and quality control throughout their analytical work. The IAEA started to produce reference materials in the early 1960s to meet the needs of the analytical laboratories in its Member States that required reference materials for quality control of their measurements. The initial efforts were focused on the preparation of environmental reference materials containing anthropogenic radionuclides for use by those laboratories employing nuclear analytical techniques. These reference materials were characterized for their radionuclide content through interlaboratory comparison involving a core group of some 10 to 20 specialist laboratories. The success of these early exercises led the IAEA to extend its activities to encompass both terrestrial and marine reference materials containing primordial radionuclides and trace elements. Today, the IAEA has more than 90 reference materials and maintains a customer base of about 5000 members from more than 85 Member States. Within the frame of IAEA activities in production and certification of RM, this report describes the certification of the IAEA 413: Major, minor and trace elements in algae. Details are given on methodologies and data evaluation

Approach for domestic preparation of standard material (LSD spike) for isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Ishikawa, Fumitaka; Sumi, Mika; Chiba, Masahiko; Suzuki, Toru; Abe, Tomoyuki; Kuno, Yusuke

2008-01-01

The accountancy analysis of the nuclear fuel material at Plutonium Fuel Development Center of JAEA is performed by isotope dilution mass spectrometry (IDMS; Isotope Dilution Mass Spectrometry). IDMS requires the standard material called LSD spike (Large Size Dried spike) which is indispensable for the accountancy in the facilities where the nuclear fuel materials are handled. Although the LSD spike and Pu source material have been supplied from foreign countries, the transportation for such materials has been getting more difficult recently. This difficulty may affect the operation of nuclear facilities in the future. Therefore, research and development of the domestic LSD spike and base material has been performed at JAEA. Certification for such standard nuclear materials including spikes produced in Japan is being studied. This report presents the current status and the future plan for the technological development. (author)

Hydrogen isotope permeation in elastomeric materials

International Nuclear Information System (INIS)

Steinmeyer, R.H.; Braun, J.D.

1976-01-01

The permeabilities of elastomeric and polymeric materials to hydrogen isotopes were measured at room temperature. The technique for measuring permeation rates is based on the following constant-volume method: a fixed pressure of gas is applied to one side of the specimen to be studied and the permeability constant is determined from the observed rate of pressure increase in an initially evacuated volume on the other side of the specimen. Permeability constants for hydrogen, deuterium, and tritium were measured for Mylar, Teflon, Kapton, Saran, Buna-N, and latex rubber. Results were compared with literature values for hydrogen and deuterium where available and showed excellent agreement

The urgent requirement for new radioanalytical certified reference materials for nuclear safeguards, forensics, and consequence management

International Nuclear Information System (INIS)

Inn, K.G.W.; Martin Johnson, Jr.C.; Warren Oldham; Lav Tandon; Simon Jerome; Thomas Schaaff; Robert Jones; Daniel Mackney; Pam MacKill; Brett Palmer

2013-01-01

A multi-agency workshop was held from 25 to 27 August 2009, at the National Institute of Standards and Technology (NIST), to identify and prioritize the development of radioanalytical Certified Reference Materials (CRMs, generally provided by National Metrology Institutes; Standard Reference Materials, a CRM issued by NIST) for field and laboratory nuclear measurement methods to be used to assess the consequences of a domestic or international nuclear event. Without these CRMs, policy makers concerned with detecting proliferation and trafficking of nuclear materials, attribution and retribution following a nuclear event, and public health consequences of a nuclear event would have difficulty making decisions based on analytical data that would stand up to scientific, public, and judicial scrutiny. The workshop concentrated on three areas: post-incident Improvised Nuclear Device (IND) nuclear forensics, safeguard materials characterization, and consequence management for an IND or a Radiological Dispersion Device detonation scenario. The workshop identified specific CRM requirements to fulfill the needs for these three measurement communities. Of highest priority are: (1) isotope dilution mass spectrometry standards, specifically 233 U, 236 gNp, 244 Pu, and 243 Am, used for quantitative analysis of the respective elements that are in critically short supply and in urgent need of replenishment and certification; (2) CRMs that are urgently needed for post-detonation debris analysis of actinides and fission fragments, and (3) CRMs used for destructive and nondestructive analyses for safeguards measurements, and radioisotopes of interest in environmental matrices. (author)

Instrumental neutron activation analysis of marine sediment in-house reference material

International Nuclear Information System (INIS)

Nazaratul Ashifa Abdullah Salim; Mohd Suhaimi Hamzah; Mohd Suhaimi Elias; Siong, W.B.; Shamsiah Abdul Rahman; Azian Hashim; Shakirah Abdul Shukor

2013-01-01

Reference materials play an important role in demonstrating the quality and reliability of analytical data. The advantage of using in-house reference materials is that they provide a relatively cheap option as compared to using commercially available certified reference material (CRM) and can closely resemble the laboratory routine test sample. A marine sediment sample was designed as an in-house reference material, in the framework of quality assurance and control (QA/QC) program of the Neutron Activation Analysis (NAA) Laboratory at Nuclear Malaysia. The NAA technique was solely used for the homogeneity test of the marine sediment sample. The CRM of IAEA- Soil 7 and IAEA- SL1 (Lake Sediment) were applied in the analysis as compatible matrix based reference materials for QA purposes. (Author)

Certification of an aluminium metal reference material for neutron dosimetry (EC nuclear reference material 523)

International Nuclear Information System (INIS)

Pauwels, J.; Ingelbrecht, C.

1990-01-01

Aluminium metal of > 99.999% nominal purity in the form of 0.1 mm and 1 mm thick foil and of 1 mm diameter wire has been certified for its sodium mass fraction. The certified value of the sodium mass fraction ( -1 ) is based on 21 results from three laboratories using two different methods, which are neutron activation analysis and atomic absorption spectrometry. The overall purity was estimated using spark source mass spectrometry and neutron activation analysis. The material is intended to be used as a reference material in neutron metrology

Production of candidate natural matrix reference materials for micro-analytical techniques

International Nuclear Information System (INIS)

Zeisler, R.; Fajgelj, A.; Zeiller, E.

2002-01-01

Homogeneity is considered to be the most vital prerequisite for a certified reference material (CRM); more stringent requirements exist for the analysis of small subsamples. Many of the natural matrix CRMs are prepared from bulk samples by grinding and milling them to a certain particle size, which is expected to provide a more homogenous material; however recommended sample sizes for biological and environmental reference materials are found to be more than 100 mg. Since the milling of materials is costly and has some drawbacks, natural materials that already occur as small particles such as air particulate matter, certain sediments, and cellular biological materials may form the basis of the required reference materials. The nature of these materials, i.e. naturally occurring particles, may provide ideal model reference material. We describe here the production of the materials and preliminary tests, the evaluation for the micro-analytical techniques

Determination of the hydrogen isotopic compositions of organic materials and hydrous minerals using thermal combustion laser spectroscopy.

Science.gov (United States)

Koehler, Geoff; Wassenaar, Leonard I

2012-04-17

Hydrogen isotopic compositions of hydrous minerals and organic materials were measured by combustion to water, followed by optical isotopic analysis of the water vapor by off-axis integrated cavity output spectroscopy. Hydrogen and oxygen isotopic compositions were calculated by numerical integration of the individual isotopologue concentrations measured by the optical spectrometer. Rapid oxygen isotope exchange occurs within the combustion reactor between water vapor and molecular oxygen so that only hydrogen isotope compositions may be determined. Over a wide range in sample sizes, precisions were ±3-4 per mil. This is comparable but worse than continuous flow-isotope ratio mass spectroscopy (CF-IRMS) methods owing to memory effects inherent in water vapor transfer. Nevertheless, the simplicity and reduced cost of this analysis compared to classical IRMS or CF-IRMS methods make this an attractive option to determine the hydrogen isotopic composition of organic materials where the utmost precision or small sample sizes are not needed.

Certification of butyltins and phenyltins in marine sediment certified reference material by species-specific isotope-dilution mass spectrometric analysis using synthesized {sup 118}Sn-enriched organotin compounds

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi [National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, National Metrology Institute of Japan (NMIJ), Tsukuba, Ibaraki (Japan)

2007-04-15

A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with {gamma}-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS) - SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with {sup 118}Sn-enriched organotin compounds synthesized from {sup 118}Sn-enriched metal used as a spike. The {sup 118}Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the {sup 118}Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44{+-}3 {mu}g kg{sup -1} as Sn, DBT 51 {+-} 2 {mu}g kg{sup -1} as Sn, MBT 67 {+-} 3 {mu}g kg{sup -1} as Sn, TPhT 6.9 {+-} 1.2 {mu}g kg{sup -1} as Sn, and DPhT 3.4 {+-} 1.2 {mu}g kg{sup -1} as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds. (orig.)

Isotope methods for the control of food products and beverages

Energy Technology Data Exchange (ETDEWEB)

Guillou, C; Reniero, F [Commission of the European Communities, Joint Research Centre, Ispra (Italy)

2001-10-01

The measurement of the stable isotope contents provides useful information for the detection of many frauds in food products. Nuclear magnetic resonance (NMR) and isotopic ratio mass spectroscopy (IRMS) are the two main analytical techniques used for the determination of stable isotope contents in food products. These analytical techniques have been considerably improved in the last years offering wider possibilities of applications for food analysis. A review of the applications for the control of food products and beverages is presented. The need for new reference materials is discussed. (author)

Isotope methods for the control of food products and beverages

International Nuclear Information System (INIS)

Guillou, C.; Reniero, F.

2001-01-01

The measurement of the stable isotope contents provides useful information for the detection of many frauds in food products. Nuclear magnetic resonance (NMR) and isotopic ratio mass spectroscopy (IRMS) are the two main analytical techniques used for the determination of stable isotope contents in food products. These analytical techniques have been considerably improved in the last years offering wider possibilities of applications for food analysis. A review of the applications for the control of food products and beverages is presented. The need for new reference materials is discussed. (author)

Development of сertified reference materials set for opened porosity of solid substances and materials (imitators

Directory of Open Access Journals (Sweden)

E. P. Sobina

2016-01-01

Full Text Available The article deals with data of research for development of certified reference materials set for opened porosity of solid substances and materials (imitators (OPTB SO UNIIM Set Certified Reference Materials GSO 10583-2015. The certified values of opened porosity of metal cylinders were established by the method of hydrostatic weighing before and after boring of holes in. The certified reference materials are intended for calibration and verification of measuring instruments of opened porosity, based on the Boyle - Mariotte's law.

Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products

Energy Technology Data Exchange (ETDEWEB)

Boulyga, Sergei F.; Heilmann, Jens; Heumann, Klaus G. [Johannes Gutenberg-University Mainz (Germany). Institute of Inorganic Chemistry and Analytical Chemistry

2005-08-01

Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different {sup 34}S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured {sup 34}S/{sup 32}S isotope ratio of the isotope-diluted sample remained constant - a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 {mu}g g{sup -1} ('sulfur-free' premium gasoline) to 10.4 mg g{sup -1} (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 {mu}g g{sup -1} and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level. (orig.)

Effectiveness of different pre-treatments in recovering pre-burial isotopic ratios of charred plants.

Science.gov (United States)

Brinkkemper, O; Braadbaart, F; van Os, B; van Hoesel, A; van Brussel, A A N; Fernandes, R

2018-02-15

Isotopic analysis of archaeological charred plant remains offers useful archaeological information. However, adequate sample pre-treatment protocols may be necessary to provide a contamination-free isotopic signal while limiting sample loss and achieving a high throughput. Under these constraints, research was undertaken to compare the performance of different pre-treatment protocols. Charred archaeological plant material was selected for isotopic analysis (δ 13 C and δ 15 N values) by isotope ratio mass spectrometry from a variety of plant species, time periods and soil conditions. Preservation conditions and the effectiveness of cleaning protocols were assessed through Fourier transform infrared spectroscopy and X-ray fluorescence (XRF) spectrometry. An acid-base-acid protocol, successfully employed in radiocarbon dating, was used to define a contamination-free isotopic reference. Acid-base-acid isotopic measurements were compared with those obtained from untreated material and an acid-only protocol. The isotopic signals of untreated material and the acid-only protocol typically did not differ more than 1‰ from those of the acid-base-acid reference. There were no significant isotopic offsets between acid-base-acid and acid-only or untreated samples. Sample losses in the acid-base-acid protocol were on average 50 ± 17% (maximum = 98.4%). Elemental XRF measurements showed promising results in the detection of more contaminated samples albeit with a high rate of false positives. For the large range of preservation conditions described in the study, untreated charred plant samples, water cleaned of sediments, provide reliable stable isotope ratios of carbon and nitrogen. The use of pre-treatments may be necessary under different preservation conditions or more conservative measurement uncertainties should be reported. Copyright © 2017 John Wiley & Sons, Ltd.

Reference materials and their role in quality assurance in environmental monitoring

International Nuclear Information System (INIS)

Cortes, Eduardo

2002-01-01

The importance of a good and routine quality control procedure for the analyses of environmental samples is presented. The use of Reference Materials as one simple procedure for validating analytical methodologies and determining the accuracy of analytical data is emphasized. The quality of the reference materials is also discussed as well as their selection and correct use. The convenience of preparing 'in-house' reference materials is discussed and attention is called to relevant aspects to be considered. An example of the preparation of a reference material is presented and some aspects of the procedure are discussed. (author)

The development of maple technology for materials testing, isotope production, and neutron-beam applications

International Nuclear Information System (INIS)

Lidstone, R.F.; Gillespie, G.E.; Lee, A.G.; Bishop, W.E.

1996-01-01

AECL has been developing MAPLE technology to meet Canadian and international requirements for high-performance research reactors. MAPLE refers to a family of open-tank-in-pool reactors that employ compact H 2 O-cooled cores within D 2 O vessels to efficiently furnish neutrons to various types of irradiation facilities. The initial focus was on a 10-MW t Canadian facility for radioisotope production, the HANARO multipurpose-reactor project, and an associated R and D program. Recently, AECL began to develop the concept for a new Canadian Irradiation Research Facility (IRF) which will support the continued evolution of CANDU (CANadian Deuterium Uranium) technology and generate neutrons for basic and applied materials science. Additionally, AECL is currently developing a standardized MAPLE research-centre design with integrated neutron-application facilities; various reactor-core options have been optimized for different combinations of utilization: a 19-site core for neutron-beam applications and ancillary isotope production, a 31-site core for multipurpose materials testing and neutron-beam applications, and twin 18-site cores for high-flux neutron-beam applications. (author)

Calcium Isotope Analysis by Mass Spectrometry

Science.gov (United States)

Boulyga, S.; Richter, S.

2010-12-01

The variations in the isotopic composition of calcium caused by fractionation in heterogeneous systems and by nuclear reactions can provide insight into numerous biological, geological, and cosmic processes, and therefore isotopic analysis finds a wide spectrum of applications in cosmo- and geochemistry, paleoclimatic, nutritional, and biomedical studies. The measurement of calcium isotopic abundances in natural samples has challenged the analysts for more than three decades. Practically all Ca isotopes suffer from significant isobaric interferences, whereas low-abundant isotopes can be particularly affected by neighboring major isotopes. The extent of natural variations of stable isotopes appears to be relatively limited, and highly precise techniques are required to resolve isotopic effects. Isotope fractionation during sample preparation and measurements and instrumental mass bias can significantly exceed small isotope abundance variations in samples, which have to be investigated. Not surprisingly, a TIMS procedure developed by Russell et al. (Russell et al., 1978. Geochim Cosmochim Acta 42: 1075-1090) for Ca isotope measurements was considered as revolutionary for isotopic measurements in general, and that approach is used nowadays (with small modifications) for practically all isotopic systems and with different mass spectrometric techniques. Nevertheless, despite several decades of calcium research and corresponding development of mass spectrometers, the available precision and accuracy is still not always sufficient to achieve the challenging goals. This presentation discusses figures of merits of presently used analytical methods and instrumentation, and attempts to critically assess their limitations. Additionally, the availability of Ca isotope reference materials will be discussed.

Preparation of isotopic molybdenum foils utilizing small quantities of material

Science.gov (United States)

Lipski, A. R.; Lee, L. L.; Liang, J. F.; Mahon, J. C.

1993-09-01

A simple method utilizing a small amount of isotopic material for production of molybdenum foils is discussed. An e-gun is used in the procedure. The Mo powder undergoes reduction-sintering and melting-solidifying steps leading to the creation of a metallic droplet suitable for further cold rolling or vacuum deposition.

Studies in the determination of lead isotope ratios by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Date, A.R.; Yuk Ying Cheung

1987-01-01

The application of ICP-MS to the determination of lead isotope ratios in geological materials is described. Data presented for a series of lead mineral concentrates are compared with reference values obtained by conventional solid source thermal ionisation mass spectrometry. The simultaneous determination of lead isotope ratios and trace elements is carried out in a rapid analysis mode. The application of an electrothermal vaporisation technique for small solution aliquots is described. Lead isotope ratio data for the United States Geological Survey standard reference silicate rock BCR-1, obtained without separation of lead from the matrix, are compared with previously published values obtained after separation. (author)

Recent developments in the field of environmental reference materials at the JRC Ispra.

Science.gov (United States)

Muntau, H

2001-06-01

The production of reference materials for environmental analysis started in the Joint Research Centre at Ispra/Italy in 1972 with the objective of later certification by the BCR, but for obvious budget reasons only a fraction of the total production achieved at Ispra ever reached certification level, although all materials were produced according to the severe quality requirements requested for certified reference materials. Therefore, the materials not destinated to certification are in growing demand as inter-laboratory test materials and as laboratory reference materials, for internal quality control, e.g., by control charts. The history of reference material production within the Joint Research Centre is briefly reviewed and the latest additions described. New developments such as micro-scale reference materials intended for analytical methods requiring sample intakes at milligram or sub-milligram level and therefor not finding supply on the reference material market, and "wet" environmental reference materials, which meet more precisely the "real-world" environmental analysis conditions, are presented and the state-of-the-art discussed.

Determination of ancient ceramics reference material by neutron activation analysis

International Nuclear Information System (INIS)

Li Huhou; Sun Jingxin; Wang Yuqi; Lu Liangcai

1986-01-01

Contents of trace elements in the reference material of ancient ceramics (KPS-1) were determined by means of activation analysis, using thermal neutron irradiation produced in nuclear reactor. KPS-1 favoured the analysis of ancient ceramics because it had not only many kinds of element but also appropriate contents of composition. The values presented here are reliable within the experimental precision, and have shown that the reference material had a good homogeneity. So KPS-1 can be used as a suitable reference material for the ancient ceramics analysis

Direct calibration of GC/MS systems using SRM (Standard Reference Material) gas cylinders. Project report, January 1984-August 1985

International Nuclear Information System (INIS)

Byrd, G.D.; Richie, K.L.; Sniegoski, L.T.; White, E.

1985-10-01

A cryogenic trapping system has been developed for use in calibrating GC/MS systems for the analysis of volatile organic compounds. This system provides for direct Standard Reference Material (SRM) traceability on data generated on gaseous samples. The cryogenic trap is a coil of stainless steel tubing immersed in a cryogen to trap and preconcentrate organic species present in a gaseous sample. The trap also contains a heated injection port for the addition of isotopically labeled compounds for use in isotope dilution measurements. The first part of this research is concerned with the development of IDMS as an independent method for the quantification of analytes in gaseous samples to be used as standards. Results are presented for the determination of bromobenzene in nitrogen at nominal concentrations of 1 and 25 ppb. In the second part of the research, a calibration curve method was developed for using these standards in auditing the performance of GC/MS systems

Automatic isotope gas analysis of tritium labelled organic materials Pt. 1

International Nuclear Information System (INIS)

Gacs, I.; Mlinko, S.

1978-01-01

A new automatic procedure developed to convert tritium in HTO hydrogen for subsequent on-line gas counting is described. The water containing tritium is introduced into a column prepared from molecular sieve-5A and heated to 550 deg C. The tritium is transferred by isotopic exchange into hydrogen flowing through the column. The radioactive gas is led into an internal detector for radioactivity measurement. The procedure is free of memory effects, provides quantitative recovery with analytical reproducibility better than 0.5% rel. at a preset number of counts. The experimental and analytical results indicate that isotopic exchange between HTO and hydrogen over a column prepared from alumina or molecular sieve-5A can be successfully applied for the quantitative transfer of tritium from HTO into hydrogen for on-line gas countinq. This provides an analytical procedure for the automatic determination of tritium in water with an analytical reproducibility better than 0.5% rel. The exchange process will also be suitable for rapid tritium transfer from water formed during the decomposition of tritium-labelled organic compounds or biological materials. The application of the procedure in automatic isotope gas analysis of organic materials labelled with tritium will be described in subsequent papers (Parts II and III). (T.G.)

Oxygen Isotopes in Early Solar System Materials: A Perspective Based on Microbeam Analyses of Chondrules from CV Carbonaceous Chondrites

Science.gov (United States)

Jones, R. H.; Leshin, L. A.; Guan, Y.

2004-01-01

Some of the biggest challenges to understanding the early history of the solar system include determining the distribution of oxygen isotopes amongst materials that existed in the solar nebula, and interpreting the processes that might have resulted in the observed isotopic distributions. Oxygen isotope ratios in any individual mineral grain from a chondritic meteorite may be the cumulative product of a variety of processes, including stellar nucleosynthetic events, gas/solid interactions in the molecular cloud, mixing of independent isotopic reservoirs in the nebula, mass-independent processing in the nebula, and mass-dependent fractionation effects in various environments. It is not possible to unravel this complex isotopic record unless the distribution of oxygen isotope ratios in chondritic materials is fully understood.

Phosphated minerals to be used as radioactive reference materials

International Nuclear Information System (INIS)

Braganca, M.J.C.S.; Tauhata, L.; Clain, A.F.; Moreira, I.

2003-01-01

The production and the supplying of certified reference materials, or deliberated contaminated materials containing natural radionuclides for laboratories which analyses environmental samples are fundamentals for the correct measurements of their radioactive levels. This analysis quality represents a important step for the safeguards of the population health, and quality control of the imported and exported products, such as minerals, agricultural and raw materials. The phosphate rocks, containing significant concentrations of thorium, and used as raw material and fertilizers justified a study for better characterization and distinction to be used cas certified reference radioactive materials. Therefore, samples from the two carboanalytical-alkaline chimneys (Araxa and Catalao), and one from metasedimentar origin (Patos de Minas), distant 100 km from each other, were collected and chemical and cholecystographic characterized by optical emission, X-ray diffraction and fluorescence. The element concentrations were determined by neutron activation analysis, ICP-MS and ICP-AES. The results, after multivariate statistical analysis and study of correlations among elements, have shown geochemical similarities of the phosphates from Araxa and Catalao, and differences from Patos de Minas, despite of the geographic proximity. The concentration of thorium between 200 and 500 (mg/g) allows to use such minerals as reference materials

Certification of an iron metal reference material for neutron dosimetry (EC nuclear reference material 524)

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.; Lievens, F.

