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Sample records for pu reference materials

  1. A 244Pu spike reference material CBNM IRM-042A

    International Nuclear Information System (INIS)

    Verbruggen, A.; Gallet, M.; Hendrickx, F.; Bievre, P. de

    1991-01-01

    An highly enriched 244 Pu isotopic reference material (CBNM IRM-042a) has been prepared and certified for 244 Pu isotope concentration. The certified value of (2.257 7 ± 0.004 4).10 18 atoms 242 Pu.kg -1 of solution has been established by isotope dilution mass spectrometry. The plutonium isotopic composition has been determined by thermal ionization mass spectrometry and calibration of these measurements by means of synthetic 242 Pu/ 239 Pu mixtures. The isotopic reference material is supplied in a sealed glass ampoule containing approximately 10 g of a 5M nitric acid solution at an approximate concentration of 1 μg Pu per g solution. This isotopic reference material is part of a systematic CBNM programme to supply spike isotopic reference materials of various isotopes at different concentrations

  2. 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)

  3. 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)

  4. Preparation and development of new Pu spike isotopic reference materials at IRMM

    Energy Technology Data Exchange (ETDEWEB)

    Jakopic, Rozle; Bauwens, Jeroen; Richter, Stephan; Sturm, Monika; Verbruggen, Andre; Wellum, Roger; Eykens, Roger; Kehoe, Frances; Kuehn, Heinz; Aregbe, Yetunde [Institute for Reference Materials and Measurements (IRMM) Joint Research Centre, European Commission, Geel, (Belgium)

    2011-12-15

    spikes are applied to measure the uranium and plutonium content of dissolved fuel solutions using IDMS. They are prepared by IRMM to fulfil the existing requirements for reliable spike IRMs in fissile material control from European Safeguards authorities and customers from industry. IRMM-046b, a mixed uranium-plutonium spike IRM of highly enriched {sup 233}U and {sup 242}Pu that dates from 1995, was re-certified for isotope amount content and isotopic composition, each with considerably smaller combined uncertainties. IRMM-046c, a new mixed uranium-plutonium spike, and IRMM-049d, a highly enriched {sup 242}Pu spike, have been prepared. IRMM-049d was prepared from the same stock solution as its predecessor IRMM-049c, dating from 1996, but the new 242Pu spike has certified values with smaller combined uncertainties. The traceability of the certified values to the SI is established through an unbroken chain of comparisons, all having stated uncertainties. IRMM is also co-operating with the Institute for Transuranium Elements (EC-JRC-ITU) in a feasibility study on the development of Pu reference materials for 'age dating' in nuclear forensics. In the course of this work, the reference materials NBS SRM 946, 947 and 948 (NBL CRM 136, 137 and 138) will be investigated among others.

  5. 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

  6. 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.)

  7. 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

  8. 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

  9. 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)

  10. 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.

  11. 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

  12. A certified reference material for radionuclides in the water sample from Irish Sea (IAEA-443)

    DEFF Research Database (Denmark)

    Pham, M.K.; Betti, M.; Povinec, P.P.

    2011-01-01

    A new certified reference material (CRM) for radionuclides in sea water from the Irish sea (IAEA-443) is described and the results of the certification process are presented. Ten radionuclides (3H, 40K, 90Sr, 137Cs, 234U, 235U, 238U, 238Pu, 239+240Pu and 241Am) have been certified, and information...... values on massic activities with 95% confidence intervals are given for four radionuclides (230Th, 232Th, 239Pu and 240Pu). Results for less frequently reported radionuclides (99Tc, 228Th, 237Np and 241Pu) are also reported. The CRM can be used for quality assurance/quality control of the analysis...

  13. 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

  14. Stabilizing And Packaging Pu Materials Per 3013 At SRS

    International Nuclear Information System (INIS)

    STEVE, HENSEL

    2005-01-01

    The Savannah River Site (SRS) began packaging Pu metals into 3013 containers in April, 2003 and oxides in October, 2003. A total of 919 outer 3013 containers were made in the FB-Line at SRS when stabilization and packaging was completed in January, 2005. Experiences, lessons learned, and an overview of packaging activities are presented

  15. Methodologies to determine the Pu content of spent fuel assemblies for input nuclear material accountancy of pyroporcessing

    International Nuclear Information System (INIS)

    Lee, Taehoon; Shin, Heesung; Kim, Youngsoo; Kim, Hodong; Kwon, Taeje

    2011-01-01

    This study shows two different non-destructive approaches to determine the Pu mass of spent fuel assemblies, and the analysis results on the errors in their Pu mass. For both methods, the Cm mass of the assembly is obtained based on the neutron measurement results. The Cm ratio of the assembly is determined from the Cm mass and the Pu mass obtained by using either of the two methods. In a comparison of two methods, the second method is simpler than the first and may not need a homogeneously-mixed sample of the spent fuel assembly. On the other hand, the second approach shows larger error in the estimated Pu mass than the first one for many different spent fuel cases of various burnup, initial enrichment, and cooling times. A member state support program for the development of the IAEA safeguards approach for an engineering-scale pyroprocessing facility, which is designated as the Reference Engineering-scale Pyroprocessing Facility(REPF), has been carried out by Korea Atomic Energy Research Institute since 2008. The nuclear material accountancy of the REPF is based on the 'Cm balance' technique. The Pu content of processing materials of pyroprocessing can be determined by measuring the Cm mass of the materials and multiplying it by the Cm ratio. The spent fuel assembly is de-cladded, and the irradiated UO 2 material of the assembly is homogeneously mixed in the homogenization process in order to obtain a representative sample of the spent fuel assembly for determining the mass of Pu, U and Cm elements, as well as the Cm ratio of the campaign. The shipper-receiver difference between the nuclear power plant and HPC of REPF is determined at this point. We found that the error for the Pu mass and Cm ratio determined from the homogenized uranium oxide powder is the most critical for the determination of the material unaccounted for throughout the whole processes. This paper presents two approaches to determine the Pu mass of spent fuel assemblies using non

  16. 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...