1993-01-01

Iron metal, of > 99.996% nominal purity, in the form of 0.1 mm thick foil and of 0.5 mm diameter wire has been certified for its manganese and cobalt mass fractions. The certified value of the cobalt mass fraction ( -1 ) is based on 39 accepted results from five laboratories using two different methods. The certified value of the manganese mass fraction ( -1 ) is based on 41 accepted results from five laboratories using three different methods. The overall purity was also verified. The material is intended to be used as a reference material in neutron dosimetry. (authors). 8 refs., 9 tabs., 2 figs

Results from an interlaboratory exercise on the determination of plutonium isotopic ratios by gamma spectrometry

International Nuclear Information System (INIS)

Ottmar, H.

1981-07-01

Results form interlaboratory comparison measurements on the determination of plutonium isotopic ratios by gamma spectrometry, organized by the ESARDA Working Group on Techniques and Standards for Nondestructive Analysis, are presented and discussed. Nine laboratories from nine countries or international organizations participated in the intercomparison exercise, which included both laboratories' own measurements on the plutonium isotopic reference materials NBS-SRM 946, 947, 948 and comparison analyses of gamma spectra from these materials distributed to the participating laboratories. Results from the intercomparison analyses have been used to reevaluate some gamma branching intensity ratios required for plutonium isotopic ratio measurements. (orig.) [de

Material synthesis and evaluation of metrological characteristics of potassium fluozirconate certified reference material

Directory of Open Access Journals (Sweden)

D. G. Lisienko

2016-01-01

Full Text Available The relevance of the study. For metrological support of control methods for composition ofpotassium fluozirconate, used in the production of metallic zirconium, applied in various technical fields, including nuclear power, electronics, chemical engineering. The purpose: development of synthesis technology, and determination of metrological characteristics of certified reference material for composition ofpotassium fluozirconate (set, intended for metrological support of measuring element mass fraction: hafnium (Hf, silicon (Si, iron (Fe, aluminium (Al, chromium (Cr, tin (Sn, titanium (Ti in potassium fluozirconate. Research methods: X-ray diffraction, differential scanning colorimetry, thermogravimetric analysis, atomic-emission spectral analysis with arc excitation, mass spectral analysis, X-ray fluorescence analysis. Results. As a result of research a set of certified reference materials for composition of potassium fluozirconate is developed and produced. The CRM type is approved by Federal Agency on Technical Regulating and Metrology and registered in State Register of Approved Reference Material Types under number GSO 10593-2015.

Preparation of reference material for the measurement of natural radioactivity

International Nuclear Information System (INIS)

Ben Tekaya, Malik

2010-01-01

The objective of this work is to prepare reference material for the calibration of gamma spectrometry, alpha and XRF .Many procedures of chemical preparation and radiological analysis of a reference material from Triple Superphosphate were tested. Several techniques and methods of measurement were used. In addition to a description and validation of these procedures, a study of repeatability was conducted which resulted in a positive characterization of this material.

Homogeneity test of the ceramic reference materials for non-destructive quantitative

International Nuclear Information System (INIS)

Li Li; Fong Songlin; Zhu Jihao; Feng Xiangqian; Xie Guoxi; Yan Lingtong

2010-01-01

In order to study elemental composition of ancient porcelain samples, we developed a set of ceramic reference materials for non-destructive quantitative analysis. In this paper,homogeneity of Al, Si, K, Ca, Ti, Mn and Fe contents in the ceramic reference materials is investigated by EDXRF. The F test and the relative standard deviation are used to treat the normalized net counts by SPSS. The results show that apart from the DY2 and JDZ4 reference materials, to which further investigation would be needed, homogeneity of the DH, DY3, JDZ3, JDZ6, GY1, RY1, LQ4, YJ1, YY2 and JY2 meets the requirements of ceramic reference materials for non-destructive quantitative analysis. (authors)

A guide for the laboratory information management system (LIMS) for light stable isotopes--Versions 7 and 8

Science.gov (United States)

Coplen, Tyler B.

2000-01-01

The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program, the Laboratory Information Management System (LIMS) for Light Stable Isotopes, is presented herein. Major benefits of this system include (i) a dramatic improvement in quality assurance, (ii) an increase in laboratory efficiency, (iii) a reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) a decrease in errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for laboratories. LIMS for Light Stable Isotopes is available for both Microsoft Office 97 Professional and Microsoft Office 2000 Professional as versions 7 and 8, respectively. Both source code (mdb file) and precompiled executable files (mde) are available. Numerous improvements have been made for continuous flow isotopic analysis in this version (specifically 7.13 for Microsoft Access 97 and 8.13 for Microsoft Access 2000). It is much easier to import isotopic results from Finnigan ISODAT worksheets, even worksheets on which corrections for amount of sample (linearity corrections) have been added. The capability to determine blank corrections using isotope mass balance from analyses of elemental analyzer samples has been added. It is now possible to calculate and apply drift corrections to isotopic

A measuring system for the fast simultaneous isotope ratio and elemental analysis of carbon, hydrogen, nitrogen and sulfur in food commodities and other biological material.

Science.gov (United States)

Sieper, Hans-Peter; Kupka, Hans-Joachim; Williams, Tony; Rossmann, Andreas; Rummel, Susanne; Tanz, Nicole; Schmidt, Hanns-Ludwig

2006-01-01

The isotope ratio of each of the light elements preserves individual information on the origin and history of organic natural compounds. Therefore, a multi-element isotope ratio analysis is the most efficient means for the origin and authenticity assignment of food, and also for the solution of various problems in ecology, archaeology and criminology. Due to the extraordinary relative abundances of the elements hydrogen, carbon, nitrogen and sulfur in some biological material and to the need for individual sample preparations for H and S, their isotope ratio determination currently requires at least three independent procedures and approximately 1 h of work. We present here a system for the integrated elemental and isotope ratio analysis of all four elements in one sample within 20 min. The system consists of an elemental analyser coupled to an isotope ratio mass spectrometer with an inlet system for four reference gases (N(2), CO(2), H(2) and SO(2)). The combustion gases are separated by reversible adsorption and determined by a thermoconductivity detector; H(2)O is reduced to H(2). The analyser is able to combust samples with up to 100 mg of organic material, sufficient to analyse samples with even unusual elemental ratios, in one run. A comparison of the isotope ratios of samples of water, fruit juices, cheese and ethanol from wine, analysed by the four-element analyser and by classical methods and systems, respectively, yielded excellent agreements. The sensitivity of the device for the isotope ratio measurement of C and N corresponds to that of other systems. It is less by a factor of four for H and by a factor of two for S, and the error ranges are identical to those of other systems. Copyright (c) 2006 John Wiley & Sons, Ltd.

Mineral associations and character of isotopically anomalous organic material in the Tagish Lake carbonaceous chondrite

Science.gov (United States)

Zega, Thomas J.; Alexander, Conel M. O.'D.; Busemann, Henner; Nittler, Larry R.; Hoppe, Peter; Stroud, Rhonda M.; Young, Andrea F.

2010-10-01

We report a coordinated analytical study of matrix material in the Tagish Lake carbonaceous chondrite in which the same small (⩽20 μm) fragments were measured by secondary ion mass spectrometry (SIMS), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), electron energy-loss spectroscopy (EELS), and X-ray absorption near-edge spectroscopy (XANES). SIMS analysis reveals H and N isotopic anomalies (hotspots), ranging from hundreds to thousands of nanometers in size, which are present throughout the fragments. Although the differences in spatial resolution of the SIMS techniques we have used introduce some uncertainty into the exact location of the hotspots, in general, the H and N isotopic anomalies are spatially correlated with C enrichments, suggesting an organic carrier. TEM analysis, enabled by site-specific extraction using a focused-ion-beam scanning-electron microscope, shows that the hotspots contain an amorphous component, Fe-Ni sulfides, serpentine, and mixed-cation carbonates. TEM imaging reveals that the amorphous component occurs in solid and porous forms, EDS indicates that it contains abundant C, and EELS and XANES at the C K edge reveal that it is largely aromatic. This amorphous component is probably macromolecular C, likely the carrier of the isotopic anomalies, and similar to the material extracted from bulk samples as insoluble organic matter. However, given the large sizes of some of the hotspots, the disparity in spatial resolution among the various techniques employed in our study, and the phases with which they are associated, we cannot entirely rule out that some of the isotopic anomalies are carried by inorganic material, e.g., sheet silicates. The isotopic composition of the organic matter points to an initially primitive origin, quite possibly within cold interstellar clouds or the outer reaches of the solar protoplanetary disk. The association of organic material with secondary phases, e.g., serpentine

Plutonium working reference materials for the NDA PDP program

International Nuclear Information System (INIS)

Marshall, R.; Foley, M.; McCullough, L.; Vance, D.

1995-01-01

Sixty-three QC standards, termed Working Reference Materials (WRMs) are being fabricated at Los Alamos for the Non-destructive Waste Assay Performance Development Plan. The WRMs require Pu and Am distributed uniformly in a low density matrix. A silicone rubber matrix initially specified has been changed to a packed, diatomaceous earth (DE) matrix to facilitate Pu-DE uniformity and minimize gas generation and WRM pressurization. Uniformity and separation stability was demonstrated with iron powder-DE mixtures. To meet the rigorous quality objectives on the mass of Pu and Am for each WRM, a uniform, stable batch of PuO2 with relatively high Am-241 content was prepared by blending, calcining, and screening. Multiple sample analyses demonstrated the PuO2 to be highly uniform and established that tight Pu and Am assay and Pu isotopic analysis precision requirements were met. Test blends were prepared and tested to successfully demonstrate Pu uniformity, freedom from PuO2 clumping, and acceptable alpha-neutron generation rates. Blends of PuO2-DE were prepared individually for each WRM; all 63 blends have been prepared. After loading and packing the blends into zircalloy cylinders, the air atmosphere will be replaced with helium and end caps inserted and welded. Following decontamination and leak checking, the cylinders will be loaded into secondary zircalloy cylinders and sealed with welded end caps

[The water content reference material of water saturated octanol].

Science.gov (United States)

Wang, Haifeng; Ma, Kang; Zhang, Wei; Li, Zhanyuan

2011-03-01

The national standards of biofuels specify the technique specification and analytical methods. A water content certified reference material based on the water saturated octanol was developed in order to satisfy the needs of the instrument calibration and the methods validation, assure the accuracy and consistency of results in water content measurements of biofuels. Three analytical methods based on different theories were employed to certify the water content of the reference material, including Karl Fischer coulometric titration, Karl Fischer volumetric titration and quantitative nuclear magnetic resonance. The consistency of coulometric and volumetric titration was achieved through the improvement of methods. The accuracy of the certified result was improved by the introduction of the new method of quantitative nuclear magnetic resonance. Finally, the certified value of reference material is 4.76% with an expanded uncertainty of 0.09%.

Certified reference materials for organic analysis

International Nuclear Information System (INIS)

QianChuanfan

2002-01-01

This presentation discusses the requirements for certified reference materials (CRMs) to be used in measurements of residues of pesticides in food and environmental samples. It deals with the types of CRMs, matrix selection, sample preparation and representativeness. It also discusses CRM validity period and gives some examples of CRM preparation

Immune reactivity of candidate reference materials

NARCIS (Netherlands)

Fernandez-Rivas, Montserrat; Aalbers, Marja; Fötisch, Kay; de Heer, Pleuni; Notten, Silla; Vieths, Stefan; van Ree, Ronald

2006-01-01

Immune reactivity is a key issue in the evaluation of the quality of recombinant allergens as potential reference materials. Within the frame of the CREATE project, the immune reactivity of the natural and recombinant versions of the major allergens of birch pollen (Bet v 1), grass pollen (Phl p 1

Evaluation of a reference material for glycated haemoglobin

NARCIS (Netherlands)

Weykamp, CW; Penders, TJ; Muskiet, FAJ; vanderSlik, W

The use of lyophilized blood as a reference material for glycated haemoglobin was investigated with respect to IFCC criteria for calibrators and control materials. Ninety-two laboratories, using 11 methods, detected no changes in glycated haemoglobin content when the lyophilizate was stored for one

Isotopes as tracers of the sources of the lunar material and processes of lunar origin.

Science.gov (United States)

Pahlevan, Kaveh

2014-09-13

Ever since the Apollo programme, isotopic abundances have been used as tracers to study lunar formation, in particular to study the sources of the lunar material. In the past decade, increasingly precise isotopic data have been reported that give strong indications that the Moon and the Earth's mantle have a common heritage. To reconcile these observations with the origin of the Moon via the collision of two distinct planetary bodies, it has been proposed (i) that the Earth-Moon system underwent convective mixing into a single isotopic reservoir during the approximately 10(3) year molten disc epoch after the giant impact but before lunar accretion, or (ii) that a high angular momentum impact injected a silicate disc into orbit sourced directly from the mantle of the proto-Earth and the impacting planet in the right proportions to match the isotopic observations. Recently, it has also become recognized that liquid-vapour fractionation in the energetic aftermath of the giant impact is capable of generating measurable mass-dependent isotopic offsets between the silicate Earth and Moon, rendering isotopic measurements sensitive not only to the sources of the lunar material, but also to the processes accompanying lunar origin. Here, we review the isotopic evidence that the silicate-Earth-Moon system represents a single planetary reservoir. We then discuss the development of new isotopic tracers sensitive to processes in the melt-vapour lunar disc and how theoretical calculations of their behaviour and sample observations can constrain scenarios of post-impact evolution in the earliest history of the Earth-Moon system. © 2014 The Author(s) Published by the Royal Society. All rights reserved.

An in-house usage assessment of print reference materials in a ...

African Journals Online (AJOL)

The study investigated the utilization of print reference materials in a Nigerian hybrid medical school library, factors influencing utilization or under utilization, and if utilization commensurate with the library's prospect on the use of these materials. During the period of study, it was assumed that all reference materials pulled ...

Standard Reference Development of nuclear material for Tensile and Hardness Test Properties

International Nuclear Information System (INIS)

Choo, Y. S.; Kim, D. S.; Yoo, B. O.; Ahn, S. B.; Baik, S. J.; Chun, Y. B.; Kim, K. H.; Hong, K. P.; Ryu, W. S.

2007-12-01

Standard reference is a official approved data such a coefficient of physics, approved material properties, and etc., which should be analyzed and evaluated by scientific method to acquire official approval for accuracy and credibility of measured data and information. So it could be used broadly and continuously by various fields of nation and society. It is classified to effective standard reference, verified standard reference, and certified standard reference. There are sixteen fields in designated standard references such a physical chemistry field, material field, metal field, and the others. The standard reference of neutron irradiated nuclear structural material is classified to metal field. This report summarized the whole processes about data collection, data production, data evaluation and the suggestion of details evaluation technical standard for tensile and hardness properties, which were achieved by carry out the project 'nuclear material standard reference development' as a result

Standard Reference Development of nuclear material for Tensile and Hardness Test Properties

Energy Technology Data Exchange (ETDEWEB)

Choo, Y. S.; Kim, D. S.; Yoo, B. O.; Ahn, S. B.; Baik, S. J.; Chun, Y. B.; Kim, K. H.; Hong, K. P.; Ryu, W. S

2007-12-15

Standard reference is a official approved data such a coefficient of physics, approved material properties, and etc., which should be analyzed and evaluated by scientific method to acquire official approval for accuracy and credibility of measured data and information. So it could be used broadly and continuously by various fields of nation and society. It is classified to effective standard reference, verified standard reference, and certified standard reference. There are sixteen fields in designated standard references such a physical chemistry field, material field, metal field, and the others. The standard reference of neutron irradiated nuclear structural material is classified to metal field. This report summarized the whole processes about data collection, data production, data evaluation and the suggestion of details evaluation technical standard for tensile and hardness properties, which were achieved by carry out the project 'nuclear material standard reference development' as a result.

Certification of a new biological reference material - Virginia Tobacco Leaves (CTA-VTL-2) and homogeneity study by NAA on this and other candidate reference materials

International Nuclear Information System (INIS)

Dybczynski, Rajmund; Polkowska-Motrenko, Halina; Samczynski, Zbigniew; Szopa, Zygmunt; Kulisa, Krzysztof; Wasek, Marek

2002-01-01

This report describes the laboratory's participation in the interlaboratory comparison run where the laboratory applied neutron activation analysis aimed at certification of the candidate reference material. Data evaluation and statistical treatment steps are discussed. The report also describes homogeneity study on the reference material and provides details of the analytical procedures

Element content and particle size characterization of a mussel candidate reference material

International Nuclear Information System (INIS)

Moreira, Edson G.; Vasconcellos, Marina B.A.; Santos, Rafaela G. dos; Martinelli, Jose R.

2011-01-01

The use of certified reference materials is an important tool in the quality assurance of analytical measurements. To assure reliability on recently prepared powder reference materials, not only the characterization of the property values of interest and their corresponding uncertainties, but also physical properties such as the particle size distribution must be well evaluated. Narrow particle size distributions are preferable than larger ones; as different size particles may have different analyte content. Due to this fact, the segregation of the coarse and the fine particles in a bottle may lead to inhomogeneity of the reference material, which should be avoided. In this study the element content as well as the particle size distribution of a mussel candidate reference material produced at IPEN-CNEN/SP was investigated. Instrumental Neutron Activation Analysis was applied to the determination of 15 elements in seven fractions of the material with different particle size distributions. Subsamples of the materials were irradiated simultaneously with elemental standards at the IEA-R1 research nuclear reactor and the induced gamma ray energies were measured in a hyperpure germanium detector. Three vials of the candidate reference material and three coarser fractions, collected during the preparation, were analyzed by Laser Diffraction Particle Analysis to determine the particle size distribution. Differences on element content were detected for fractions with different particle size distribution, indicating the importance of particle size control for biological reference materials. From the particle size analysis, Gaussian particle size distribution was observed for the candidate reference material with mean particle size μ = 94.6 ± 0.8 μm. (author)

Preparation and certification of rice flour reference materials for trace elements analysis

International Nuclear Information System (INIS)

Cho, Kyung Haeng; Park, Chang Joon; Woo, Jin Choon; Suh, Jung Ki; Han, Myung Sub; Lee, Jong Hae

1998-01-01

Rice flour reference materials were prepared from the unpolished rice grown in korea and certified for elemental composition. The reference materials consist of two samples containing normal and high level. The reference material at elevated level was prepared by spiking to the normal rice flour six toxic elements of As, Cd, Cu, Cr, Hg, Pb with 1.0μg/g on a dry weight basis. Homogeneity of the prepared materials was evaluated through the determination of Ca, Cu, Fe, Mn, Zn by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). Small variance of elemental composition among inter-bottled samples assured homogeneity of the prepared materials. The materials were decomposed by high pres-sure digestion and microwave digestion method. INAA, AAS, inductively coupled plasma-atomic absorption spectrometry (ICP-AES), ICP-mass spectrometry (MS) and vapour generation techniques were employed to analyze the reference materials. From this independent analytical results, the certified or reference values are determined for As, Ca, Cd, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, P, Pb, Se, Zn

The Mantle Isotopic Array: A Tale of Two FOZOs

Science.gov (United States)

Apen, F. E.; Mukhopadhyay, S.; Williams, C. D.

2017-12-01

Oceanic basalts display isotopic arrays that suggest mixing between a depleted component, several enriched components, and a primitive component. The topology of the arrays provides information on mantle mixing, the distribution of heterogeneities, and information on mantle structure. Here we use a global compilation of mid-ocean ridge basalt (MORB) and ocean island basalt (OIB) He-Sr-Nd-Pb isotopic data to further analyze the topology of these arrays. Previous work indicated that OIB isotopic arrays converge to a common component [1-3] referred to as the focus zone, or FOZO. Our analyses suggest that while all OIBs do point to a common component with unradiogenic 4He/3He ratios relative to MORBs, this component has to be quite variable in its He, Sr, Nd and Pb isotopic compositions. FOZO cannot be a pure component but must represent a heterogeneous mixture of primitive and recycled material. Our analyses of the MORB and OIB isotopic compositions also indicate that while MORBs and OIBs sample the same components, the topology of their mixing arrays are quite distinct. Different MOR segments show quasi-linear isotopic arrays that all converge to a common component. This component is distinctive from the OIB FOZO being more depleted and more restrictive in its He, Sr, Nd and Pb composition. We suggest two common but distinguishable components are present in the mantle arrays: one common to MORBs and the other to OIBs, and we refer to them as MORB-FOZO and OIB-FOZO, respectively. We interpret the two FOZOs to represent the average composition of small-scale heterogeneities that make up the background matrix in the sources of MORBs and OIBs. The depleted and enriched components that are sampled in MORBs and OIBs reflect relatively large-scale heterogeneities distributed within the matrix, material that have yet to be deformed into the smaller length scales of the matrix material. Differences between the two FOZO compositions reflects the inclusion of a component with

Micro-homogeneity evaluation of a bovine kidney candidate reference material

Energy Technology Data Exchange (ETDEWEB)

Castro, Liliana; Moreira, Edson G.; Vasconcellos, Marina B.A., E-mail: lcastroesnal@usp.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

2017-07-01

The minimum sample intake for which a reference material remains homogeneous is one of the parameters that must be estimated in the homogeneity assessment study of reference materials. In this work, Instrumental Neutron Activation Analysis was used to evaluate this quantity in a bovine kidney candidate reference material. The mass fractions of 9 inorganic constituents were determined in subsamples between 1 and 2 mg in order to estimate the relative homogeneity factor (HE) and the minimum sample mass to achieve 5% and 10% precision on a 95% confidence level. Results obtained for H{sub E} in all the analyzed elements were satisfactory. The estimated minimum sample intake was between 2 mg and 40 mg, depending on the element. (author)

High Flux Isotope Reactor cold neutron source reference design concept

International Nuclear Information System (INIS)

Selby, D.L.; Lucas, A.T.; Hyman, C.R.

1998-05-01

In February 1995, Oak Ridge National Laboratory's (ORNL's) deputy director formed a group to examine the need for upgrades to the High Flux Isotope Reactor (HFIR) system in light of the cancellation of the Advanced neutron Source Project. One of the major findings of this study was that there was an immediate need for the installation of a cold neutron source facility in the HFIR complex. In May 1995, a team was formed to examine the feasibility of retrofitting a liquid hydrogen (LH 2 ) cold source facility into an existing HFIR beam tube. The results of this feasibility study indicated that the most practical location for such a cold source was the HB-4 beam tube. This location provides a potential flux environment higher than the Institut Laue-Langevin (ILL) vertical cold source and maximizes the space available for a future cold neutron guide hall expansion. It was determined that this cold neutron beam would be comparable, in cold neutron brightness, to the best facilities in the world, and a decision was made to complete a preconceptual design study with the intention of proceeding with an activity to install a working LH 2 cold source in the HFIR HB-4 beam tube. During the development of the reference design the liquid hydrogen concept was changed to a supercritical hydrogen system for a number of reasons. This report documents the reference supercritical hydrogen design and its performance. The cold source project has been divided into four phases: (1) preconceptual, (2) conceptual design and testing, (3) detailed design and procurement, and (4) installation and operation. This report marks the conclusion of the conceptual design phase and establishes the baseline reference concept

LBA-ECO CD-02 Carbon, Nitrogen, Oxygen Stable Isotopes in Organic Material, Brazil

Data.gov (United States)

National Aeronautics and Space Administration — This data set reports the measurement of stable carbon, nitrogen, and oxygen isotope ratios in organic material (plant, litter and soil samples) in forest canopy...

LBA-ECO CD-02 Carbon, Nitrogen, Oxygen Stable Isotopes in Organic Material, Brazil

Data.gov (United States)

National Aeronautics and Space Administration — ABSTRACT: This data set reports the measurement of stable carbon, nitrogen, and oxygen isotope ratios in organic material (plant, litter and soil samples) in forest...

Titanium carbide-carbon porous nanocomposite materials for radioactive ion beam production: processing, sintering and isotope release properties

CERN Document Server

AUTHOR|(CDS)2081922; Stora, Thierry

2017-01-26

The Isotope Separator OnLine (ISOL) technique is used at the ISOLDE - Isotope Separator OnLine DEvice facility at CERN, to produce radioactive ion beams for physics research. At CERN protons are accelerated to 1.4 GeV and made to collide with one of two targets located at ISOLDE facility. When the protons collide with the target material, nuclear reactions produce isotopes which are thermalized in the bulk of the target material grains. During irradiation the target is kept at high temperatures (up to 2300 °C) to promote diffusion and effusion of the produced isotopes into an ion source, to produce a radioactive ion beam. Ti-foils targets are currently used at ISOLDE to deliver beams of K, Ca and Sc, however they are operated at temperatures close to their melting point which brings target degradation, through sintering and/or melting which reduces the beam intensities over time. For the past 10 years, nanostructured target materials have been developed and have shown improved release rates of the produced i...

Maintaining high precision of isotope ratio analysis over extended periods of time.

Science.gov (United States)

Brand, Willi A

2009-06-01

Stable isotope ratios are reliable and long lasting process tracers. In order to compare data from different locations or different sampling times at a high level of precision, a measurement strategy must include reliable traceability to an international stable isotope scale via a reference material (RM). Since these international RMs are available in low quantities only, we have developed our own analysis schemes involving laboratory working RM. In addition, quality assurance RMs are used to control the long-term performance of the delta-value assignments. The analysis schemes allow the construction of quality assurance performance charts over years of operation. In this contribution, the performance of three typical techniques established in IsoLab at the MPI-BGC in Jena is discussed. The techniques are (1) isotope ratio mass spectrometry with an elemental analyser for delta(15)N and delta(13)C analysis of bulk (organic) material, (2) high precision delta(13)C and delta(18)O analysis of CO(2) in clean-air samples, and (3) stable isotope analysis of water samples using a high-temperature reaction with carbon. In addition, reference strategies on a laser ablation system for high spatial resolution delta(13)C analysis in tree rings is exemplified briefly.

Characterization of nanoparticles as candidate reference materials

International Nuclear Information System (INIS)

Martins Ferreira, E.H.; Robertis, E. de; Landi, S.M.; Gouvea, C.P.; Archanjo, B.S.; Almeida, C.A.; Araujo, J.R. de; Kuznetsov, O.; Achete, C.A.

2013-01-01

We report the characterization of three different nanoparticles (silica, silver and multi-walled carbon nanotubes) as candidate reference material. We focus our analysis on the size distribution of those particles as measured by different microscopy techniques. (author)

Production and certification of reference materials

International Nuclear Information System (INIS)

Sarkis, Jorge Eduardo de S.; Kakazu, Mauricio H.; Hespanhol, Emilio Carlos B.; Martins, Elaine Arantes J.

1996-01-01

The reference materials used in analytical chemistry permit us to evaluate correctly the analytical producers as well as experimental set up. U 3 O 8 was produced at IPEN to be used as a secondary standard. We present the first results on U 3 O 8 and discuss the method, preparation, and characterization of that oxide. (author)

Sulfate and sulfide sulfur isotopes (δ34S and δ33S) measured by solution and laser ablation MC-ICP-MS: An enhanced approach using external correction

Science.gov (United States)

Pribil, Michael; Ridley, William I.; Emsbo, Poul

2015-01-01

Isotope ratio measurements using a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) commonly use standard-sample bracketing with a single isotope standard for mass bias correction for elements with narrow-range isotope systems measured by MC-ICP-MS, e.g. Cu, Fe, Zn, and Hg. However, sulfur (S) isotopic composition (δ34S) in nature can range from at least − 40 to + 40‰, potentially exceeding the ability of standard-sample bracketing using a single sulfur isotope standard to accurately correct for mass bias. Isotopic fractionation via solution and laser ablation introduction was determined during sulfate sulfur (Ssulfate) isotope measurements. An external isotope calibration curve was constructed using in-house and National Institute of Standards and Technology (NIST) Ssulfate isotope reference materials (RM) in an attempt to correct for the difference. The ability of external isotope correction for Ssulfate isotope measurements was evaluated by analyzing NIST and United States Geological Survey (USGS) Ssulfate isotope reference materials as unknowns. Differences in δ34Ssulfate between standard-sample bracketing and standard-sample bracketing with external isotope correction for sulfate samples ranged from 0.72‰ to 2.35‰ over a δ34S range of 1.40‰ to 21.17‰. No isotopic differences were observed when analyzing Ssulfide reference materials over a δ34Ssulfide range of − 32.1‰ to 17.3‰ and a δ33S range of − 16.5‰ to 8.9‰ via laser ablation (LA)-MC-ICP-MS. Here, we identify a possible plasma induced fractionation for Ssulfate and describe a new method using external isotope calibration corrections using solution and LA-MC-ICP-MS.

Laser separation of uranium isotopes

International Nuclear Information System (INIS)

Porter, J.T.

1981-01-01

Method and apparatus for separating uranium isotopes are claimed. The method comprises the steps of irradiating a uranyl source material at a wavelength selective to a desired isotope and at an effective temperature for isotope spectral line splitting below about 77 deg.K., further irradiating the source material within the fluorescent lifetime of the source material to selectively photochemically reduce the excited isotopic species, and chemically separating the reduced isotope species from the remaining uranyl salt compound

IAEA programme of natural matrix reference materials for the determination of radionuclides

International Nuclear Information System (INIS)

Strachnov, V.; Valkovic, V.; LaRosa, J.; Dekner, R.; Zeisler, R.

1993-01-01

The International Atomic Energy Agency has been providing analytical quality control services (AQCS) to its Member States since the 1960's. The AQCS programme distributes reference materials (RMs), organizes intercomparison runs, and provides training courses for quality assurance in chemical analysis and radioactivity measurements of food, biological, environmental and marine materials. This paper focusses on those aspects of the subject dealing with reference materials and intercomparison runs for the determination of radionuclides. Nineteen natural matrix reference materials are available for the determination of radionuclides. Twelve new intercomparison and reference materials are in preparation or under consideration. The radionuclides of interest include: K-40, Mn-54, Co-60, Sr-90, Tc-99, Ru-106, Ba-133, Cs-134, Cs-137, Pb-210, Ra-226, Th-228, Th-232, Pu-238, Pu-239 + 240. (orig.)

The application of isotopic dating methods for prospection and exploration of nuclear raw material

International Nuclear Information System (INIS)

Komlev, L.V.; Anderson, E.B.

1977-01-01

Among the geological and geochemical methods for prospecting and searching the nuclear raw material, the isotope-dating methods determine the most important search criterion - the time of the ore-forming. The elaboration and use of these methods in uranium-ore regions reveal a series of geochemical epochs of uranium and thorium accumulation connected naturally with the history of geological evolution of the earth crust. The isotope-dating methods enable with confidence to establish the stages of tectono-magmatic activity resulting in the redistribution and the local concentration of uranium. The wide use of isotopic methods is a necessary condition for reasonable trends of the modern geological exploration [ru

Inter-laboratory comparison of elemental analysis and gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS). Part I: delta13C measurements of selected compounds for the development of an isotopic Grob-test.

Science.gov (United States)

Serra, F; Janeiro, A; Calderone, G; Rojas, J M Moreno; Rhodes, C; Gonthier, L A; Martin, F; Lees, M; Mosandl, A; Sewenig, S; Hener, U; Henriques, B; Ramalho, L; Reniero, F; Teixeira, A J; Guillou, C

2007-03-01

This study was directed towards investigating suitable compounds to be used as stable isotope reference materials for gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) calibration. Several compounds were selected from those used in the 'Grob-test' mixture. Oxygen- and nitrogen-containing substances were added to these compounds to allow the mixture to be used as a possible multi-isotopic calibration tool for 2H/1H, 13C/12C, 15N/14N and 18O/16O ratio determinations. In this paper we present the results of delta13C measurements performed by the consortium of the five laboratories taking part in this inter-calibration exercise. All the compounds were individually assessed for homogeneity, short-term stability and long-term stability by means of EA-IRMS, as required by the bureau communitaire de reference (BCR) Guide for Production of Certified Reference Materials. The results were compared then with the GC-C-IRMS measurements using both polar and non-polar columns, and the final mixture of selected compounds underwent a further certification exercise assessing limits of accuracy and reproducibility under specified GC-C-IRMS conditions. Copyright 2007 John Wiley & Sons, Ltd.

Isotope separation process

International Nuclear Information System (INIS)

Lyon, R.K.

1976-01-01

The instant invention relates to a process for separating a material into two or more parts in each of which the abundances of the isotopes of a given element differ from the abundances of the isotopes of the same material in said material. In one embodiment, the invention relates to a method for the isotopically selective excitation of gas phase molecules by multiple infrared photon absorption followed by selective dissociation of said excited molecules by the absorption of a single photon of visible or ultraviolet light. This invention is useful for, but not limited to, the separation of the principal isotopes of uranium. 11 Claims, 2 Drawing Figures

Isotope dilution surface ionization mass spectrometry of silver in environmental materials

Energy Technology Data Exchange (ETDEWEB)

Murozumi, M; Nakamura, S; Suga, K [Muroran Inst. of Tech., Hokkaido (Japan)

1981-03-01

Surface ionization mass spectrometry has been developed to measure isotopic abundances and concentrations of silver in commercial high-purity metals, environmental materials such as rocks and plants, and /sup 109/Ag and /sup 107/Ag spikes. A minute amount of silver is extracted into a dithizone chloroform solution from a nitric acid solution of above samples. After the silver is back-extracted into 6.0 ml of a 7 mol/l HNO/sub 3/ solution, the solution is evaporated to dryness under the nitrogen atmosphere. Silver nitrate thus formed is dissolved in a mixture of 60 ..mu..l of an 0.003% silica gel suspended water and 5 ..mu..l of a 2% phosphoric acid. An aliquot of this solution is applied to the mass spectrometry using a rhenium single filament as an ion emitter. The proposed method can detect the presence of 10/sup -14/ g of silver on the ion emitter, and measure the /sup 109/Ag//sup 107/Ag isotopic ratio in environmental materials with the accuracy of 0.1 -- 0.2% in the coefficient of variation. Isotope dilution mass spectrometry using a /sup 107/Ag spike has revealed the silver concentration in the environmental standard materials, which were prepared by the National Bureau of Standards, U.S.A. and National Institute of Environmental Studies of Japan, as follows; 27.9 +- 0.2 ppb for the Orchard Leaves and 34.3 +- 0.3 ppb in the Pepper Bush. The determined values of silver in the Granodiorite, JG-1, and Basalt, JB-1 powders made by the Geological Survey of Japan are 25.4 +- 0.4 ppb and 41.3 +- 0.1 ppb respectively. Silver concentration in a coastal sea water sample is found to be at the level of 2.5 +- 0.4 ppt.

Preparation and certification of reference materials for the nuclear industry

International Nuclear Information System (INIS)

Wagner, J.F.

1994-01-01

CETAMA (Commission for the Establishment of Analytical Methods) of the Cea group is producing and certifying uranium and plutonium reference materials to meet the requirements of analytical laboratories in the nuclear industry. Reference materials are required at all stages in the fuel cycle: from extraction of uranium, purification, conversion, uranium enrichment, fuel fabrication until reprocessing of spent fuel, management and storage of waste. 3 tabs

Isotope puzzle in sputtering

International Nuclear Information System (INIS)

Zheng Liping

1998-01-01

Mechanisms affecting multicomponent material sputtering are complex. Isotope sputtering is the simplest in the multicomponent materials sputtering. Although only mass effect plays a dominant role in the isotope sputtering, there is still an isotope puzzle in sputtering by ion bombardment. The major arguments are as follows: (1) At the zero fluence, is the isotope enrichment ejection-angle-independent or ejection-angle-dependent? (2) Is the isotope angular effect the primary or the secondary sputter effect? (3) How to understand the action of momentum asymmetry in collision cascade on the isotope sputtering?

Reference mean temperature for evaluation of performance of thermal diffusion column for isotope separation

International Nuclear Information System (INIS)

Yamamoto, Ichiro; Kanagawa, Akira

1987-01-01

In order to evaluate separative performance of a thermal diffusion column, a simplification is usually made in which the temperature dependence of the relevant properties such as thermal diffusion constant is ignored and some proper mean values evaluated at a specific ''mean'' temperature are used. Adoption of weighted average of temperature distribution is common for the ''mean'' temperature, but there exists no definite way of determining mean temperature. The present paper proposes a new reference mean temperature determined by the equation governing the free convection. It is based on the fact that the multiplication effect of free convection is essential to separation by thermal diffusion column. The reference mean temperature is related to pressure difference between top and bottom of column and is higher than a mass-averaged temperature (due to gravitational force) by a contribution of viscous force. The reference mean temperature was calculated, as a reference, for an Ar isotope separating column with an inner hot radius of 0.2 mm and an outer cold radius of 5 mm. The results confirmed the validity of an approximate formula expressing effects of temperature difference and ratio of inner and outer radii of column explicitly for the temperature. The reference mean temperature calculated from pressure difference given by axisymmetric solution of equations of change was in good agreement with the analytical solution. (author)

Development studies of captopril certified reference material

Directory of Open Access Journals (Sweden)

Raquel Nogueira

2011-06-01

Full Text Available This paper describes the studies performed with the candidate Certified Reference Material (CRM of captopril, the first CRM of an active pharmaceutical ingredient (API in Brazil, including determination of impurities (organic, inorganic and volatiles, homogeneity testing, short- and long-term stability studies, calculation of captopril content using the mass balance approach, and estimation of the associated measurement uncertainty.Este artigo descreve os estudos realizados com o candidato a Material de Referência Certificado (MRC de captopril, primeiro MRC de fármacos no Brasil, incluindo a determinação de impurezas (orgânicas, inorgânicas e voláteis, testes de homogeneidade, testes de estabilidade de curta e longa duração, cálculo do teor de captopril por balanço de massa e estimativa da incerteza de medição associada ao valor certificado.

The determination of minor isotope abundances in naturally occurring uranium materials. The tracing power of isotopic signatures for uranium

International Nuclear Information System (INIS)

Ovaskainen, R.

1999-01-01

The mass spectrometric determination of minor abundant isotopes, 234 U and 236 U in naturally occurring uranium materials requires instruments of high abundance sensitivity and the use of highly sensitive detection systems. In this study the thermal ionisation mass spectrometer Finnigan MAT 262RPQ was used. It was equipped with 6 Faraday cups and a Secondary Electron Multiplier (SEM), which was operated in pulse counting mode for the detection of extremely low ion currents. The dynamic measurement range was increased considerably combining these two different detectors. The instrument calibration was performed carefully. The linearity of each detector, the deadtime of the ion counting detector, the detector normalisation factor, the baseline of each detector and the mass discrimination in the ion source were checked and optimised. A measurement technique based on the combination of a Gas Source Mass Spectrometry (GSMS) and a Thermal Ionisation Mass Spectrometry (TIMS) was developed for the accurate determination of isotopic composition in naturally occurring uranium materials. Because the expected ratio of n( 234 U)/n( 238 U) exceeded the dynamic measurement range of the Faraday detectors of the TIMS instrument, an experimental design using a combination of two detectors was developed. The n( 234 U)/n( 235 U) and n( 236 U)/n( 235 U) ratios were determined using ion counting in combination with the decelerating device. The n( 235 U)/n( 238 U) ratio was determined by the Faraday detector. This experimental design allowed the detector cross calibration to be circumvented. Precisions of less than 1 percent for the n( 234 U)/n( 235 U) ratios and 5-25 percent for the n( 236 U)/n( 235 U) ratios were achieved. The purpose of the study was to establish a register of isotopic signatures for natural uranium materials. The amount ratio, and isotopic composition of 18 ore concentrates, collected by the International Atomic Energy Agency (IAEA) from uranium milling and mining

High Flux Isotope Reactor cold neutron source reference design concept

Energy Technology Data Exchange (ETDEWEB)

Selby, D.L.; Lucas, A.T.; Hyman, C.R. [and others

1998-05-01

In February 1995, Oak Ridge National Laboratory`s (ORNL`s) deputy director formed a group to examine the need for upgrades to the High Flux Isotope Reactor (HFIR) system in light of the cancellation of the Advanced neutron Source Project. One of the major findings of this study was that there was an immediate need for the installation of a cold neutron source facility in the HFIR complex. In May 1995, a team was formed to examine the feasibility of retrofitting a liquid hydrogen (LH{sub 2}) cold source facility into an existing HFIR beam tube. The results of this feasibility study indicated that the most practical location for such a cold source was the HB-4 beam tube. This location provides a potential flux environment higher than the Institut Laue-Langevin (ILL) vertical cold source and maximizes the space available for a future cold neutron guide hall expansion. It was determined that this cold neutron beam would be comparable, in cold neutron brightness, to the best facilities in the world, and a decision was made to complete a preconceptual design study with the intention of proceeding with an activity to install a working LH{sub 2} cold source in the HFIR HB-4 beam tube. During the development of the reference design the liquid hydrogen concept was changed to a supercritical hydrogen system for a number of reasons. This report documents the reference supercritical hydrogen design and its performance. The cold source project has been divided into four phases: (1) preconceptual, (2) conceptual design and testing, (3) detailed design and procurement, and (4) installation and operation. This report marks the conclusion of the conceptual design phase and establishes the baseline reference concept.

Recommended reference materials for realization of physicochemical properties pressure-volume-temperature relationships

CERN Document Server

Herington, E F G

1977-01-01

Recommended Reference Materials for Realization of Physicochemical Properties presents recommendations of reference materials for use in measurements involving physicochemical properties, namely, vapor pressure; liquid-vapor critical temperature and critical pressure; orthobaric volumes of liquid and vapor; pressure-volume-temperature properties of the unsaturated vapor or gas; and pressure-volume-temperature properties of the compressed liquid. This monograph focuses on reference materials for vapor pressures at temperatures up to 770 K, as well as critical temperatures and critical pressures

Stable isotope quality assurance using the 'calibrated IRMS' strategy.

Science.gov (United States)

Meijer, Harro A J

2009-06-01

Procedures in our laboratory have always been directed towards complete understanding of all processes involved and corrections needed etc., instead of relying fully on laboratory reference materials. This rather principal strategy (or attitude) is probably not optimal in the economic sense, and is not necessarily more accurate either. Still, it has proven to be very rewarding in its capability to detect caveats that go undiscovered in the standard way of measurement, but that do influence the accuracy or reliability of the measurement procedure. An additional benefit of our laboratory procedures is that it makes us capable of assisting the International Atomic Energy Agency (IAEA) with primary questions like mutual scale assignments and comparison of isotope ratios of the same isotope in different matrices (like delta(18)O in water, carbonates and atmospheric CO(2)), establishment of the (17)O-(18)O relation, and the replenishment of the calibration standards. Finally, for manual preparation systems with a low sample throughput (and thus only few reference materials analysed) it may well be the only way to produce reliable results.

Isotope separation process

International Nuclear Information System (INIS)

Lyon, R.K.

1977-01-01

The instant invention relates to a process for separating a material into two or more parts in each of which the abundances of the isotopes of a given element differ from the abundances of the isotopes of the same material in said material. More particularly, the invention relates to a method for the isotopically selective excitation of gas phase molecules by multiple infrared photon absorption followed by a step wherein more of the excited molecules than nonexcited molecules are converted to a chemically different form which may be separated by means known in the art. This invention is useful for, but not limited to, the separation of the principal isotopes of uranium. 15 claims, 1 figure

Static, Mixed-Array Total Evaporation for Improved Quantitation of Plutonium Minor Isotopes in Small Samples

Science.gov (United States)

Stanley, F. E.; Byerly, Benjamin L.; Thomas, Mariam R.; Spencer, Khalil J.

2016-06-01

Actinide isotope measurements are a critical signature capability in the modern nuclear forensics "toolbox", especially when interrogating anthropogenic constituents in real-world scenarios. Unfortunately, established methodologies, such as traditional total evaporation via thermal ionization mass spectrometry, struggle to confidently measure low abundance isotope ratios (evaporation techniques as a straightforward means of improving plutonium minor isotope measurements, which have been resistant to enhancement in recent years because of elevated radiologic concerns. Results are presented for small sample (~20 ng) applications involving a well-known plutonium isotope reference material, CRM-126a, and compared with traditional total evaporation methods.

The precise measurement of TL isotopic compositions by MC-ICPMS: Application to the analysis of geological materials and meteorites.

Science.gov (United States)

Rehkämper, Mark; Halliday, Alex N.

1999-07-01

The precision of Tl isotopic measurements by thermal ionization mass spectrometry (TIMS) is severely limited by the fact that Tl possesses only two naturally occurring isotopes, such that there is no invariant isotope ratio that can be used to correct for instrumental mass discrimination. In this paper we describe new chemical and mass spectrometric techniques for the determination of Tl isotopic compositions at a level of precision hitherto unattained. Thallium is first separated from the geological matrix using a two-stage anion-exchange procedure. Thallium isotopic compositions are then determined by multiple-collector inductively coupled plasma-mass spectrometry with correction for mass discrimination using the known isotopic composition of Pb that is admixed to the sample solutions. With these procedures we achieve a precision of 0.01-0.02% for Tl isotope ratio measurements in geological samples and this is a factor of ≥3-4 better than the best published results by TIMS. However, without adequate precautions, experimental artifacts can be generated that result in apparent Tl isotopic fractionations of up to one per mil. Analysis of five terrestrial samples indicate the existence of Tl isotopic variations related to natural fractionation processes on the Earth. Two of the three igneous rocks analyzed in this study display Tl isotopic compositions indistinguishable from our laboratory standard, the reference material NIST-997 Tl. A third sample, however, is characterized by ɛ Tl ≈ 2.5 ± 1.5, where ɛ Tl represents the deviation of the 205Tl/ 203Tl ratio of the sample relative to NIST-997 Tl in parts per 10 4. Even larger deviations were identified for two ferromanganese crusts from the Pacific Ocean, which display ɛ Tl-values of +5.0 ± 1.5 and +11.7 ± 1.3. We suggest that the large variability of Tl isotopic compositions in the latter samples are caused by low-temperature processes related to the formation of the Fe-Mn crusts by precipitation and

Determination of polybrominated diphenyl ethers in environmental standard reference materials

Energy Technology Data Exchange (ETDEWEB)

Stapleton, Heather M.; Schantz, Michele M.; Wise, Stephen A. [National Institute of Standards and Technology, Analytical Chemistry Division, Gaithersburg, MD (United States); Keller, Jennifer M.; Kucklick, John R. [National Institute of Standards and Technology, Analytical Chemistry Division, Hollings Marine Laboratory, Charleston, SC (United States); Leigh, Stefan D. [National Institute of Standards and Technology, Statistical Engineering Division, Gaithersburg, MD (United States)

2007-04-15

Standard reference materials (SRMs) are valuable tools in developing and validating analytical methods to improve quality assurance standards. The National Institute of Standards and Technology (NIST) has a long history of providing environmental SRMs with certified concentrations of organic and inorganic contaminants. Here we report on new certified and reference concentrations for 27 polybrominated diphenyl ether (PBDE) congeners in seven different SRMs: cod-liver oil, whale blubber, fish tissue (two materials), mussel tissue and sediment (two materials). PBDEs were measured in these SRMs, with the lowest concentrations measured in mussel tissue (SRM 1974b) and the highest in sediment collected from the New York/New Jersey Waterway (SRM 1944). Comparing the relative PBDE congener concentrations within the samples, we found the biota SRMs contained primarily tetrabrominated and pentabrominated diphenyl ethers, whereas the sediment SRMs contained primarily decabromodiphenyl ether (BDE 209). The cod-liver oil (SRM 1588b) and whale blubber (SRM 1945) materials were also found to contain measurable concentrations of two methoxylated PBDEs (MeO-BDEs). Certified and reference concentrations are reported for 12 PBDE congeners measured in the biota SRMs and reference values are available for two MeO-BDEs. Results from a sediment interlaboratory comparison PBDE exercise are available for the two sediment SRMs (1941b and 1944). (orig.)

Isotope separation process

International Nuclear Information System (INIS)

1976-01-01

The invention relates to a process for separating a given material into two or more parts, in each of which the abundances of the isotopes of a given element differ from the abundances of the isotopes of the same material in the said material. More particularly, the invention relates to a method for the isotopically selective excitation of gas phase UF 6 by infrared photon absorption followed by selective reaction of said excited UF 6 with atomic chlorine, bromine, or iodine to form a product which may be separated by means known in the art

Round robin testing of thermal conductivity reference materials

International Nuclear Information System (INIS)

Hulstrom, L.C.; Tye, R.P.; Smith, S.E.

1985-07-01

The Basalt Waste Isolation Project (BWIP), operated by Rockwell Hanford Operations, has a need to determine the thermal properties of basalt in the region being considered for a nuclear waste repository in basalt. Experimental data on thermal conductivity and its variation with temperature are information required for the characterization of basalt. To establish thermal conductivity values for the reference materials, an interlaboratory measurements program was undertaken. The program was planned to meet the objectives of performing an experimental characterization of the new stock and providing a detailed analysis of the results such that reference values of thermal conductivity could be determined. This program of measurements of the thermal conductivity of Pyrex 7740 and Pyroceram 9606 has produced recommended values that are within +- 1% of those accepted previously. These measurements together with those of density indicate that the present lots of material are similar to those previously available. Pyrex 7740 and Pyroceram 9606 can continue to be used with confidence as thermal conductivity reference materials for studies on rocks and minerals and other materials of similar thermal conductivity. The uncertainty range for Pyrex 7740 and Pyroceram 9606 up to 300 0 C is +- 10.3% and +- 5.6%, respectively. This range is similar to that indicated for the previously recommended values proposed some 18 years ago. It would appear that the overall state of the art in thermal conductivity measurements for materials in this range has changed little in the intervening years. The above uncertainties, which would have been greater had not three data sets been eliminated, are greater than those which are normally claimed for each individual method. Analyses of these differences through refinements in techniques and additional measurements to higher temperatures are required. 13 refs., 7 figs., 4 tabs

Certification of a copper metal reference material for neutron dosimetry. (EC nuclear reference material 522)

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.; Lievens, F.

1993-01-01

Copper metal of ≥ 99.995% nominal purity in the form of 0.1 and 1.0 mm thick foil and 0.5 and 1.0 mm diameter wire has been certified for its cobalt and silver mass fractions. The certified values are -1 and 0.95 ± 0.04 mg.kg -1 respectively, based on 66 results for cobalt and 88 results for silver obtained by nine laboratories using three methods. This reference material, EC-NRM 522, is intended for reactor neutron dosimetry. (authors). 14 refs., 1 annexe, 10 tabs., 2 figs

Production and Evaluation of 236gNp and Reference Materials for Naturally Occurring Radioactive Materials

Science.gov (United States)

Larijani, Cyrus Kouroush

This thesis is based on the development of a radiochemical separation scheme capable of separating both 236gNp and 236Pu from a uranium target of natural isotopic composition ( 1 g uranium) and 200 MBq of fission decay products. The isobaric distribution of fission residues produced following the bombardment of a natural uranium target with a beam of 25 MeV protons has been evaluated. Decay analysis of thirteen isobarically distinct fission residues were carried out using high-resolution gamma-ray spectrometry at the UK National Physical Laboratory. Stoichiometric abundances were calculated via the determination of absolute activity concentrations associated with the longest-lived members of each isobaric chain. This technique was validated by computational modelling of likely sequential decay processes through an isobaric decay chain. The results were largely in agreement with previously published values for neutron bombardments on natural uranium at energies of 14 MeV. Higher relative yields of products with mass numbers A 110-130 were found, consistent with the increasing yield of these radionuclides as the bombarding energy is increased. Using literature values for the production cross-section for fusion of protons with uranium targets, it is estimated that an upper limit of approximately 250 Bq of activity from the 236Np ground state was produced in this experiment. Using a radiochemical separation scheme, Np and Pu fractions were separated from the produced fission decay products, with analyses of the target-based final reaction products made using Inductively Couple Plasma Mass Spectrometry (ICP-MS) and high-resolution alpha and gamma-ray spectrometry. In a separate research theme, reliable measurement of Naturally Occurring Radioactive Materials is of significance in order to comply with environmental regulations and for radiological protection purposes. The thesis describes the standardisation of three reference materials, namely Sand, Tuff and TiO2 which

The determination of minor isotope abundances in naturally occurring uranium materials. The tracing power of isotopic signatures for uranium

Energy Technology Data Exchange (ETDEWEB)

Ovaskainen, R

1999-11-01

The mass spectrometric determination of minor abundant isotopes, {sup 234}U and {sup 236}U in naturally occurring uranium materials requires instruments of high abundance sensitivity and the use of highly sensitive detection systems. In this study the thermal ionisation mass spectrometer Finnigan MAT 262RPQ was used. It was equipped with 6 Faraday cups and a Secondary Electron Multiplier (SEM), which was operated in pulse counting mode for the detection of extremely low ion currents. The dynamic measurement range was increased considerably combining these two different detectors. The instrument calibration was performed carefully. The linearity of each detector, the deadtime of the ion counting detector, the detector normalisation factor, the baseline of each detector and the mass discrimination in the ion source were checked and optimised. A measurement technique based on the combination of a Gas Source Mass Spectrometry (GSMS) and a Thermal Ionisation Mass Spectrometry (TIMS) was developed for the accurate determination of isotopic composition in naturally occurring uranium materials. Because the expected ratio of n({sup 234}U)/n({sup 238}U) exceeded the dynamic measurement range of the Faraday detectors of the TIMS instrument, an experimental design using a combination of two detectors was developed. The n({sup 234}U)/n({sup 235}U) and n({sup 236}U)/n({sup 235}U) ratios were determined using ion counting in combination with the decelerating device. The n({sup 235}U)/n({sup 238}U) ratio was determined by the Faraday detector. This experimental design allowed the detector cross calibration to be circumvented. Precisions of less than 1 percent for the n({sup 234}U)/n({sup 235}U) ratios and 5-25 percent for the n({sup 236}U)/n({sup 235}U) ratios were achieved. The purpose of the study was to establish a register of isotopic signatures for natural uranium materials. The amount ratio, and isotopic composition of 18 ore concentrates, collected by the International

U. S. programs on reference and advanced cladding/duct materials

International Nuclear Information System (INIS)

Bennett, J.W.; Holmes, J.J.; Laidler, J.J.

1977-05-01

Two coordinated national programs are presently in place in the United States for development of reference and advanced cladding and duct alloys for near-term and long-term LMFBR applications. A number of government, industrial and university laboratories are active participants in these two ERDA-sponsored programs. The programs are administered by ERDA through a task group organization, with each task group representing a particular technical activity and the membership of the task group drawn from among the laboratories with active involvement in that activity. Technical coordination of the two programs is provided by the Hanford Engineering Development Laboratory. The National Reference Cladding and Duct Program is charged with the responsibility for development of the required technology to permit full utilization of the reference material, 20 percent cold-worked Type 316 stainless steel, in early LMFBR core applications. The current schedule calls for full evaluation of FFTF-related design base data prior to full-power operation of FFTF in early 1980, followed by a confirmation in early 1983 of reference material performance capabilities for initial-core CRBRP applications. Comprehensive evaluation of reference material performance to commercial plant goal fluence levels will be complete by 1985. The National Advanced Alloy Development Program was instituted in 1974 with the objective to develop, by 1986, advanced cladding and duct materials compatible with advanced fuel systems having peak burnup capabilities up to 150 MWD/kg and doubling times of 15 years or less. Screening of a large number of potential alloys was completed in mid-1975, and there are presently 16 candidate alloys under active investigation

Particle size studies in the preparation of AQCS reference materials

International Nuclear Information System (INIS)

Fajgelj, A.; Zeisler, R.; Benesch, T.; Dekner, R.

1994-01-01

Particle size determination is one of the important steps in the characterization of physical properties of each particulate material. However, particle size distribution effects also a chemical composition of the material in terms of homogeneity and representativeness of the sample, as well as allows or not a possible sub-sampling of the material. All this is of great importance in the preparation of reference materials for which the chemical composition and physical properties have to be extremely well characterized. In the present paper we intend to present same efforts which have been done by Analytical Quality Control Services (AQCS) of the International Atomic Energy Agency (IAEA) in the field of particle size determination in the production of reference materials. The Malvern product MasterSizer X, based on laser light scattering is used for this purpose and the technique is also shortly discussed. (author)

Automatic isotope gas analysis of tritium labelled organic materials Pt. 3

International Nuclear Information System (INIS)

Gacs, I.; Mlinko, S.; Payer, K.; Otvos, L.; Banfi, D.; Palagyi, T.

1978-01-01

An isotope analytical procedure and an automatic instrument developed for the determination of tritium in organic compounds and biological materials by internal gas counting are described. The sample is burnt in a stream of oxygen and the combustion products including water vapour carrying the tritium are led onto a column of molecular sieve-5A heated to 550 deg C. Tritium is retained temporarily on the column, then transferred into a stream of hydrogen by isotope exchange. After addition of butane, the tritiated hydrogen is led into an internal detector and enclosed there for radioactivity measurement. The procedure, providing quantitative recovery, is completed in five minutes. It is free of memory effect and suitable for the determination of tritium in a wide range of organic compounds and samples of biological origin. (author)

Characterization of uranium isotopic abundances in depleted uranium metal assay standard 115

International Nuclear Information System (INIS)

Mathew, K.J.; Singleton, G.L.; Essex, R.M.; Hasozbek, A.; Orlowicz, G.; Soriano, M.

2013-01-01

Certified reference material (CRM) 115, Uranium (Depleted) Metal (Uranium Assay Standard), was analyzed using a TRITON Thermal Ionization Mass Spectrometer to characterize the uranium isotope-amount ratios. The certified 235 U/ 238 U 'major' isotope-amount ratio of 0.0020337 (12) in CRM 115 was determined using the total evaporation (TE) and the modified total evaporation (MTE) analytical techniques. In the MTE method, the total evaporation process is interrupted on a regular basis to allow correction of background from peak tailing, internal calibration of the secondary electron multiplier detector versus the Faraday cups, peak-centering, and ion source re-focusing. For the 'minor' 234 U/ 238 U and 236 U/ 238 U isotope-amount ratio measurements using MTE, precision and accuracy comparable to conventional analyses are achieved, without compromising the quality of the 235 U/ 238 U isotope-amount ratios. Characterized values of the 234 U/ 238 U and 236 U/ 238 U isotope-amount ratios in CRM 115 are 0.000007545 (10) and 0.000032213 (84), respectively. The 233 U/ 238 U isotope-amount ratio in CRM 115 is estimated to be -9 . The homogeneity of the CRM 115 materials is established through the absence of any statistically significant unit-to-unit variation in the uranium isotope-amount ratios. The measurements leading to the certification of uranium isotope-amount ratios are discussed. (author)

Investigation of the isotopic composition of lead and of trace elements concentrations in natural uranium materials as a signature in nuclear forensics

Energy Technology Data Exchange (ETDEWEB)

Svedkauskaite-LeGore, J. [European Commission, Joint Research Centre, Karlsruhe (Germany). Inst. for Transuranium Elements; Institute of Physics, Vilnius (Lithuania); Mayer, K.; Millet, S.; Nicholl, A.; Rasmussen, G. [European Commission, Joint Research Centre, Karlsruhe (Germany). Inst. for Transuranium Elements; Baltrunas, D. [Institute of Physics, Vilnius (Lithuania)

2007-07-01

Lead is contained as trace element in uranium ores and propagates throughout the production process to intermediate products like yellow cake or uranium oxide. The lead isotopes in such material originate from two sources: natural lead and radiogenic lead. The variability of the isotopic composition of lead in ores and yellow cakes was studied and the applicability of this parameter for nuclear forensic investigations was investigated. Furthermore, the chemical impurities contained in these materials were measured in order to identify characteristic differences between materials from different mines. For the samples investigated, it could be shown, that the lead isotopic composition varies largely from mine to mine and it may be used as one of the parameters to distinguish between materials of different origins. Some of the chemical impurities show a similar pattern and support the conclusions drawn from the lead isotope data. (orig.)

Certified reference materials of trace elements in water

Indian Academy of Sciences (India)

Many decisions regarding the suitability of material/products are based on the ... In the present scenario of globalization of economy, use of certified reference ... our national accreditation body, National Accreditation Board for Testing and ...

Application of heavy stable isotopes in forensic isotope geochemistry: A review

International Nuclear Information System (INIS)

Aggarwal, Jugdeep; Habicht-Mauche, Judith; Juarez, Chelsey

2008-01-01

Light stable isotopes have been used for many years to characterize the source and transport of materials. More recently heavy isotope systems such as Sr, Nd and Pb have been added to this list in order to aid source identification. With the advent of multiple collector ICP-MS, the range of isotopic tools now available has increased considerably, however, until the isotope systematics of these new non-traditional isotope systems have become better understood, they will not be as useful in characterizing material source and transportation. Applications using heavy metal stable isotopes (mostly traditional heavy isotopes) have reached most avenues in science, including earth sciences, archaeology, anthropology, animal physiology, ecology and toxicology. This field will continue to grow as new applications are developed and techniques become simpler and quicker. This paper provides a review of how this field has grown and presents two new applications using Pb and Sr isotopes in glazes to determine the source of ore used in glazes, and using Sr isotopes to determine the origin of undocumented deceased Mexican border crossers

Application of heavy stable isotopes in forensic isotope geochemistry: A review

Energy Technology Data Exchange (ETDEWEB)

Aggarwal, Jugdeep [W.M. Keck Isotope Laboratory, Department of Earth Sciences, University of California, Santa Cruz, CA 95064 (United States)], E-mail: jaggarwal@pmc.ucsc.edu; Habicht-Mauche, Judith; Juarez, Chelsey [Department of Anthropology, University of California, Santa Cruz, CA 95064 (United States)

2008-09-15

Light stable isotopes have been used for many years to characterize the source and transport of materials. More recently heavy isotope systems such as Sr, Nd and Pb have been added to this list in order to aid source identification. With the advent of multiple collector ICP-MS, the range of isotopic tools now available has increased considerably, however, until the isotope systematics of these new non-traditional isotope systems have become better understood, they will not be as useful in characterizing material source and transportation. Applications using heavy metal stable isotopes (mostly traditional heavy isotopes) have reached most avenues in science, including earth sciences, archaeology, anthropology, animal physiology, ecology and toxicology. This field will continue to grow as new applications are developed and techniques become simpler and quicker. This paper provides a review of how this field has grown and presents two new applications using Pb and Sr isotopes in glazes to determine the source of ore used in glazes, and using Sr isotopes to determine the origin of undocumented deceased Mexican border crossers.

The development and evaluation of reference materials for food microbiology

NARCIS (Netherlands)

Veld, in 't P.

1998-01-01

Since 1986 the National Institute of Public Health and the Environment (RIVM) has worked on the development and evaluation of microbiological reference materials (RMs) with support from the European Communities Bureau of Reference (BCR), now called Standards Measurement and Testing

Reference materials for nondestructive assay of special nuclear material. Volume 1. Uranium oxide plus graphite powder

International Nuclear Information System (INIS)

Sprinkle, J.K.; Likes, R.N.; Parker, J.L.; Smith, H.A.

1983-10-01

This manual describes the fabrication of reference materials for use in gamma-ray-based nondestructive assay of low-density uranium-bearing samples. The sample containers are 2-l bottles. The reference materials consist of small amounts of UO 2 spread throughout a graphite matrix. The 235 U content ranges from 0 to 100 g. The manual also describes the far-field assay procedure used with low-resolution detectors

Isotopes: technologies, materials and application. II International scientific conference of young scientists, post-graduate students and students. Book of abstracts

International Nuclear Information System (INIS)

2015-01-01

The collection contains materials of abstracts of the conference participants to sum up the experience of research and development in the field of isotope production technologies, the use of compounds specified isotopic composition in different sectors of the economy, as well as the disposal and storage technology of the isotope production wastes. Advanced ideas produce isotopes of rare elements for medicine, microelectronics and nuclear industries are presented. Prospectively projects of scientists of Tomsk Polytechnic University in isotope modifying substances are discussed [ru

Sr-Nd-Hf Isotopic Analysis of <10 mg Dust Samples: Implications for Ice Core Dust Source Fingerprinting

DEFF Research Database (Denmark)

Ujvari, Gabor; Wegner, Wencke; Klötzli, Urs

2018-01-01

Combined Sr‐Nd‐Hf isotopic data of two reference materials (AGV‐1/BCR2) and 50, 10, and 5 mg aliquots of carbonate‐free fine grain (isotopic...... compositions (ICs) demonstrate that robust isotopic ratios can be obtained from 5 to 10 mg size rock samples using the ion exchange/mass spectrometry techniques applied. While 87Sr/86Sr ratios of dust aluminosilicate fractions are affected by even small changes in pretreatments, Nd isotopic ratios are found...... to be insensitive to acid leaching, grain‐size or weathering effects. However, the Nd isotopic tracer is sometimes inconclusive in dust source fingerprinting (BEI and NUS both close to ɛNd(0) –10). Hafnium isotopic values (

Certification of biological reference materials by instrumental neutron activation analysis

International Nuclear Information System (INIS)

Lanjewar, Mamata R.; Lanjewar, R.B.

2014-01-01

A multielemental instrumental neutron activation analysis (INAA) method by short and long irradiation has been employed for the determination of 21 minor and trace elements in two standard Reference Materials P-RBF and P-WBF from Institute of Radioecology and Applied Nuclear Techniques ,Czechoslovakia. Also some biological standards such as Bowen's kale, cabbage leaves (Poland) including wheat and rice flour samples of local origin were analysed. It is suggested that INAA is an ideal method for the certification of Reference Materials of Biological Matrices. (author)

Reference material for radionuclides in sediment IAEA-384 (Fangataufa Lagoon sediment)

DEFF Research Database (Denmark)

Povinec, P.P.; Pham, M.K.; Sanchez-Cabeza, J.A.

2007-01-01

A reference material designed for the determination of anthropogenic and natural radionuclides in sediment, IAEA-384 (Fangataufa Lagoon sediment), is described and the results of certification are presented. The material has been certified for 8 radionuclides (K-40, Co-60, Eu-155, Th-230, U-238, ...... management of radioanalytical laboratories engaged in the analysis of radionuclides in the environment, as well as for the development and validation of analytical methods and for training purposes. The material is available from IAEA in 100 g units.......A reference material designed for the determination of anthropogenic and natural radionuclides in sediment, IAEA-384 (Fangataufa Lagoon sediment), is described and the results of certification are presented. The material has been certified for 8 radionuclides (K-40, Co-60, Eu-155, Th-230, U-238, Pu......-238, Pu239+240 and Am-241). Information values are given for 12 radionuclides (Sr-90, Cs-137, Pb-210 (Po-210), Ra-226, Ra-228, Th-232, U-234, U-235, Pu-239, Pu-240 and Pu-241). Less reported radionuclides include Th-228, U-236, Np-239 and Pu-242. The reference material may be used for quality...

Compound specific stable isotopes as probes for distinguishing the sources of biomolecules in terrestrial and extraterrestrial materials

Science.gov (United States)

Engel, M. H.; Macko, S. A.

2003-04-01

Life on Earth consists of orderly arrangements of several key types of organic compounds (amino acids, sugars, fatty acids, nucleic bases) that are the building blocks of proteins, carbohydrates, lipids and nucleotides. Subsequent to death, macromolecules are commonly broken down to their molecular constituents or other similar scale components. Thus, in ancient terrestrial and extraterrestrial materials, it is far more likely to expect the presence of simple compounds such as amino acids rather than the proteins from which they were possibly derived. Given that amino acids, for example, are common components of all extinct and extant organisms, the challenge has been to develop methods for distinguishing their sources. Stable isotopes are powerful probes for determining the origins of organic matter. Amino acid constituents of all organisms on Earth exhibit characteristic stable isotope compositions owing to fractionations associated with their biosynthesis. These fractionations are distinct from those observed for amino acids formed by abiotic processes. Thus it should be possible to use isotopes as probes for determining whether amino acids in ancient rocks on Earth are biotic or abiotic, based on their relative isotopic compositions. Also, owing to differences in the isotope compositions of precursors, amino acids in extraterrestrial materials such as carbonaceous meteorites are moderately to substantially enriched in the heavy isotopes of C, N and H relative to terrestrial amino acids. Assuming that the isotope compositions of the gaseous components of, for example, the Martian atmosphere were distinct from Earth at such time when organic molecules may have formed, it should be possible to distinguish these components from terrestrial contaminants by determining their isotope compositions and/or those of their respective enantiomers. Also, if life as we know it existed on another planet such as Mars, fractionations characteristic of biosynthesis should be

Preparation and evaluation of reference materials for accountancy analysis. (2) Evaluation results

International Nuclear Information System (INIS)

Sumi, Mika; Abe, Katsuo; Kageyama, Tomio; Nakazawa, Hiroaki; Takamatsu, Mai; Kacchi, Tomokazu; Murakami, Toshiki; Ai, Hironobu

2009-01-01

Destructive analysis for accountancy at nuclear fuel facilities should attain international target values for measurement uncertainties in safeguarding nuclear materials (ITVs). Since measurement uncertainties of isotope dilution mass spectrometry depend on uncertainties of spikes (standard materials) used, utilizing highly reliable standard material is essential. The LSD spikes prepared under collaboration work with JAEA and JNFL has different Pu/U ratio and smaller nuclear material in a spike compared with the LSD spikes used a safeguard laboratories, and the value of Pu which separated and purified from MOX and used as raw material for one of the LSD spike prepared at JAEA were measured at JAEA. Uncertainties of the prepared LSD spikes and the measurement results of actual samples with these LSD spikes were evaluated based on ISO-GUM and compared with ITVs. (author)

Isotopic fractionation of NBS oxalic acid and its influence in the calculated age of materials

International Nuclear Information System (INIS)

Nehmi, V.A.

1979-10-01

The intensity of the isotopic fractionation during the oxidation of NBS oxalic acid to carbon dioxide was checked. 30 reactions of oxidation of NBS oxalic acid with potassium permanganate were made. The resultant isotopic composition of CO 2 has been determined with a mass-spectrometer. A conclusion has been reached that the average of Δ 13 C is - 18.9% o with variation between - 17.7 and - 21.2%o. For values of Δ 13 C equal to - 22.0%o, the calculated age with isotopic correction shows the following deviations in relation to non-corrected age: 4% for materials of 1,000 years and 0.3% for 20,000 years.(Author) [pt

Newly developed standard reference materials for organic contaminant analysis

Energy Technology Data Exchange (ETDEWEB)

Poster, D.; Kucklick, J.; Schantz, M.; Porter, B.; Wise, S. [National Inst. of Stand. and Technol., Gaithersburg, MD (USA). Center for Anal. Chem.

2004-09-15

The National Institute of Standards and Technology (NIST) has issued a number of Standard Reference Materials (SRM) for specified analytes. The SRMs are biota and biological related materials, sediments and particle related SRMs. The certified compounds for analysis are polychlorinated biphenyls (PCB), polycylic aromatic hydrocarbons (PAH) and their nitro-analogues, chlorinated pesticides, methylmercury, organic tin compounds, fatty acids, polybrominated biphenyl ethers (PBDE). The authors report on origin of materials and analytic methods. (uke)

Double spike with isotope pattern deconvolution for mercury speciation

International Nuclear Information System (INIS)

Castillo, A.; Rodriguez-Gonzalez, P.; Centineo, G.; Roig-Navarro, A.F.; Garcia Alonso, J.I.

2009-01-01

Full text: A double-spiking approach, based on an isotope pattern deconvolution numerical methodology, has been developed and applied for the accurate and simultaneous determination of inorganic mercury (IHg) and methylmercury (MeHg). Isotopically enriched mercury species ( 199 IHg and 201 MeHg) are added before sample preparation to quantify the extent of methylation and demethylation processes. Focused microwave digestion was evaluated to perform the quantitative extraction of such compounds from solid matrices of environmental interest. Satisfactory results were obtained in different certificated reference materials (dogfish liver DOLT-4 and tuna fish CRM-464) both by using GC-ICPMS and GC-MS, demonstrating the suitability of the proposed analytical method. (author)

Biological and environmental reference materials in neutron activation analysis work

International Nuclear Information System (INIS)

Guinn, V.P.; Gavrilas, M.

1990-01-01

The great usefulness of reference materials, especially ones of certified elemental composition, is discussed with particular attention devoted to their use in instrumental neutron activation analysis (INAA) work. Their use, including both certified and uncertified values, in calculations made by the INAA Advance Prediction Computer Program (APCP) is discussed. The main features of the APCP are described, and mention is made of the large number of reference materials run on the APCP (including the new personal computer version of the program), with NBS Oyster Tissue SRM-1566 used as the principal examle. (orig.)

On criteria for examining analysis quality with standard reference material

International Nuclear Information System (INIS)

Yang Huating

1997-01-01

The advantages and disadvantages and applicability of some criteria for examining analysis quality with standard reference material are discussed. The combination of the uncertainties of the instrument examined and the reference material should be determined on the basis of specific situations. Without the data of the instrument's uncertainty, it would be applicable to substitute the standard deviation multiplied by certain times for the uncertainty. The result of the examining should not result in more error reported in routine measurements than it really is. Over strict examining should also be avoided

Lawrence Livermore National Laboratory Working Reference Material Production Pla

Energy Technology Data Exchange (ETDEWEB)

Wong, Amy; Thronas, Denise; Marshall, Robert

1998-11-04

This Lawrence Livermore National Laboratory (LLNL) Working Reference Material Production Plan was written for LLNL by the Los Alamos National Laboratory to address key elements of producing seven Pu-diatomaceous earth NDA Working Reference Materials (WRMS). These WRMS contain low burnup Pu ranging in mass from 0.1 grams to 68 grams. The composite Pu mass of the seven WRMS was designed to approximate the maximum TRU allowable loading of 200 grams Pu. This document serves two purposes: first, it defines all the operations required to meet the LLNL Statement of Work quality objectives, and second, it provides a record of the production and certification of the WRMS. Guidance provided in ASTM Standard Guide C1128-89 was used to ensure that this Plan addressed all the required elements for producing and certifying Working Reference Materials. The Production Plan was written to provide a general description of the processes, steps, files, quality control, and certification measures that were taken to produce the WRMS. The Plan identifies the files where detailed procedures, data, quality control, and certification documentation and forms are retained. The Production Plan is organized into three parts: a) an initial section describing the preparation and characterization of the Pu02 and diatomaceous earth materials, b) middle sections describing the loading, encapsulation, and measurement on the encapsulated WRMS, and c) final sections describing the calculations of the Pu, Am, and alpha activity for the WRMS and the uncertainties associated with these quantities.

Isotopically controlled semiconductors

Energy Technology Data Exchange (ETDEWEB)

Haller, Eugene E.

2006-06-19

The following article is an edited transcript based on the Turnbull Lecture given by Eugene E. Haller at the 2005 Materials Research Society Fall Meeting in Boston on November 29, 2005. The David Turnbull Lectureship is awarded to recognize the career of a scientist who has made outstanding contributions to understanding materials phenomena and properties through research, writing, and lecturing, as exemplified by the life work of David Turnbull. Haller was named the 2005 David Turnbull Lecturer for his 'pioneering achievements and leadership in establishing the field of isotopically engineered semiconductors; for outstanding contributions to materials growth, doping and diffusion; and for excellence in lecturing, writing, and fostering international collaborations'. The scientific interest, increased availability, and technological promise of highly enriched isotopes have led to a sharp rise in the number of experimental and theoretical studies with isotopically controlled semiconductor crystals. This article reviews results obtained with isotopically controlled semiconductor bulk and thin-film heterostructures. Isotopic composition affects several properties such as phonon energies, band structure, and lattice constant in subtle, but, for their physical understanding, significant ways. Large isotope-related effects are observed for thermal conductivity in local vibrational modes of impurities and after neutron transmutation doping. Spectacularly sharp photoluminescence lines have been observed in ultrapure, isotopically enriched silicon crystals. Isotope multilayer structures are especially well suited for simultaneous self- and dopant-diffusion studies. The absence of any chemical, mechanical, or electrical driving forces makes possible the study of an ideal random-walk problem. Isotopically controlled semiconductors may find applications in quantum computing, nanoscience, and spintronics.

Oxygen isotope exchange with quartz during pyrolysis of silver sulfate and silver nitrate.

Science.gov (United States)

Schauer, Andrew J; Kunasek, Shelley A; Sofen, Eric D; Erbland, Joseph; Savarino, Joel; Johnson, Ben W; Amos, Helen M; Shaheen, Robina; Abaunza, Mariana; Jackson, Terri L; Thiemens, Mark H; Alexander, Becky

2012-09-30

Triple oxygen isotopes of sulfate and nitrate are useful metrics for the chemistry of their formation. Existing measurement methods, however, do not account for oxygen atom exchange with quartz during the thermal decomposition of sulfate. We present evidence for oxygen atom exchange, a simple modification to prevent exchange, and a correction for previous measurements. Silver sulfates and silver nitrates with excess (17)O were thermally decomposed in quartz and gold (for sulfate) and quartz and silver (for nitrate) sample containers to O(2) and byproducts in a modified Temperature Conversion/Elemental Analyzer (TC/EA). Helium carries O(2) through purification for isotope-ratio analysis of the three isotopes of oxygen in a Finnigan MAT253 isotope ratio mass spectrometer. The Δ(17)O results show clear oxygen atom exchange from non-zero (17)O-excess reference materials to zero (17)O-excess quartz cup sample containers. Quartz sample containers lower the Δ(17)O values of designer sulfate reference materials and USGS35 nitrate by 15% relative to gold or silver sample containers for quantities of 2-10 µmol O(2). Previous Δ(17)O measurements of sulfate that rely on pyrolysis in a quartz cup have been affected by oxygen exchange. These previous results can be corrected using a simple linear equation (Δ(17)O(gold) = Δ(17)O(quartz) * 1.14 + 0.06). Future pyrolysis of silver sulfate should be conducted in gold capsules or corrected to data obtained from gold capsules to avoid obtaining oxygen isotope exchange-affected data. Copyright © 2012 John Wiley & Sons, Ltd.

Fresh biological reference materials. Use in inter laboratory studies and as CRMs

International Nuclear Information System (INIS)

De Boer, J.

1999-01-01

Biological reference materials were prepared and packed in tins and glass jars to be used in inter laboratory studies on chlorobiphenyls and organochlorine pesticides, and trace metals, respectively. The materials were homogenised, sterilised and packed as wet tissue, which is unique for the purpose of inter laboratory studies and offers the advantage of studying the extraction and destruction steps of the analytical methods. In addition to their use in inter laboratory studies, some materials have been prepared or are being prepared as certified reference material for chlorobiphenyl analysis. (author)

Nuclear fuel and/or fertile material element suitable for non-destructive determination of burn-up

International Nuclear Information System (INIS)

Muench, E.

1976-01-01

The invention refers to a nuclear fuel and/or fertile material element suitable for non-destructive burn-up analysis, where an isotope or a mixture of isotopes capable of being activated is provided for measuring the intensity of radiation emitted from radioactive nuclides, especially the intensity of gamma rays. The half-life of radioactive decay of the isotope or the mixture mentioned above after being activated is sufficiently large compared with the irradiation of the fuel and/or fertile material element in the nuclear reactor. (orig.) [de

Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material; Analisis de Estano en una Ceniza de Combustion mediante Espectrometria de Masas de Ionizacion Termica con Dilucion Isotopica

Energy Technology Data Exchange (ETDEWEB)

Hernandez, C; Fernandez, M; Quejido, A L

2006-07-01

Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound exposure time. Due to the complex matrix of this fly ash material, a two-step purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs.

Uncertainty assessment in gamma spectrometric measurements of plutonium isotope ratios and age

Energy Technology Data Exchange (ETDEWEB)

Ramebaeck, H., E-mail: henrik.ramebeck@foi.se [Swedish Defence Research Agency, FOI, Division of CBRN Defence and Security, SE-901 82 Umea (Sweden); Chalmers University of Technology, Department of Chemical and Biological Engineering, Nuclear Chemistry, SE-412 96 Goeteborg (Sweden); Nygren, U.; Tovedal, A. [Swedish Defence Research Agency, FOI, Division of CBRN Defence and Security, SE-901 82 Umea (Sweden); Ekberg, C.; Skarnemark, G. [Chalmers University of Technology, Department of Chemical and Biological Engineering, Nuclear Chemistry, SE-412 96 Goeteborg (Sweden)

2012-09-15

A method for the assessment of the combined uncertainty in gamma spectrometric measurements of plutonium composition and age was evaluated. Two materials were measured. Isotope dilution inductively coupled plasma sector field mass spectrometry (ID-ICP-SFMS) was used as a reference method for comparing the results obtained with the gamma spectrometric method for one of the materials. For this material (weapons grade plutonium) the measurement results were in agreement between the two methods for all measurands. Moreover, the combined uncertainty in all isotope ratios considered in this material (R{sub Pu238/Pu239}, R{sub Pu240/Pu239}, R{sub Pu241/Pu239}, and R{sub Am241/Pu241} for age determination) were limited by counting statistics. However, the combined uncertainty for the other material (fuel grade plutonium) were limited by the response fit, which shows that the uncertainty in the response function is important to include in the combined measurement uncertainty of gamma spectrometric measurements of plutonium.

Initiative to manufacture and characterize Baculovirus Reference Material

NARCIS (Netherlands)

Kamen, A.; Aucoin, M.; Merten, O.W.; Alves, P.C.M.; Hashimoto, Y.; Airenne, K.; Hu, Y.C.; Mezzina, M.; Oers, van M.M.

2011-01-01

This letter to the editor brings to the attention of researchers an initiative to develop a baculovirus reference material repository. To be successful this initiative needs the support of a broad panel of researchers working with baculovirus vectors for recombinant protein production and gene

Environmental isotope hydrology

International Nuclear Information System (INIS)

1973-01-01

Environmental isotope hydrology is a relatively new field of investigation based on isotopic variations observed in natural waters. These isotopic characteristics have been established over a broad space and time scale. They cannot be controlled by man, but can be observed and interpreted to gain valuable regional information on the origin, turnover and transit time of water in the system which often cannot be obtained by other techniques. The cost of such investigations is usually relatively small in comparison with the cost of classical hydrological studies. The main environmental isotopes of hydrological interest are the stable isotopes deuterium (hydrogen-2), carbon-13, oxygen-18, and the radioactive isotopes tritium (hydrogen-3) and carbon-14. Isotopes of hydrogen and oxygen are ideal geochemical tracers of water because their concentrations are usually not subject to change by interaction with the aquifer material. On the other hand, carbon compounds in groundwater may interact with the aquifer material, complicating the interpretation of carbon-14 data. A few other environmental isotopes such as 32 Si and 238 U/ 234 U have been proposed recently for hydrological purposes but their use has been quite limited until now and they will not be discussed here. (author)

Assessment of a dynamic reference material for calibration of full-field measurement systems

Science.gov (United States)

Hack, Erwin; Feligiotti, Mara; Davighi, Andrea; Whelan, Maurice; Wang, Weizhuo V.; Patterson, Eann A.

2012-10-01

For holography and speckle interferometry the calibration of the sensitivity is a must, because illumination and observation directions vary across the field of view. A numerical estimate or a static calibration using rigid body motions is standard, and reference materials exist for static strain calibration. Recently, reference materials for the dynamic calibration of optical instruments of displacement and strain measurement were designed and prototypes were manufactured in the European FP7 project ADVISE. We review the properties of the reference material and the concept of traceability for the field of displacement values by using a calibrated single point transducer. The mode shape is assessed using out-of-plane DSPI, Finite Element Analysis as well as analytic solutions of the plate vibration. We present measurements using stroboscopic DSPI on the reference material under acoustic excitation and compare the measured mode shapes to the ones predicted by FE analysis. We apply different comparison methodologies based on point-by-point deviations and on decomposition of the mode shapes into a set of orthogonal basis functions. The latter method is well suited to assess stability and reproducibility of a mode shape. Finally, the deviations are used to estimate the reference material uncertainty which is an essential parameter for determining the calibration uncertainty. Uncertainty contributions of the DSPI set-up are taken into account. To conclude, the application area and limitations of the reference material are discussed.

Separation of uranium isotopes

International Nuclear Information System (INIS)

Porter, J.T.

1980-01-01

Methods and apparatus are disclosed for separation of uranium isotopes by selective isotopic excitation of photochemically reactive uranyl salt source material at cryogenic temperatures, followed by chemical separation of selectively photochemically reduced U+4 thereby produced from remaining uranyl source material

Isotope separation process

International Nuclear Information System (INIS)

Thomas, W.R.L.

1979-01-01

The instant invention relates to an improved process for separating a material into two or more parts in each of which the abundances of the isotopes of a given element differ from the abundances of the isotopes of the same element in said material. More particularly, the invention relates to a method for the isotopically selective excitation of gas phase molecules by multiple infrared photon absorption followed by a step wherein more of the excited molecules than non-excited molecules are converted to a chemically different form which may be separated by means known in the art. This invention is useful for, but not limited to, the separation of the principal isotopes of uranium

Geographic variation of stable isotopes in African elephant ivory

Science.gov (United States)

Ziegler, S.; Merker, S.; Jacob, D.

2012-04-01

In 1989, the international community listed the African elephant in Appendix I of the Convention on International Trade in Endangered Species of Wild Fauna and Flora (CITES) thus prohibiting commercial ivory trade. Recent surveillance data show that the illegal trade in ivory has been growing worldwide. Long-term preservation of many of the African elephant populations can be supported with a control mechanism that helps with the implementation of remedial conservation action. Therefore, setting up a reference database that predicts the origin of ivory specimens can assist in determining smuggling routes and the provenance of illegal ivory. Our research builds on earlier work to seek an appropriate method for determining the area of origin for individual tusks. Several researchers have shown that the provenance of elephant ivory can be traced by its isotopic composition, but this is the first attempt to produce an integrated isotopic reference database of elephant ivory provenance. We applied a combination of various routine geochemical analyses to measure the stable isotope ratios of hydrogen, carbon, nitrogen, oxygen, and sulphur. Up to now, we analysed 606 ivory samples of known geographical origin from African range states, museums and private collections, comprising 22 African elephant range states. The isotopic measurements were superimposed with data layers from vegetation, geology and climate. A regression function for the isotope composition of the water isotopes in precipitation and collagen in ivory was developed to overcome the problem of imprecise origin of some of the sampled material. Multivariate statistics, such as nearest neighborhood and discriminate analysis were applied to eventually allow a statistical determination of the provenance for ivory of unknown origin. Our results suggest that the combination of isotopic parameters have the potential to provide predictable and complementary markers for estimating the origin of seized elephant ivory.

A Reference Guide for Cryogenic Properties of Materials

Energy Technology Data Exchange (ETDEWEB)

Weisend, John G

2003-09-16

A thorough knowledge of the behavior of materials at cryogenic temperatures is critical for the design of successful cryogenic systems. Over the past 50 years, a tremendous amount of material properties at cryogenic temperatures have been measured and published. This guide lists resources for finding these properties. It covers online databases, computer codes, conference proceedings, journals, handbooks, overviews and monographs. It includes references for finding reports issued by government laboratories and agencies. Most common solids and fluids used in cryogenics are covered.

Uranium tailings reference materials

International Nuclear Information System (INIS)

Smith, C.W.; Steger, H.F.; Bowman, W.S.

1984-01-01

Samples of uranium tailings from Bancroft and Elliot Lake, Ontario, and from Beaverlodge and Rabbit Lake, Saskatchewan, have been prepared as compositional reference materials at the request of the National Uranium Tailings Research Program. The four samples, UTS-1 to UTS-4, were ground to minus 104 μm, each mixed in one lot and bottled in 200-g units for UTS-1 to UTS-3 and in 100-g units for UTS-4. The materials were tested for homogeneity with respect to uranium by neutron activation analysis and to iron by an acid-decomposition atomic absorption procedure. In a free choice analytical program, 18 laboratories contributed results for one or more of total iron, titanium, aluminum, calcium, barium, uranium, thorium, total sulphur, and sulphate for all four samples, and for nickel and arsenic in UTS-4 only. Based on a statistical analysis of the data, recommended values were assigned to all elements/constituents, except for sulphate in UTS-3 and nickel in UTS-4. The radioactivity of thorium-230, radium-226, lead-210, and polonium-210 in UTS-1 to UTS-4 and of thorium-232, radium-228, and thorium-228 in UTS-1 and UTS-2 was determined in a radioanalytical program composed of eight laboratories. Recommended values for the radioactivities and associated parameters were calculated by a statistical treatment of the results

Certified reference materials for the determination of uranium, thorium, and plutonium

International Nuclear Information System (INIS)

Santoliquido, P.M.

1990-01-01

The New Brunswick Laboratory (NBL) is the Department of Energy's Nuclear Materials Measurements and Standards Laboratory. As part of its mission, NBL provides certified reference materials (CRMs) for the analysis of various types of materials encountered in the nuclear fuel cycle. The reference material program at NBL gained greater prominence in 1981, when an interagency agreement between NBL and NBS established NBL as the distributor of one category of SRMs, the special nuclear materials SRMs. When NBS reorganized and became NIST in 1987, NBL bought out the remaining inventory of these particular SRMs which it was already distributing and renamed them as CRMs. The difference between the radioactivity SRMs which NIST still provides and the nuclear material CRMs which NBL provides will be explained. NBL CRMs are distributed worldwide and are used in nuclear safeguards applications and in geological and environmental research. The current NBL CRM inventory will be described

Automated spike preparation system for Isotope Dilution Mass Spectrometry (IDMS)

International Nuclear Information System (INIS)

Maxwell, S.L. III; Clark, J.P.

1990-01-01

Isotope Dilution Mass Spectrometry (IDMS) is a method frequently employed to measure dissolved, irradiated nuclear materials. A known quantity of a unique isotope of the element to be measured (referred to as the ''spike'') is added to the solution containing the analyte. The resulting solution is chemically purified then analyzed by mass spectrometry. By measuring the magnitude of the response for each isotope and the response for the ''unique spike'' then relating this to the known quantity of the ''spike'', the quantity of the nuclear material can be determined. An automated spike preparation system was developed at the Savannah River Site (SRS) to dispense spikes for use in IDMS analytical methods. Prior to this development, technicians weighed each individual spike manually to achieve the accuracy required. This procedure was time-consuming and subjected the master stock solution to evaporation. The new system employs a high precision SMI Model 300 Unipump dispenser interfaced with an electronic balance and a portable Epson HX-20 notebook computer to automate spike preparation

A new digestion and chemical separation technique for rapid and highly reproducible determination of Lu/Hf and Hf isotope ratios in geological materials by mc-ICP-MS

DEFF Research Database (Denmark)

Bizzarro, Martin; Baker, J.A.; Ulfbeck, D.

2003-01-01

for isotopic analysis of the Sm-Nd system and/or the other HFSE (Ti, Zr). Total procedural blanks for this technique are 5 g) samples. We present data from replicate digestions of international rock reference materials which....... The relative simplicity of this technique, coupled with the ease of digestion (and samplespike equilibration) of large difficult-to-dissolve samples, and the speed (2 days) with which samples can be digested and processed through the chemical separation scheme makes it an attractive new method for preparing...

Contribution of bulk mass spectrometry isotopic analysis to characterization of materials in the framework of CMX-4

International Nuclear Information System (INIS)

Kuchkin, A.; Stebelkov, V.; Zhizhin, K.; Lierse von Gostomski, Ch.; Kardinal, Ch.; Loi, E.; Keegan, E.; Kristo, M.J.

2018-01-01

Seven laboratories used the results of bulk uranium isotopic analysis by either inductively coupled plasma mass spectrometry (ICP-MS) or thermal ionization mass spectrometry (TIMS) for characterization of the samples in the Nuclear Forensic International Technical Working Group fourth international collaborative material exercise, CMX-4. Comparison of the measured isotopic compositions of uranium in three exercise samples is implemented for identifying any differences or similarities between the samples. The role of isotopic analyses in the context of a real nuclear forensic investigation is discussed. Several limitations in carrying out ICP-MS or TIMS analysis in CMX-4 are noted. (author)

Isotope-beam modification of materials at eV energies

International Nuclear Information System (INIS)

Krug, C.; Radtke, C.; Stedile, F.C.; Baumvol, I.J.R.

2001-01-01

We developed a low energy ion beam deposition system for isotope-selective modification of materials. It consists of a conventional ion implanter (HVEE 500 kV) and an attachable deceleration system. 29 (N 2 ) + ion beams were used for the nitridation of Si(0 0 1) and the resulting 15 N retained doses and profiles were determined by narrow nuclear resonance profiling. 29 Si was deposited on amorphous carbon films on Si(0 0 1) and the doses evaluated by channeled α particle beams with detection of scattered α at grazing angles. 29 Si was also deposited on Si(0 0 1) and the resulting profiles determined by narrow nuclear resonance

Direct lead isotope analysis in Hg-rich sulfides by LA-MC-ICP-MS with a gas exchange device and matrix-matched calibration

Energy Technology Data Exchange (ETDEWEB)

Zhang, Wen [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China); Hu, Zhaochu, E-mail: zchu@vip.sina.com [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China); Günther, Detlef, E-mail: guenther@inorg.chem.ethz.ch [ETH Zurich, Laboratory for Inorganic Chemistry, CH-8093, Zurich (Switzerland); Liu, Yongsheng; Ling, Wenli; Zong, Keqing; Chen, Haihong; Gao, Shan [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China)

2016-12-15

In situ Pb isotope data of sulfide samples measured by LA-MC-ICP-MS provide valuable geochemical information for studies of the origin and evolution of ore deposits. However, the severe isobaric interference of {sup 204}Hg on {sup 204}Pb and the lack of matrix-matched sulfide reference materials limit the precision of Pb isotopic analyses for Hg-rich sulfides. In this study, we observe that Hg forms vapor and can be completely removed from sample aerosol particles produced by laser ablation using a gas exchange device. Additionally, this device does not influence the signal intensities of Pb isotopes. The within-run precision, the external reproducibility and the analytical accuracy are significantly improved for the Hg-rich sulfide samples using this mercury-vapor-removing device. Matrix effects are observed when using silicate glass reference materials as the external standards to assess the relationship of mass fractionation factors between Tl and Pb in sulfide samples, resulting in a maximum deviation of ∼0.20% for {sup 20x}Pb/{sup 204}Pb. Matrix-matched reference materials are therefore required for the highly precise and accurate Pb isotope analyses of sulfide samples. We investigated two sulfide samples, MASS-1 (the Unites States Geological Survey reference materials) and Sph-HYLM (a natural sphalerite), as potential candidates. Repeated analyses of the two proposed sulfide reference materials by LA-MC-ICP-MS yield good external reproducibility of <0.04% (RSD, k = 2) for {sup 20x}Pb/{sup 206}Pb and <0.06% (RSD, k = 2) for {sup 20x}Pb/{sup 204}Pb with the exception of {sup 20x}Pb/{sup 204}Pb in MASS-1, which provided an external reproducibility of 0.24% (RSD, k = 2). Because the concentration of Pb in MASS-1 (76 μg g{sup −1}) is ∼5.2 times lower than that in Sph-HYLM (394 ± 264 μg g{sup −1}). The in situ analytical results of MASS-1 and Sph-HYLM are consistent with the values obtained by solution MC-ICP-MS, demonstrating the reliability

10 CFR 433.3 - Materials incorporated by reference.

Science.gov (United States)

2010-01-01

... 10 Energy 3 2010-01-01 2010-01-01 false Materials incorporated by reference. 433.3 Section 433.3 Energy DEPARTMENT OF ENERGY ENERGY CONSERVATION ENERGY EFFICIENCY STANDARDS FOR THE DESIGN AND...) 741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations...

Approved reference and testing materials for use in Nuclear Waste Management Research and Development Programs

International Nuclear Information System (INIS)

Mellinger, G.B.; Daniel, J.L.

1984-12-01

This document, addressed to members of the waste management research and development community summarizes reference and testing materials available from the Nuclear Waste Materials Characterization Center (MCC). These materials are furnished under the MCC's charter to distribute reference materials essential for quantitative evaluation of nuclear waste package materials under development in the US. Reference materials with known behavior in various standard waste management related tests are needed to ensure that individual testing programs are correctly performing those tests. Approved testing materials are provided to assist the projects in assembling materials data base of defensible accuracy and precision. This is the second issue of this publication. Eight new Approved Testing Materials are listed, and Spent Fuel is included as a separate section of Standard Materials because of its increasing importance as a potential repository storage form. A summary of current characterization information is provided for each material listed. Future issues will provide updates of the characterization status of the materials presented in this issue, and information about new standard materials as they are acquired. 7 references, 1 figure, 19 tables

Development of a highly precise ID-ICP-SFMS method for analysis of low concentrations of lead in rice flour reference materials.

Science.gov (United States)

Zhu, Yanbei; Inagaki, Kazumi; Yarita, Takashi; Chiba, Koichi

2008-07-01

Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion blank for Pb was reduced to 0.21 ng g(-1) after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 +/- 0.8 ng g(-1) (mean +/- expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 +/- 3 ng g(-1) and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a, NIES CRM 10-a, and NIES CRM 10-b, were 7.32 +/- 0.24 ng g(-1) (n = 5), 1010 +/- 10 ng g(-1) (n = 5), and 1250 +/- 20 ng g(-1) (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the National Metrology Institute of Japan (NMIJ) was observed to be 4.36 +/- 0.28 ng g(-1) (n = 10 bottles).

The stability of uranium microspheres for future application as reference standard in analytical measurements

Energy Technology Data Exchange (ETDEWEB)

Middendorp, R.; Duerr, M.; Bosbach, D. [Forschungszentrum Juelich GmbH, IEK-6, 52428 Juelich (Germany)

2016-07-01

The monitoring of fuel-cycle facilities provides a tool to confirm the compliant operation, for example with respect to emissions into the environment or to supervise non-proliferation commitments. Hereby, anomalous situations can be detected in a timely manner and responsive action can be initiated to prevent an escalation into an event of severe consequence to society. In order to verify non-nuclear weapon states' compliance with the non-proliferation treaty (NPT), international authorities such as the International Atomic Energy Agency (IAEA) conduct inspections at facilities dealing with fissile or fertile nuclear materials. One measure consists of collection of swipe samples through inspectors for later analysis of collected nuclear material traces in the laboratory. Highly sensitive mass spectrometric methods provide a means to detect traces from nuclear material handling activities that provide indication of undeclared use of the facility. There are, however, no relevant (certified) reference materials available that can be used as calibration or quality control standards. Therefore, an aerosol-generation based process was established at Forschungszentrum Juelich for the production of spherical, mono-disperse uranium oxide micro-particles with accurately characterized isotopic compositions and amounts of uranium in the pico-gram range. The synthesized particles are studied with respect to their suitability as (certified) reference material in ultra-trace analysis. Several options for preparation and stabilization of the particles are available, where preparation of particles in suspension offers the possibility to produces specific particle mixtures. In order to assess the stability of particles, dissolution behavior and isotope exchange effects of particles in liquid suspension is studied on the bulk of suspended particles and also via micro-analytical methods applied for single particle characterization. The insights gained within these studies will

Uranium isotope fractionation resulting from UF6 vapor distillation from containers

International Nuclear Information System (INIS)

Hedge, W.D.; Turner, C.M.

1985-01-01

This empirical study for possible isotopic fractionation due to UF 6 vapor distillation from valved containers was performed to determine the effects of repeated vapor sampling. Four different experiments were performed, each of which varied by the method of measuring the isotopic contents and/or by the difference in temperature gradients as follows: The ratio of the parent UF 6 to the desublimed UF 6 collected at liquid nitrogen temperature and homogenized was measured by sampling the containers. The ratio of the parent UF 6 to the desublimed UF 6 collected at liquid nitrogen temperature and homogenized was measured by direct comparison to each other without subsampling. The ratio of the parent UF 6 to the desublimed UF 6 collected at liquid nitrogen and ice-water temperatures and homogenized was measured by indirect comparison to a common UF 6 reference material without subsampling. The ratio of the parent UF 6 to the desublimed UF 6 collected at liquid nitrogen temperature without homogenizing was measured by indirect comparison to a common UF 6 reference. Gas-phase, relative mass spectrometry was used for all isotopic measurements. Results of the study indicate that fractionation does occur. The U-235 isotope becomes more enriched in the parent container as the UF 6 is vaporized from it and desublimed into the receiving cylinder; i.e., the vaporized fraction is enriched in the U-238 isotope. The degree of fractionation indicates that the separation is due to the U-238 isotope of UF 6 having a higher vapor pressure than the U-235 isotope of UF 6 . 3 refs., 4 figs., 4 tabs

Soiled-based uranium disequilibrium and mixed uranium-thorium series radionuclide reference materials

International Nuclear Information System (INIS)

Donivan, S.; Chessmore, R.

1988-12-01

The US Department of Energy (DOE) Office of Remedial Action and Waste Technology has assigned the Technical Measurements Center (TMC), located at the DOE Grand Junction Colorado, Projects Office and operated by UNC Geotech (UNC), the task of supporting ongoing remedial action programs by providing both technical guidance and assistance in making the various measurements required in all phases of remedial action work. Pursuant to this task, the Technical Measurements Center prepared two sets of radionuclide reference materials for use by remedial action contractors and cognizant federal and state agencies. A total of six reference materials, two sets comprising three reference materials each, were prepared with varying concentrations of radionuclides using mill tailings materials, ores, and a river-bottom soil diluent. One set (disequilibrium set) contains varying amounts of uranium with nominal amounts of radium-226. The other set (mixed-nuclide set) contains varying amounts of uranium-238 and thorium-232 decay series nuclides. 14 refs., 10 tabs

Target materials for exotic ISOL beams

CERN Document Server

Gottberg, A

2016-01-01

The demand for intensity, purity, reliability and availability of short-lived isotopes far from stability is steadily high, and considerably exceeding the supply. In many cases the ISOL (Isotope Separation On-Line) method can provide beams of high intensity and purity. Limitations in terms of accessible chemical species and minimum half-life are driven mainly by chemical reactions and physical processes inside of the thick target. A wide range of materials are in use, ranging from thin metallic foils and liquids to refractory ceramics, while poly-phasic mixed uranium carbides have become the reference target material for most ISOL facilities world-wide. Target material research and development is often complex and especially important post-irradiation analyses are hindered by the high intrinsic radiotoxicity of these materials. However, recent achievements have proven that these investigations are possible if the effort of different facilities is combined, leading to the development of new material matrices t...

Evaluation of Botanical Reference Materials for the Determination of Vanadium in Biological Samples

DEFF Research Database (Denmark)

Heydorn, Kaj; Damsgaard, Else

1982-01-01

Three botanical reference materials prepared by the National Bureau of Standards have been studied by neutron activation analysis to evaluate their suitability with respect to the determination of vanadium in biological samples. Various decomposition methods were applied in connection with chemic....... A reference value of 1.15 mg/kg of this material is recommended, based on results from 3 different methods. All three materials are preferable to SRM 1571 Orchard Leaves, while Bowen's Kale remains the material of choice because of its lower concentration....

Stable isotope enrichment: Current and future potential

International Nuclear Information System (INIS)

Tracy, J.G.; Aaron, W.S.

1992-01-01

Oak Ridge National Laboratory (ORNL) operates the Isotope Enrichment Facility for the purpose of providing enriched stable isotopes, selected radioactive isotopes (including the actinides), and isotope-related materials and services for use in various research applications. ORNL is responsible for isotope enrichment and the distribution of approximately 225 nongaseous stable isotopes from 50 multi-isotopic elements. Many enriched isotope products are of prime importance in the fabrication of nuclear targets and the subsequent production of special radionuclides. State-of-the-art techniques to achieve special isotopic, chemical, and physical requirements are performed at ORNL This report describes the status and capabilities of the Isotope Enrichment Facility and the Isotope Research Materials Laboratory as well as emphasizing potential advancements in enrichment capabilities

Stable isotope enrichment - current and future potential

International Nuclear Information System (INIS)

Tracy, J.G.; Aaron, W.S.

1993-01-01

Oak Ridge National Laboratory (ORNL) operates the Isotope Enrichment Facility for the purpose of providing enriched stable isotopes, selected radioactive isotopes (including the actinides), and isotope-related materials and services for use in various research applications. ORNL is responsible for isotope enrichment and the distribution of approximately 225 nongaseous stable isotopes from 50 multi-isotopic elements. Many enriched isotope products are of prime importance in the fabrication of nuclear targets and the subsequent production of special radionuclides. State-of-the-art techniques to achieve special isotopic, chemical, and physical requirements are performed at ORNL. This report describes the status and capabilities of the Isotope Enrichment Facility and the Isotope Research Materials Laboratory as well as emphasizing potential advancements in enrichment capabilities. (orig.)

Development of C-reactive protein certified reference material NMIJ CRM 6201-b: optimization of a hydrolysis process to improve the accuracy of amino acid analysis.

Science.gov (United States)

Kato, Megumi; Kinumi, Tomoya; Yoshioka, Mariko; Goto, Mari; Fujii, Shin-Ichiro; Takatsu, Akiko

2015-04-01

To standardize C-reactive protein (CRP) assays, the National Metrology Institute of Japan (NMIJ) has developed a C-reactive protein solution certified reference material, CRM 6201-b, which is intended for use as a primary reference material to enable the SI-traceable measurement of CRP. This study describes the development process of CRM 6201-b. As a candidate material of the CRM, recombinant human CRP solution was selected because of its higher purity and homogeneity than the purified material from human serum. Gel filtration chromatography was used to examine the homogeneity and stability of the present CRM. The total protein concentration of CRP in the present CRM was determined by amino acid analysis coupled to isotope-dilution mass spectrometry (IDMS-AAA). To improve the accuracy of IDMS-AAA, we optimized the hydrolysis process by examining the effect of parameters such as the volume of protein samples taken for hydrolysis, the procedure of sample preparation prior to the hydrolysis, hydrolysis temperature, and hydrolysis time. Under optimized conditions, we conducted two independent approaches in which the following independent hydrolysis and liquid chromatography-isotope dilution mass spectrometry (LC-IDMS) were combined: one was vapor-phase acid hydrolysis (130 °C, 24 h) and hydrophilic interaction liquid chromatography-mass spectrometry (HILIC-MS) method, and the other was microwave-assisted liquid-phase acid hydrolysis (150 °C, 3 h) and pre-column derivatization liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. The quantitative values of the two different amino acid analyses were in agreement within their uncertainties. The certified value was the weighted mean of the results of the two methods. Uncertainties from the value-assignment method, between-method variance, homogeneity, long-term stability, and short-term stability were taken into account in evaluating the uncertainty for a certified value. The certified value and the

APEX (Air Pollution Exercise) Volume 20: Reference Materials.

Science.gov (United States)

Environmental Protection Agency, Research Triangle Park, NC. Office of Manpower Development.

The Reference Materials Manual is part of a set of 21 manuals (AA 001 009-001 029) used in APEX (Air Pollution Exercise), a computerized college and professional level "real world" game simulation of a community with urban and rural problems, industrial activities, and air pollution difficulties. For the purposes of the gaming exercise, APEX…

Instrumental neutron activation analysis for the certification of biological reference materials

International Nuclear Information System (INIS)

Ambulkar, M.N.; Chutke, N.L.; Garg, A.N.

1992-01-01

A multielemental instrumental neutron activation analysis (INAA) method by short and long irradiation has been employed for the determination of 22 minor and trace constituents in two proposed Standard Reference Materials P-RBF and P-WBF from Institute of Radioecology and Applied Nuclear Techniques, Czechoslovakia. Also some biological standards such as Bowen's Kale, Cabbage leaves (Poland) including wheat and rice flour samples of local origin were analysed. It is suggested that INAA is an ideal method for the certification of reference materials of biological matrices. (author). 7 refs., 1 tab

Survey of currently available reference materials for use in connection with the determination of trace elements in biological materials

International Nuclear Information System (INIS)

Parr, R.M.

1983-09-01

Elemental analysis of biological materials is at present the subject of intensive study by many different research groups throughout the world, in view of the importance of these trace elements in health and medical diagnosis. IAEA and other organizations are now making a variety of suitable reference materials available for use in connection with the determination of trace elements in biological materials. To help analysts in making a selection from among these various materials, the present report provides a brief survey of data for all such biological reference materials known to the author. These data are compiled by the author from January 1982 to June 1983

Uncertainties achievable for uranium isotope-amount ratios. Estimates based on the precision and accuracy of recent characterization measurements

International Nuclear Information System (INIS)

Mathew, K.J.; Essex, R.M.; Gradle, C.; Narayanan, U.

2015-01-01

Certified reference materials (CRMs) recently characterized by the NBL for isotope-amount ratios are: (i) CRM 112-A, Uranium (normal) Metal Assay and Isotopic Standard, (ii) CRM 115, Uranium (depleted) Metal Assay and Isotopic Standard, and (iii) CRM 116-A, Uranium (enriched) Metal Assay and Isotopic Standard. NBL also completed re-characterization of the isotope-amount ratios in CRM 125-A, Uranium (UO 2 ) Pellet Assay, Isotopic, and Radio-chronometric Standard. Three different TIMS analytical techniques were employed for the characterization analyses. The total evaporation technique was used for the major isotope-amount ratio measurement, the modified total evaporation technique was used for both the major and minor isotope-amount ratios, and minor isotope-amount ratios were also measured using a Conventional technique. Uncertainties for the characterization studies were calculated from the combined TIMS data sets following the ISO Guide to the expression of uncertainty in measurement. The uncertainty components for the isotope-amount ratio values are discussed. (author)

Quality of Standard Reference Materials for Short Time Activation Analysis

International Nuclear Information System (INIS)

Ismail, S.S.; Oberleitner, W.

2003-01-01

Some environmental reference materials (CFA-1633 b, IAEA-SL-1, SARM-1,BCR-176, Coal-1635, IAEA-SL-3, BCR-146, and SRAM-5) were analysed by short-time activation analysis. The results show that these materials can be classified in three groups, according to their activities after irradiation. The obtained results were compared in order to create a quality index for determination of short-lived nuclides at high count rates. It was found that Cfta is not a suitable standard for determining very short-lived nuclides (half-lives<1 min) because the activity it produces is 15-fold higher than that SL-3. Biological reference materials, such as SRM-1571, SRM-1573, SRM-1575, SRM-1577, IAEA-392, and IAEA-393, were also investigated by a higher counting efficiency system. The quality of this system and its well-type detector for investigating short-lived nuclides was discussed

Measurement of zinc stable isotope ratios in biogeochemical matrices by double-spike MC-ICPMS and determination of the isotope ratio pool available for plants from soil.

Science.gov (United States)

Arnold, Tim; Schönbächler, Maria; Rehkämper, Mark; Dong, Schuofei; Zhao, Fang-Jie; Kirk, Guy J D; Coles, Barry J; Weiss, Dominik J

2010-12-01

Analysis of naturally occurring isotopic variations is a promising tool for investigating Zn transport and cycling in geological and biological settings. Here, we present the recently installed double-spike (DS) technique at the MAGIC laboratories at Imperial College London. The procedure improves on previous published DS methods in terms of ease of measurement and precisions obtained. The analytical method involves addition of a (64)Zn-(67)Zn double-spike to the samples prior to digestion, separation of Zn from the sample matrix by ion exchange chromatography, and isotopic analysis by multiple-collector inductively coupled plasma mass spectrometry. The accuracy and reproducibility of the method were validated by analyses of several in-house and international elemental reference materials. Multiple analyses of pure Zn standard solutions consistently yielded a reproducibility of about ±0.05‰ (2 SD) for δ(66)Zn, and comparable precisions were obtained for analyses of geological and biological materials. Highly fractionated Zn standards analyzed by DS and standard sample bracketing yield slightly varying results, which probably originate from repetitive fractionation events during manufacture of the standards. However, the δ(66)Zn values (all reported relative to JMC Lyon Zn) for two less fractionated in-house Zn standard solutions, Imperial Zn (0.10 ± 0.08‰: 2 SD) and London Zn (0.08 ± 0.04‰), are within uncertainties to data reported with different mass spectrometric techniques and instruments. Two standard reference materials, blend ore BCR 027 and ryegrass BCR 281, were also measured, and the δ(66)Zn were found to be 0.25 ± 0.06‰ (2 SD) and 0.40 ± 0.09‰, respectively. Taken together, these standard measurements ascertain that the double-spike methodology is suitable for accurate and precise Zn isotope analyses of a wide range of natural samples. The newly installed technique was consequently applied to soil samples and soil leachates to

Element concentrations in candidate biological and environmental reference materials by k0-standardized INAA

International Nuclear Information System (INIS)

Freitas, M.C.

1993-01-01

K 0 -Based Neutron Activation Analysis (k 0 INAA) was used to analyze the candidate reference materials Apple Leaves and Peach Leaves, and Oriental Tobacco Leaves and Virginia Tobacco Leaves. Concentration values for 27 elements were measured. The accuracy was ascertained by analysis of two certified reference materials. NIST 1572 Citrus Leaves and 1573 Tomato Leaves. The homogeneity test of the IAEA Evernia prunastri candidate reference material in aliquots ≥ 100 mg is extended to the elements Sc, Cr, Fe, Co, Zn, Rb, Sb, Cs, Ba, Ce and Th. (orig.)

Survey of currently available reference materials for use in connection with the determination of trace elements in biological and environmental materials

International Nuclear Information System (INIS)

Muramatsu, Y.; Parr, R.M.

1985-12-01

This report focuses on analytical reference materials which have been developed for use in connection with the determination of toxic and essential trace elements in biomedical and health-related environmental samples. Data are reported on 60 biological and 40 environmental (non-biological) reference materials from 11 suppliers. Certified concentration values (or their equivalents) and non-certified concentration values (or information values) are presented in various tables which are intended to help the user select a reference material that matches as closely as possible (i.e. with respect to matrix type and concentration of the element of interest) the ''real'' samples that are to be analysed. These tables have been generated from a database characterized by the following parameters: total number of reference materials=100; total number of elements recorded=69; total number of concentration values recorded=1771. Also included in the report is information (where available) on the cost of each material, the unit weight or volume supplied, and the minimum weight of material recommended for analysis. (author)

pH-dependent equilibrium isotope fractionation associated with the compound specific nitrogen and carbon isotope analysis of substituted anilines by SPME-GC/IRMS.

Science.gov (United States)

Skarpeli-Liati, Marita; Turgeon, Aurora; Garr, Ashley N; Arnold, William A; Cramer, Christopher J; Hofstetter, Thomas B

2011-03-01

Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry (GC/IRMS) was used to elucidate the effects of N-atom protonation on the analysis of N and C isotope signatures of selected aromatic amines. Precise and accurate isotope ratios were measured using polydimethylsiloxane/divinylbenzene (PDMS/DVB) as the SPME fiber material at solution pH-values that exceeded the pK(a) of the substituted aniline's conjugate acid by two pH-units. Deviations of δ(15)N and δ(13)C-values from reference measurements by elemental analyzer IRMS were small (IRMS. Under these conditions, the detection limits for accurate isotope ratio measurements were between 0.64 and 2.1 mg L(-1) for δ(15)N and between 0.13 and 0.54 mg L(-1) for δ(13)C, respectively. Substantial inverse N isotope fractionation was observed by SPME-GC/IRMS as the fraction of protonated species increased with decreasing pH leading to deviations of -20‰ while the corresponding δ(13)C-values were largely invariant. From isotope ratio analysis at different solution pHs and theoretical calculations by density functional theory, we derived equilibrium isotope effects, EIEs, pertinent to aromatic amine protonation of 0.980 and 1.001 for N and C, respectively, which were very similar for all compounds investigated. Our work shows that N-atom protonation can compromise accurate compound-specific N isotope analysis of aromatic amines.

Data on trapping and re-emission of energetic hydrogen isotopes and helium in materials, supplement 1

International Nuclear Information System (INIS)

Yamaguchi, Sadae; Sugizaki, Yasuaki; Ozawa, Kunio; Nakai, Yohta.

1984-05-01

This is the supplement to the data on trapping and re-emission of energetic hydrogen isotopes and helium in materials (JAERI-M 82-118). It contains 32 data up to end of 1982, dividing it into following 6 sections: 1) Dose Dependence, 2) Target Material Dependence, 3) Target Temperature Dependence, 4) Incident Energy Dependence, 5) Damage Effects and 6) Ion-Induced Release. (author)

Analysis of FDA in-house food reference materials with anticoincidence INAA

International Nuclear Information System (INIS)

Anderson, D.L.; Cunningham, W.C.

2013-01-01

In-house reference material (IRM) cocoa powder (CCP) has been in use at US Food and Drug Administration laboratories for about 15 years. A single lot of commercial material was originally characterized for 32 elements by several laboratories and five techniques. A unique approach for basis weight determination based upon ambient relative humidity was developed for CCP, eliminating the need for dry weight determinations. The CCP Reference Sheet is updated by incorporating new results approximately every 5 years. The last update occurred in 2006. As part of an effort to revalidate and update values for CCP, anticoincidence instrumental neutron activation analysis (INAA) was used to determine mass fractions for 16 of the originally characterized elements, as well as to provide information on 16 other elements. Results were in very good agreement with 2006 Reference Sheet values. A new candidate IRM, fresh-frozen swordfish (FFSF) powder, was produced by adding inorganic As, Cd, Cr, Hg, Pb, Sb, and Se to liquid nitrogen-frozen commercial swordfish filets which were then homogenized. Portions of FFSF were analyzed by INAA to provide mass fraction and homogeneity information for As, Cd, Cr, Hg, Sb, and Se as well as for eight other elements occurring naturally in the material. Non-homogeneities were ≤2.5 % for As, Br, Cd, and Cs, and ≤1.8 % for Cr, Hg, Rb, Sb, and Se. Certified reference materials DORM-3 Fish Protein powder and fresh-frozen SRM 1947 Lake Michigan Fish Tissue were analyzed as controls. (author)

Optimization of instrumental neutron activation analysis for the within-bottle homogeneity study of reference materials of marine origin

International Nuclear Information System (INIS)

Silva, Daniel Pereira da

2017-01-01

The use of reference materials has been increasing in chemical analysis laboratories as its use is important for measurement validation in analytical chemistry. Such materials are generally imported, which require high financial investments in order to acquire them, and therefore it impacts on the difficulty to many national laboratories to use reference materials in their chemical analysis routine. Certification of reference materials is a complex process that assumes that the user is given appropriate assigned values of the properties of interests in the material. In this process, the homogeneity of the material must be checked. In this study, the within-bottle homogeneity study for the elements K, Mg, Mn, Na and V was performed for two reference materials of marine origin: the mussel reference material produced at the Neutron Activation Laboratory (LAN) of IPEN - CNEN/SP and an oyster tissue reference material produced abroad. For this purpose, the elements were determined in subsamples with masses varying between 1 and 250 mg by Instrumental Neutron Activation Analysis (INAA) and minimum sample intakes were estimated, ranging from 0.015 g for Na in the mussel reference material to 0.100 g for V in the two reference materials. (author)

Quantification of urea in serum by isotope dilution HPLC/MS

International Nuclear Information System (INIS)

Lee, Hwa Shim; Park, Sang Ryoul

2005-01-01

Urea in blood has been measured as an effective marker for diagnosis of renal function. Urea which is the end-product of nitrogen containing metabolites such as proteins is filtered through glomeruli of kidneys and then excreted as urine. If the renal function is deteriorated, the urea concentration in blood will be increased, from which the healthiness of renal function is judged. In order to improve the confidence of diagnosis results, the results must keep traceability chain to certified reference materials, which was certified by primary reference method. In this study, we proposed Isotope Dilution-Liquid Chromatography/Mass Spectrometry (ID-LC/MS) as a candidate primary method, in which 15 N 2 -urea is used as an internal reference material. The developed method is highly accurate in principle and is convenient as it does not require cumbersome derivatization 0.1 mmol/L ammonium chloride was selected as a mobile phase for HPLC because it provide low interference in MS analysis of relatively low molecular weighted urea. HPLC and MS were connected with an ElectroSpry Ionization(ESI) interface of positive mode, which provided high sensitivity and reproducibility. The developed method was validated with internationally recognized reference materials, and we have obtained satisfactory results in an international ring trial. The expanded uncertainty calculated according to ISO guide was 1.8% at 95% confidence interval. The developed method is being used as a primary reference measurement method such as for certification of serum Certified Reference Materials (CRMs)

Proper use of reference materials for trace element analysis and updates on their availability

International Nuclear Information System (INIS)

Snell, J.P.

2009-01-01

Full text: As different spectroscopic methods are used to certify reference materials (RMs) for element content, there is close interrelation between development of new methods and availability of new certified reference materials (CRMs). The Institute for Reference Materials and Measurements (IRMM) monitors changing scientific and regulatory interests, and adapts materials to current and predicted needs. This includes the development of CRMs with new matrices, or changing analytes and concentration levels for existing types of CRMs. Recent examples are CRMs to support the EC Directives on air quality and water, for nanoparticle characterization, and progressing international standards for biofuel measurements. User guidance including appropriate CRM selection, and use of uncertainties in comparing results will be highlighted. (author)

Study on material attractiveness aspect of spent nuclear fuel of LWR and FBR cycles based on isotopic plutonium production

International Nuclear Information System (INIS)

Permana, Sidik; Suzuki, Mitsutoshi; Saito, Masaki; Novitrian,; Waris, Abdul; Suud, Zaki

2013-01-01

Highlights: • The paper analyzes the plutonium production of recycling nuclear fuel option. • To evaluate material attractiveness based on intrinsic feature of material barrier. • Evaluation based on isotopic plutonium composition of spent fuel LWR and FBR. • Even mass number of plutonium gives a significant contribution to material barrier, in particular Pu-238 and Pu-240. • Doping MA in FBR blanket is effective to increase material barrier from weapon grade plutonium to more than MOX fuel grade. - Abstract: Recycling minor actinide (MA) as well as used uranium and plutonium can be considered to reduce nuclear waste production as well as to increase the intrinsic aspect of nuclear nonproliferation as doping material. Plutonium production as a significant aspect of recycling nuclear fuel option, gives some advantages and challenges, such as fissile material utilization of plutonium as well as production of some even mass number plutonium. The study intends to evaluate the material attractiveness based on the intrinsic feature of material barrier such as plutonium composition, decay heat and spontaneous fission neutron components from spent fuel (SF) light water reactor (LWR) and fast breeder reactor (FBR) cycles. A significant contribution has been shown by decay heat (DH) and spontaneous fission neutron (SFN) of even mass number of plutonium isotopes to the total DH and SFN of plutonium element, in particular from isotopic plutonium Pu-238 and Pu-240 contributions. Longer decay cooling time and higher burnup are effective to increase the material barrier (DH and SFN) level from reactor grade plutonium level to MOX grade plutonium level. Material barrier of plutonium element from spent fuel (SF) FBR in the core regions has similarity to the material barrier profile of SF LWR which can be categorized as MOX fuel grade plutonium. Plutonium compositions, DH and SFN components are categorized as weapon grade plutonium level for FBR blanket regions with no

Sr and Pb isotopic composition of five USGS glasses (BHVO-2G, BIR-1G, BCR-2G, TB-1G, NKT-1G)

NARCIS (Netherlands)

Elburg, M.A.; Vroon, P.Z.; van der Wagt, R.A.C.A.; Tchalikian, A.

2005-01-01

Sr isotopic compositions and Rb/Sr ratios of three USGS glasses (BHVO-2G, BIR-1G, BCR-2G) are identical to those of the original USGS reference materials. NKT-1G and TB-1G give values of 0.70351 and 0.70558, respectively. Pb isotopic ratios were measured by the standard-sample bracketing technique

Isotope production

Energy Technology Data Exchange (ETDEWEB)

Lewis, Dewi M.

1995-07-15

Some 2 0% of patients using radiopharmaceuticals receive injections of materials produced by cyclotrons. There are over 200 cyclotrons worldwide; around 35 are operated by commercial companies solely for the production of radio-pharmaceuticals with another 25 accelerators producing medically useful isotopes. These neutron-deficient isotopes are usually produced by proton bombardment. All commonly used medical isotopes can be generated by 'compact' cyclotrons with energies up to 40 MeV and beam intensities in the range 50 to 400 microamps. Specially designed target systems contain gram-quantities of highly enriched stable isotopes as starting materials. The targets can accommodate the high power densities of the proton beams and are designed for automated remote handling. The complete manufacturing cycle includes large-scale target production, isotope generation by cyclotron beam bombardment, radio-chemical extraction, pharmaceutical dispensing, raw material recovery, and labelling/packaging prior to the rapid delivery of these short-lived products. All these manufacturing steps adhere to the pharmaceutical industry standards of Good Manufacturing Practice (GMP). Unlike research accelerators, commercial cyclotrons are customized 'compact' machines usually supplied by specialist companies such as IBA (Belgium), EBCO (Canada) or Scanditronix (Sweden). The design criteria for these commercial cyclotrons are - small magnet dimensions, power-efficient operation of magnet and radiofrequency systems, high intensity extracted proton beams, well defined beam size and automated computer control. Performance requirements include rapid startup and shutdown, high reliability to support the daily production of short-lived isotopes and low maintenance to minimize the radiation dose to personnel. In 1987 a major step forward in meeting these exacting industrial requirements came when IBA, together with the University of Louvain-La-Neuve in Belgium, developed the Cyclone-30

Discrimination of source reactor type by multivariate statistical analysis of uranium and plutonium isotopic concentrations in unknown irradiated nuclear fuel material.

Science.gov (United States)

Robel, Martin; Kristo, Michael J

2008-11-01

The problem of identifying the provenance of unknown nuclear material in the environment by multivariate statistical analysis of its uranium and/or plutonium isotopic composition is considered. Such material can be introduced into the environment as a result of nuclear accidents, inadvertent processing losses, illegal dumping of waste, or deliberate trafficking in nuclear materials. Various combinations of reactor type and fuel composition were analyzed using Principal Components Analysis (PCA) and Partial Least Squares Discriminant Analysis (PLSDA) of the concentrations of nine U and Pu isotopes in fuel as a function of burnup. Real-world variation in the concentrations of (234)U and (236)U in the fresh (unirradiated) fuel was incorporated. The U and Pu were also analyzed separately, with results that suggest that, even after reprocessing or environmental fractionation, Pu isotopes can be used to determine both the source reactor type and the initial fuel composition with good discrimination.

The calibration of XRF polyethylene reference materials with k 0-NAA and ICP-AES

International Nuclear Information System (INIS)

Swagten, Josefien; Bossus, Daniel; Vanwersch, Hanny

2006-01-01

Due to the lack of commercially available polyethylene reference materials for the calibration of X-ray fluorescence spectrometers (XRF), DSM Resolve, in cooperation with PANalytical, prepared and calibrated such a set of standards in 2005. The reference materials were prepared based on the addition of additives to virgin polyethylene. The mentioned additives are added to improve the performance of the polymers. The elements present in additives are tracers for the used additives. The reference materials contain the following elements: F, Na, Mg, Al, Si, P, S, Ca, Ti and Zn in the concentration range of 5 mg/kg for Ti, up to 600 mg/kg for Mg. The calibration of the reference materials, including a blank, was performed using inductively coupled plasma atomic emission spectrometry (ICP-AES) and Neutron Activation Analysis (k 0 -NAA). ICP-AES was used to determine the elements Na, Mg, Al, P, Ca, Ti and Zn whereas k 0 -NAA was used for F, Na, Mg, Al, Ca, Ti and Zn. Over the complete concentration range, a good agreement of the results was found between the both techniques. This project has shown that within DSM Resolve, it is possible to develop and to calibrate homogenous reference materials for XRF

Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers

Science.gov (United States)

Abad, Carlos; Florek, Stefan; Becker-Ross, Helmut; Huang, Mao-Dong; Heinrich, Hans-Joachim; Recknagel, Sebastian; Vogl, Jochen; Jakubowski, Norbert; Panne, Ulrich

2017-10-01

Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0 → 0) and (1 → 1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements.

ENAA of iodine in standard reference material lyophilized human urine

International Nuclear Information System (INIS)

Zhang Yongbao; Wang Ke; Wang Ganfeng

1997-01-01

The contents of iodine in two kinds of standard reference materials lyophilized human urine are determined by ENAA. The sensitivity of this method is ten times higher than that of TNAA, and the relative standard deviations of ten measurements are 2.9% and 3.3%, respectively. Two certificated reference samples are used for verification of the analysis. The analytical results are in agreement with the recommended values, and the relative error is less than 3%

Baseline Assessment of 25-Hydroxyvitamin D Reference Material and Proficiency Testing/External Quality Assurance Material Commutability: A Vitamin D Standardization Program Study.

Science.gov (United States)

Phinney, Karen W; Sempos, Christopher T; Tai, Susan S-C; Camara, Johanna E; Wise, Stephen A; Eckfeldt, John H; Hoofnagle, Andrew N; Carter, Graham D; Jones, Julia; Myers, Gary L; Durazo-Arvizu, Ramon; Miller, W Greg; Bachmann, Lorin M; Young, Ian S; Pettit, Juanita; Caldwell, Grahame; Liu, Andrew; Brooks, Stephen P J; Sarafin, Kurtis; Thamm, Michael; Mensink, Gert B M; Busch, Markus; Rabenberg, Martina; Cashman, Kevin D; Kiely, Mairead; Galvin, Karen; Zhang, Joy Y; Kinsella, Michael; Oh, Kyungwon; Lee, Sun-Wha; Jung, Chae L; Cox, Lorna; Goldberg, Gail; Guberg, Kate; Meadows, Sarah; Prentice, Ann; Tian, Lu; Brannon, Patsy M; Lucas, Robyn M; Crump, Peter M; Cavalier, Etienne; Merkel, Joyce; Betz, Joseph M

2017-09-01

The Vitamin D Standardization Program (VDSP) coordinated a study in 2012 to assess the commutability of reference materials and proficiency testing/external quality assurance materials for total 25-hydroxyvitamin D [25(OH)D] in human serum, the primary indicator of vitamin D status. A set of 50 single-donor serum samples as well as 17 reference and proficiency testing/external quality assessment materials were analyzed by participating laboratories that used either immunoassay or LC-MS methods for total 25(OH)D. The commutability test materials included National Institute of Standards and Technology Standard Reference Material 972a Vitamin D Metabolites in Human Serum as well as materials from the College of American Pathologists and the Vitamin D External Quality Assessment Scheme. Study protocols and data analysis procedures were in accordance with Clinical and Laboratory Standards Institute guidelines. The majority of the test materials were found to be commutable with the methods used in this commutability study. These results provide guidance for laboratories needing to choose appropriate reference materials and select proficiency or external quality assessment programs and will serve as a foundation for additional VDSP studies.

Preparation and characterization of a Perna perna (Linnaeus, 1758) mussel reference material

International Nuclear Information System (INIS)

Moreira, Edson Goncalves

2010-01-01

The use of certified reference materials in chemical analysis is an important requirement in quality assurance systems, as it allows the validation of analytical methods and the realization of the metrological traceability of results. Then, it is possible to obtain valid and comparable results not only in space, but also in time. In this study, all the steps for the preparation of a national mussel reference material were attained, from the collection of the bulk material to processing steps such as freeze-drying, grinding, bottling and sterilization. Internationally accepted principles were applied for the homogeneity and stability assessment of the material, using instrumental neutron activation analysis and atomic absorption spectrometry as analytical techniques. By means of a collaborative program with participation of Brazilian and foreign laboratories, the chemical characterization of the material was performed. Element content in the mass percentage to mg kg -1 range was determined for 47 elements and some radionuclides, naturally present in the material. With the application of suitable statistical treatment to the data, it was considered that the content of 11 of those elements may be certified: As, Ca, Cl, Co, K, Mg, Mn, Na, Se, Th and Zn. This study may be considered an important step in the national metrological development, as it shows that the production and characterization of biological reference materials, mussel in particular, is feasible in Brazil, as a tool for quality assurance of environmental and nutritional studies performed in the country. (author)

Evaluation of lead isotope compositions of NIST NBS 981 measured by thermal ionization mass spectrometer and multiple-collector inductively coupled plasma mass spectrometer

Directory of Open Access Journals (Sweden)

Honglin Yuan

2016-09-01

Full Text Available Because Pb isotopes can be used for tracing, they are widely used in many disciplines. The detection and analysis of Pb isotopes of bulk samples are usually conducted using thermal ionization mass spectrometer (TIMS and multiple-collector inductively coupled plasma mass spectrometer (MC-ICP-MS, both of which need external reference materials with known isotopic compositions to correct for the mass discrimination effect produced during analysis. NIST NBS 981 is the most widely used reference material for Pb isotope analysis; however, the isotopic compositions reported by various analytical laboratories, especially those using TIMS, vary from each other. In this study, we statistically evaluated 229 reported TIMS analysis values collected by GeoReM in the last 30 years, 176 reported MC-ICP-MS analysis values, and 938 MC-ICP-MS analysis results from our laboratory in the last five years. After careful investigation, only 40 TIMS results were found to have double or triple spikes. The ratios of the overall weighted averages, 206Pb/204Pb, 207Pb/204Pb, and 208Pb/204Pb, obtained from 40 spiked TIMS reports and 1114 MC-ICP-MS results of NIST NBS 981 isotopes were 16.9406 ± 0.0003 (2s, 15.4957 ± 0.0002 (2s, and 36.7184 ± 0.0007 (2s, respectively.

Use of an excess variance approach for the certification of reference materials by interlaboratory comparison

International Nuclear Information System (INIS)

Crozet, M.; Rigaux, C.; Roudil, D.; Tuffery, B.; Ruas, A.; Desenfant, M.

2014-01-01

In the nuclear field, the accuracy and comparability of analytical results are crucial to insure correct accountancy, good process control and safe operational conditions. All of these require reliable measurements based on reference materials whose certified values must be obtained by robust metrological approaches according to the requirements of ISO guides 34 and 35. The data processing of the characterization step is one of the key steps of a reference material production process. Among several methods, the use of interlaboratory comparison results for reference material certification is very common. The DerSimonian and Laird excess variance approach, described and implemented in this paper, is a simple and efficient method for the data processing of interlaboratory comparison results for reference material certification. By taking into account not only the laboratory uncertainties but also the spread of the individual results into the calculation of the weighted mean, this approach minimizes the risk to get biased certified values in the case where one or several laboratories either underestimate their measurement uncertainties or do not identify all measurement biases. This statistical method has been applied to a new CETAMA plutonium reference material certified by interlaboratory comparison and has been compared to the classical weighted mean approach described in ISO Guide 35. This paper shows the benefits of using an 'excess variance' approach for the certification of reference material by interlaboratory comparison. (authors)

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

International Nuclear Information System (INIS)

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

2002-01-01

analyses are to be used in legal proceedings and prosecutions, and also in investigative research. From the legal perspective, one must assume that any results obtained would be used as evidence in a court of law for prosecution of criminal acts. Consequently, Quality Assurance requirements are very demanding and unforgiving. For example, forensics analysis results that cannot be independently verified against certified reference materials of known composition and isotopics, may not be accepted in a court of law as reliable evidence. Thus, the ability to provide certified and traceable reference materials used in the analyses are extremely important in nuclear forensics. In addition to nuclear signatures, other signatures such as any organics or plant and animal residue that are also on the intercepted materials, become important in identifying the origin of the intercepted nuclear material, and will require traceable, known standards. This paper will describe the quality assurance requirements and considerations that must be adopted and developed for application and use in nuclear forensics. Recommendations and minimum requirements for standardization of a nuclear forensics quality assurance program that could be internationally accepted will also be presented. (author)

Multielement comparison of instrumental neutron activation analysis techniques using reference materials

International Nuclear Information System (INIS)

Ratner, R.T.; Vernetson, W.G.

1995-01-01

Several instrumental neutron activation analysis techniques (parametric, comparative, and k o -standardization) are evaluated using three reference materials. Each technique is applied to National Institute of Standards and Technology standard reference materials, SRM 1577a (Bovine Liver) and SRM 2704 (Buffalo River Sediment), and the United States Geological Survey standard BHVO-1 (Hawaiian Basalt Rock). Identical (but not optimum) irradiation, decay, and counting schemes are employed with each technique to provide a basis for comparison and to determine sensitivities in a routine irradiation scheme. Fifty-one elements are used in this comparison; however, several elements are not detected in the reference materials due to rigid analytical conditions (e.g. insufficient length of irradiation or activity for radioisotope of interest decaying below the lower limit of detection before counting interval). Most elements are normally distributed around certified or consensus values with a standard deviation of 10%. For some elements, discrepancies are observed and discussed. The accuracy, precision, and sensitivity of each technique are discussed by comparing the analytical results to consensus values for the Hawaiian Basalt Rock to demonstrate the diversity of multielement applications. (author) 4 refs.; 2 tabs

Building materials as intrinsic sources of sulphate: A hidden face of salt weathering of historical monuments investigated through multi-isotope tracing (B, O, S)

International Nuclear Information System (INIS)

Kloppmann, W.; Bromblet, P.; Vallet, J.M.; Verges-Belmin, V.; Rolland, O.; Guerrot, C.; Gosselin, C.

2011-01-01

Sulphate neoformation is a major factor of degradation of stone monuments. Boron, sulphur and oxygen isotope signatures were investigated for five French historical monuments (Bourges, Chartres and Marseille cathedrals, Chenonceau castle, and Versailles garden statues) to investigate the role of intrinsic sulphate sources (gypsum plasters and mortars) in stone degradation, compared to the influence of extrinsic sources such as atmospheric pollution. Gypsum plasters and gypsum-containing mortars fall systematically in the δ 34 S and δ 18 O range of Paris Basin Eocene evaporites indicating the origin of the raw materials (so-called 'Paris plaster'). Black crusts show the typical S and O isotope signatures observed elsewhere in Europe that can be attributed to atmospheric pollution, together with a marine component for Marseille. Boron isotopes for black crusts indicate coal combustion as principal boron source. Mortar isotope compositions discriminate three types, one similar to gypsum plasters, one strongly depleted in 34 S, attributed to pyrite oxidation, and a third one close to atmospheric sulphates. The isotopic composition of sulphates and boron of most degraded building stones of the different monuments is well explained by the identified sulphate sources. In several cases (in particular for Chenonceau and Bourges, to some extent for Chartres), the impact of gypsum plaster as building and restoration material on the degradation of the stones in its vicinity was clearly demonstrated. The study illustrates the usefulness of multi-isotope studies to investigate stone degradation factors, as the combination of several isotope systematics increases the discriminatory power of isotope studies with respect to contaminant sources. - Research Highlights: → Insight in stone weathering mechanisms by multi-isotope fingerprinting (B, S, O). → Intrinsic sulphate sources (gypsum plaster, mortar) contribute to stone degradation. → Origin of building materials

Building materials as intrinsic sources of sulphate: A hidden face of salt weathering of historical monuments investigated through multi-isotope tracing (B, O, S)

Energy Technology Data Exchange (ETDEWEB)

Kloppmann, W., E-mail: w.kloppmann@brgm.fr [BRGM, BP 6009, F-45060 Orleans cedex 2 (France); Bromblet, P.; Vallet, J.M. [CICRP, 21, rue Guibal, F-13003 Marseille (France); Verges-Belmin, V. [LRMH, 29, rue de Paris, F-77420 Champs sur Marne (France); Rolland, O. [Independent restorer, 3, rue du Gue, 37270 Montlouis s/Loire (France); Guerrot, C. [BRGM, BP 6009, F-45060 Orleans cedex 2 (France); Gosselin, C. [BRGM, BP 6009, F-45060 Orleans cedex 2 (France); LRMH, 29, rue de Paris, F-77420 Champs sur Marne (France)

2011-04-01

Sulphate neoformation is a major factor of degradation of stone monuments. Boron, sulphur and oxygen isotope signatures were investigated for five French historical monuments (Bourges, Chartres and Marseille cathedrals, Chenonceau castle, and Versailles garden statues) to investigate the role of intrinsic sulphate sources (gypsum plasters and mortars) in stone degradation, compared to the influence of extrinsic sources such as atmospheric pollution. Gypsum plasters and gypsum-containing mortars fall systematically in the {delta}{sup 34}S and {delta}{sup 18}O range of Paris Basin Eocene evaporites indicating the origin of the raw materials (so-called 'Paris plaster'). Black crusts show the typical S and O isotope signatures observed elsewhere in Europe that can be attributed to atmospheric pollution, together with a marine component for Marseille. Boron isotopes for black crusts indicate coal combustion as principal boron source. Mortar isotope compositions discriminate three types, one similar to gypsum plasters, one strongly depleted in {sup 34}S, attributed to pyrite oxidation, and a third one close to atmospheric sulphates. The isotopic composition of sulphates and boron of most degraded building stones of the different monuments is well explained by the identified sulphate sources. In several cases (in particular for Chenonceau and Bourges, to some extent for Chartres), the impact of gypsum plaster as building and restoration material on the degradation of the stones in its vicinity was clearly demonstrated. The study illustrates the usefulness of multi-isotope studies to investigate stone degradation factors, as the combination of several isotope systematics increases the discriminatory power of isotope studies with respect to contaminant sources. - Research Highlights: {yields} Insight in stone weathering mechanisms by multi-isotope fingerprinting (B, S, O). {yields} Intrinsic sulphate sources (gypsum plaster, mortar) contribute to stone degradation

Magnesium Isotopes as a Tracer of Crustal Materials in Volcanic Arc Magmas in the Northern Cascade Arc

Directory of Open Access Journals (Sweden)

Aaron W. Brewer

2018-03-01

Full Text Available Fifteen North Cascade Arc basalts and andesites were analyzed for Mg isotopes to investigate the extent and manner of crustal contributions to this magmatic system. The δ26Mg of these samples vary from within the range of ocean island basalts (the lightest being −0.33 ± 0.07‰ to heavier compositions (as heavy as −0.15 ± 0.06‰. The observed range in chemical and isotopic composition is similar to that of other volcanic arcs that have been assessed to date in the circum-pacific subduction zones and in the Caribbean. The heavy Mg isotope compositions are best explained by assimilation and fractional crystallization within the deep continental crust with a possible minor contribution from the addition of subducting slab-derived fluids to the primitive magma. The bulk mixing of sediment into the primitive magma or mantle source and the partial melting of garnet-rich peridotite are unlikely to have produced the observed range of Mg isotope compositions. The results show that Mg isotopes may be a useful tracer of crustal input into a magma, supplementing traditional methods such as radiogenic isotopic and trace element data, particularly in cases in which a high fraction of crustal material has been added.

Three whole-wood isotopic reference materials, USGS54, USGS55, and USGS56, for δ2H, δ13C, δ15N, and δ18O measurements

Science.gov (United States)

Qi, Haiping; Coplen, Tyler B.; Jordan, James A.

2016-01-01

Comparative measurements of stable hydrogen and oxygen isotopes in wood are hampered by the lack of proper reference materials (RMs). The U.S. Geological Survey (USGS) has prepared three powdered, whole-wood RMs, USGS54 (Pinus contorta, Canadian lodgepole pine), USGS55 (Cordia cf. dodecandra, Mexican ziricote), and USGS56 (Berchemia cf. zeyheri, South African red ivorywood). The stable isotopes of hydrogen, oxygen, carbon, and nitrogen in these RMs span ranges as δ2HVSMOW from –150.4 to –28.2 mUr or ‰, as δ18OVSMOW from + 17.79 to + 27.23 mUr, as δ13CVPDB from –27.13 to –24.34 mUr, and as δ15N AIR-N2 from –2.42 to + 1.8 mUr. These RMs will enable users to normalize measurements of wood samples to isotope–delta scales, and they are intended primarily for the normalization of δ2H and δ18O measurements of unknown wood samples. However, they also are suitable for normalization of stable isotope measurements of carbon and nitrogen in wood samples. In addition, these RMs are suitable for inter-laboratory calibration for the dual-water suilibration procedure for the measurements of δ2HVSMOW values of non-exchangeable hydrogen. The isotopic compositions with 1-σ uncertainties, mass fractions of each element, and fractions of exchangeable hydrogen of these materials are:USGS54 (Pinus contorta, Canadian Lodgepole pine)δ2HVSMOW = –150.4 ± 1.1 mUr (n = 29), hydrogen mass fraction = 6.00 ± 0.04 % (n = 10)Fraction of exchangeable hydrogen = 5.4 ± 0.6 % (n = 29)δ18OVSMOW = + 17.79 ± 0.15 mUr (n = 18), oxygen mass fraction = 40.4 ± 0.2 % (n = 6)δ13CVPDB = –24.43 ± 0.02 mUr (n = 18), carbon mass fraction = 48.3 ± 0.4 % (n = 12)δ15NAIR-N2 = –2.42 ± 0.32 mUr (n = 17), nitrogen mass fraction = 0.05 % (n = 4)USGS55 (Cordia cf. dodecandra, Mexican ziricote)δ2HVSMOW = –28.2 ± 1.7 mUr (n = 30), hydrogen mass fraction = 5.65 ± 0.06 % (n = 10)Fraction of exchangeable

Development of a certified reference materials for composition of citric acid

Directory of Open Access Journals (Sweden)

D. H. Kulev

2014-01-01

Full Text Available The paper presents a summary of analyzing Technical Regulations of the Customs Union TR TC 029/2012 "Safety Requirements for Food Additives, Flavorings and Technological Processing Aids". Information on certified reference materials (RMs for composition of citric acid is provided. Certified characteristics of the RM are, on the one hand, mass fraction of the base substance and, on the other hand, mass fraction of impurities - toxic elements (lead, arsenic, cadmium, mercury. The first batches of the given RMs are produced, which are registered in the State Register of the approved types of certified reference materials GS010300-2013 and GS010143-2012.

Certification measurement of the cadmium, copper and lead contents in rice using isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Vassileva, Emilia; Quetel, Christophe R.

2004-01-01

This paper describes the certification of the Cd, Cu and Pb amount contents in a rice material, that were used as reference values for round 19 of the international measurement evaluation programme (IMEP). The protocol developed in this study was based on isotope dilution associated to inductively coupled plasma mass spectrometry (ID-ICP-MS). A multiple spiking approach was applied to reduce significantly the number of analytical steps. For the decomposition of the sample, three different microwave assisted digestion procedures were tested and compared. The use of hydrofluoric acid was found necessary to ensure full solubilisation and complete isotopic equilibration. Estimation of the combined uncertainty attached to the measurement results was performed according to the ISO guidelines. Contributions from the correction for moisture content, sample homogeneity, procedural blank, spike impurities, spectral interferences, instrumental background and dead-time effects were evaluated. SI-traceable values with less than 2% combined uncertainty (k = 2) were obtained for Cd, Cu and Pb, respectively, (14.39 ± 0.21) x 10 -6 mol kg -1 , (44.31 ± 0.42) x 10 -6 mol kg -1 and (2.034 ± 0.034) x 10 -6 mol kg -1 . The rice powder was observed to be highly hygroscopic and a second series of isotope dilution mass spectrometry measurements was carried out on samples in equilibrium with the ambient moisture conditions ('saturated' samples). The Comite Consultatif pour la Quantite de Matiere (CCQM) requested this approach for the participation to the key comparison 24 on the same rice test material. The excellent agreement for Cd between the IMEP-19 reference value, the value submitted by the institute for reference materials and measurements (IRMM) to CCQM-K24 and the corresponding reference value obtained as the arithmetic mean from the results of the 11 participating National Measurement Institutes (less than 0.27% difference) further validated this work. Eventually, this series

Chemical separation of boron isotopes

Energy Technology Data Exchange (ETDEWEB)

Palko, A.A.

1978-06-01

This is the final report of the research performed at ORNL on the chemical fractionation of boron isotopes between BF/sub 3/ gas and the liquid molecular addition compounds of BF/sub 3/. Thirty compounds were studied, ten of them in detail. Graphs and equations are given for variation of isotopic equilibrium constant, vapor pressure, and BF/sub 3/ solubility as a function of temperature. Rate of isotopic exchange and melting points were determined. Several of the compounds are likely candidates for use in a gas-liquid countercurrent exchange system for large-scale separation of boron isotopes. 23 figs, 53 tables, 39 references.

Chemical separation of boron isotopes

International Nuclear Information System (INIS)

Palko, A.A.

1978-06-01

This is the final report of the research performed at ORNL on the chemical fractionation of boron isotopes between BF 3 gas and the liquid molecular addition compounds of BF 3 . Thirty compounds were studied, ten of them in detail. Graphs and equations are given for variation of isotopic equilibrium constant, vapor pressure, and BF 3 solubility as a function of temperature. Rate of isotopic exchange and melting points were determined. Several of the compounds are likely candidates for use in a gas-liquid countercurrent exchange system for large-scale separation of boron isotopes. 23 figs, 53 tables, 39 references

Proposals for the use of reference materials and for the development of in-house quality control materials for food analysis

International Nuclear Information System (INIS)

Ihnat, Milan

2002-01-01

A summary is presented of factors to be considered in the development of food-based in-house quality control materials to augment available Reference Materials and for frequent, concerted data quality control. Some guidelines are offered regarding approaches to the many considerations required for such an endeavour. Preliminary draft recommendations containing a sequence of steps has been compiled as a starting proposal for a food quality control material development scheme, for a range of natural matrices and measurands. In addition, information on the selection and utilization of Certified Reference Materials and procedures for performance interpretation and corrective action is provided. (author)

An improved reference measurement procedure for triglycerides and total glycerides in human serum by isotope dilution gas chromatography-mass spectrometry.

Science.gov (United States)

Chen, Yizhao; Liu, Qinde; Yong, Sharon; Teo, Hui Ling; Lee, Tong Kooi

2014-01-20

Triglycerides are widely tested in clinical laboratories using enzymatic methods for lipid profiling. As enzymatic methods can be affected by interferences from biological samples, this together with the non-specific nature of triglycerides measurement makes it necessary to verify the accuracy of the test results with a reference measurement procedure. Several such measurement procedures had been published. These procedures generally involved lengthy and laborious sample preparation steps. In this paper, an improved reference measurement procedure for triglycerides and total glycerides was reported which simplifies the sample preparation steps and greatly shortens the time taken. The procedure was based on isotope dilution gas chromatography-mass spectrometry (IDGC-MS)with tripalmitin as the calibration standard. Serum samples were first spiked with isotope-labeled tripalmitin. For the measurement of triglycerides, the serum samples were subjected to lipid extraction followed by separation of triglycerides from diglycerides and monoglycerides. Triglycerides were then hydrolyzed to glycerol, derivatized and injected into the GC–MS for quantification. For the measurement of total glycerides, the serum samples were hydrolyzed directly and derivatized before injection into the GC-MS for quantification. All measurement results showed good precision with CV triglycerides and total glycerides were well within the certified ranges of the CRM, with deviation triglycerides and total glycerides.

Stable oxygen and hydrogen isotopes of brines - comparing isotope ratio mass spectrometry and isotope ratio infrared spectroscopy

Science.gov (United States)

Ahrens, Christian; Koeniger, Paul; van Geldern, Robert; Stadler, Susanne

2013-04-01

Today's standard analytical methods for high precision stable isotope analysis of fluids are gas-water equilibration and high temperature pyrolysis coupled to isotope ratio mass spectrometers (IRMS). In recent years, relatively new laser-based analytical instruments entered the market that are said to allow high isotope precision data on nearly every media. This optical technique is referred to as isotope ratio infrared spectroscopy (IRIS). The objective of this study is to evaluate the capability of this new instrument type for highly saline solutions and a comparison of the analytical results with traditional IRMS analysis. It has been shown for the equilibration method that the presence of salts influences the measured isotope values depending on the salt concentration (see Lécuyer et al, 2009; Martineau, 2012). This so-called 'isotope salt effect' depends on the salt type and salt concentration. These factors change the activity in the fluid and therefore shift the isotope ratios measured by the equilibration method. Consequently, correction factors have to be applied to these analytical data. Direct conversion techniques like pyrolysis or the new laser instruments allow the measurement of the water molecule from the sample directly and should therefore not suffer from the salt effect, i.e. no corrections of raw values are necessary. However, due to high salt concentrations this might cause technical problems with the analytical hardware and may require labor-intensive sample preparation (e.g. vacuum distillation). This study evaluates the salt isotope effect for the IRMS equilibration technique (Thermo Gasbench II coupled to Delta Plus XP) and the laser-based IRIS instruments with liquid injection (Picarro L2120-i). Synthetic salt solutions (NaCl, KCl, CaCl2, MgCl2, MgSO4, CaSO4) and natural brines collected from the Stassfurt Salt Anticline (Germany; Stadler et al., 2012) were analysed with both techniques. Salt concentrations ranged from seawater salinity

Thermal desorption spectroscopy for investigating hydrogen isotope behavior in materials

International Nuclear Information System (INIS)

Xia Tirui; Yang Hongguang; Zhan Qin; Han Zhibo; He Changshui

2012-01-01

The behavior of hydrogen isotope generated in fusion reactor materials is the key issue for safety and economic operation of fusion reactors and becomes an interesting field. In order to investigate the mechanism of hydrogen isotope such as diffusion, release and retention, a high-sensitivity thermal desorption spectroscopy (TDS) in combination with a quadruple mass spectrometer (QMS) was developed. A major technical breakthrough in ultrahigh vacuum (UHV), low hydrogen background, linear heating and sensitivity calibration of TDS system was made. UHV of l × 10 -7 Pa and low hydrogen background of l × 10 -9 Pa were obtained by combining turbo molecule pump and sputter ion pump. Specimens can be linearly heated up to 1173 K at the rate of 1 to 50 K/min under the MCGS PID software. Sensitivity calibration of the TDS system was accomplished using a special deuterium leak in the detector mode of QMS second electron multiplier. The desorption sensitivity coefficient and the minimum detection limit of deuterium desorption rate are 6.22 × l0 24 s -l · and l.24 × l0 -10 s -1 , respectively. The measurement was also routinely conducted on a specimen of standard, deuterium-containing Zr-4 alloy maintained in the laboratory, so as to validate the TDS method. (authors)

Selected bibliography on deuterium isotope effects and heavy water

International Nuclear Information System (INIS)

Dave, S.M.; Donde, M.M.

1983-01-01

In recent years, there has been a great deal of interest in using deuterium and heavy water not only in nuclear industry but also in various fields of basic as well as applied research in physics, chemistry and biology. As a result, the literature is being enriched with a large number of research papers and technical reports published each year. Thus, to enable the scientists to have an easy reference to these works, an endeavour has been made in this selected bibliography, to enlist the publications related to these fields. Since the interest is concerned mainly with heavy water production processes, deuterium isotope effects etc., several aspects (e.g. nuclear) of deuterium have not been covered here. The material in this bibliography which cites 2388 references has been classified under six broad headings, viz. (1) Production of heavy water, (2) Study of deuterium isotope effects, (3) Analysis and Properties of heavy water, (4) Laser Separation of deuterium, (5) Isotopic exchange reactions, and (6) Miscellaneous. The sources of information used for this compilation are chemical abstracts, nuclear science abstracts, INIS Atomindex and also some scattered search through journals and reports available in the B.A.R.C. library. However, in spite of sincere attempts for a wide coverage, no claim is being made towards the exhaustiveness of this bibliography. (author)

Reexamination of the source material of acid igneous rocks, based on the selected Sr isotopic data

International Nuclear Information System (INIS)

Kagami, Hiroo; Shuto, Kenji; Gorai, Masao

1975-01-01

The relation between the ages and the initial strontium isotopic compositions obtained from acid igneous rocks by the whole-rock isochron method is re-examined, on the basis of the selected data. The points based on the data having high values of standard deviation (on the isochrons) show considerable scattering. This is probably ascribed to admixture of sialic materials, or secondary alteration and other geologic causes. The points based on the data having lower values of standard deviation (sigma value: 0.0001 - 0.0019), on the other hand, are evidently plotted within a narrow region just above the presumed Sr evolutional region of the source material of oceanic tholeiites. It is noteworthy that the former region meets the latter region at an earlier stage of the evolutional history of the earth (about 40 x 10 8 yrs. ago or older). It may be conceivable that the former region is the Sr evolutional region of the source material of acid igneous rocks. Considering from the inclination of the above Sr evolutional region, the source material of most of acid igneous rocks may possibly be a certain basic material, chemically similar to the continental tholeiitic basalts or basaltic andesites. On the other hand, the source material of a few acid igneous rocks with low initial strontium isotopic ratios may be a certain basic material resembling the oceanic tholeiites. Another possibility is that these acid igneous rocks and oceanic tholeiites may have been formed, under different physical conditions, directly from a certain common source material presumably of peridotitic composition. (auth.)

Development of anabolic-androgenic steroids purity certified reference materials for anti-doping.

Science.gov (United States)

Quan, Can; Su, Fuhai; Wang, Haifeng; Li, Hongmei

2011-12-20

The need for certified reference materials (CRM) of anabolic-androgenic steroids reference materials was emphasized by the Beijing 2008 Olympic game as a tool to improve comparability, ensuring accuracy and traceability of analytical results for competing athletes. The China National Institute of Metrology (NIM) responded to the state request by providing seven anabolic-androgenic steroids (AAS) reference materials for Beijing Olympic anti-doping, GBW (E) 100086-GBW (E) 100092. This work describes the production of the series of AAS CRMs, according to ISO Guides 34 and 35 [1,2], which comprises the material processing, homogeneity and stability assessment, CRMs' characterization including moisture content, trace metal content. The AASs' purity values were assigned with collaborative study involved eight laboratories applying high resolution liquid chromatography-diode array detector (HPLC-DAD). Homogeneity of the AAS CRMs were determined by an in-house validated liquid chromatographic methodology. Potential degradation during storage was also investigated and a shelf-life based on this value was established. The certified values of CRMs were 99.76±0.079%, 99.76±0.25%, 99.63±0.09%, 99.67±0.11%, 98.82±0.56%, 96.30±0.39% and 99.71±0.49% (purity±expanded uncertainty with confidence level of 95%) for methyltestosterone, testosterone propionate, nandrolone, nandrolone 17-propionate, boldenone, trenbolone acetate and testosterone respectively. The certified values for all the studied AAS reference materials are traceable to the international system of units (SI). The CRMs developed were applied by 32 laboratory including sports organizations and analytical laboratories during the 2008 Olympic game for anti-doping control. Copyright © 2011 Elsevier Inc. All rights reserved.

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

Indications of a major Neolithic trade route? An archaeometric geochemical and Sr, Pb isotope study on amphibolitic raw material from present day Europe

International Nuclear Information System (INIS)

Christensen, A.-M.; Holm, P.M.; Schuessler, U.; Petrasch, J.

2006-01-01

In order to interpret pre-historic cultural interactions, the provenance of amphibolitic raw material used for flat-axes and adzes in lower to middle Neolithic cultures throughout present day Germany were investigated by elemental and Sr, Pb isotopic methods. Within all settlements studied, a homogeneous actinolite-hornblende schist rock type (AHS) was found to be massively dominating, with a distinct petrography of needle-shaped actinolite interwoven with single larger grains of hornblende along with calcic plagioclase and large amounts of ilmenite. Geochemically, the AHS group is very homogeneous and has a signature of an enriched basaltic precursor with high concentrations of particularly the LIL-elements. The geochemical signature is relatively rare and can not be matched in nearby geological outcrops, wherefore the conclusion of 'imported material' is quickly reached. Strontium and Pb isotopic analyses of the AHS were compared to the isotopic composition of amphibolitic rocks with similar petrography and trace elemental signatures within possible archaeological trade regions. The isotopic data of the archaeological material point roughly to a Proterozoic age of the stone used; an age which can be reasonable matched to a single outcrop situated at Jistebsko within the Czech Republic. This area further shows archaeological traces of prehistoric mining. Based on petrographic, geochemical and isotopic evidence, this area is here presented as the provenance area of the stone raw material, which later spread throughout prehistoric Europe - establishing contact and trade routes between Neolithic cultures

Measurement of polybrominated diphenyl ethers in environmental matrix standard reference materials