  17. Certified Reference Material IAEA-446 for radionuclides in Baltic Sea seaweed

    DEFF Research Database (Denmark)

    Pham, M.K.; Benmansour, M.; Carvalho, F.P.

    2014-01-01

    A Certified Reference Material (CRM) for radionuclides in seaweed (Fucus vesiculosus) from the Baltic Sea (IAEA-446) is described and the results of the certification process are presented. The 40K, 137Cs, 234U and 239þ240Pu radionuclides were certified for this material, and information values...... for 12 other radionuclides (90Sr, 99Tc, 210Pb (210Po), 226Ra, 228Ra, 228Th, 230Th, 232Th, 235U, 238U, 239Pu and 240Pu) are presented. The CRM can be used for Quality Assurance/Quality Control of analysis of radionuclides in seaweed and other biota samples, as well as for development and validation...

  18. Safety Analysis Report: Packages, Pu oxide and Am oxide shipping cask: Packaging of fissile and other radioactive materials: Final report

    International Nuclear Information System (INIS)

    Chalfant, G.G.

    1984-12-01

    The PuO 2 cask or 5320-3 cask is designed for shipment of americium or plutonium by surface transportation modes. The cask design was physically tested to demonstrate that it met the criteria specified in US ERDA Manual Chapter 0529, dated 12/21/76, which invokes Title 10 Code of Federal Regulations, Part 71 (10 CFR 71) ''Packaging of Radioactive Materials for Transport,'' and Title 49 CFR Parts 171.179 ''Hazardous Materials Regulations.'' (US DOE Order 4580.1A, Chapter III, superseded manual chapter 0529 effective May 1981, but it retained the same 10 CFR 71 and 49 CFR 171-179 references

  19. 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

  20. Determination of {sup 240}Pu/{sup 239}Pu ratio and its significance in environmental studies

    Energy Technology Data Exchange (ETDEWEB)

    Muramatsu, Yasuyuki [National Inst. of Radiological Sciences, Chiba (Japan)

    1999-03-01

    Analytical procedures for the determination of Pu concentrations and its isotopic ratios in environmental samples were developed by using ICP-MS. Detection limit of Pu by ICP-MS was about 0.02 pg ml{sup -1} (0.05 mBq ml{sup -1} for {sup 239}Pu; 0.17 mBq ml{sup -1} for {sup 240}Pu) in the sample solution. Analytical results of {sup 239+240}Pu in IAEA standard reference materials indicated that the accuracy of this method was satisfactory. Data on the {sup 240}Pu/{sup 239}Pu atom ratios, which are rare in the literature, were also obtained for soil and sediment samples (including IAEA standard reference materials) from different areas such as Irish Sea, Mururoa Atoll, Marshall Islands, Chernobyl, Kyshtym, Nagasaki and some other places in Japan. The range of the {sup 240}Pu/{sup 239}Pu ratios was about 0.04-0.4, and the ratios are depending on the origin of the materials. Analytical results for the {sup 240}Pu/{sup 239}Pu atom ratios provide information about the source of the contamination and the transfer of plutonium in the environment. (author)

  1. 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.)

  2. Certified reference material for radionuclides in fish flesh sample IAEA-414 (mixed fish from the Irish Sea and North Sea)

    International Nuclear Information System (INIS)

    Pham, M.K.; Sanchez-Cabeza, J.A.; Povinec, P.P.; Arnold, D.; Benmansour, M.; Bojanowski, R.; Carvalho, F.P.; Kim, C.K.; Esposito, M.; Gastaud, J.; Gasco, C.L.; Ham, G.J.; Hegde, A.G.; Holm, E.; Jaskierowicz, D.; Kanisch, G.; Llaurado, M.; La Rosa, J.; Lee, S.-H.; Liong Wee Kwong, L.; Le Petit, G.; Maruo, Y.; Nielsen, S.P.; Oh, J.-S.; Oregioni, B.; Palomares, J.; Pettersson, H.B.L.; Rulik, P.; Ryan, T.P.; Sato, K.; Schikowski, J.; Skwarzec, B.; Smedley, P.A.; Tarjan, S.; Vajda, N.; Wyse, E.

    2006-01-01

    A certified reference material (CRM) for radionuclides in fish sample IAEA-414 (mixed fish from the Irish Sea and North Seas) is described and the results of the certification process are presented. Nine radionuclides ( 4 K, 137 Cs, 232 Th, 234 U, 235 U, 238 U, 238 Pu, 239+24 Pu and 241 Am) were certified for this material. Information on massic activities with 95% confidence intervals is given for six other radionuclides ( 9 Sr, 21 Pb( 21 Po), 226 Ra, 239 Pu, 24 Pu 241 Pu). Less frequently reported radionuclides ( 99 Tc, 129 I, 228 Th, 23 Th and 237 Np) and information on some activity and mass ratios are also included. The CRM can be used for quality assurance/quality control of the analysis of radionuclides in fish sample, for the development and validation of analytical methods and for training purposes. The material is available from IAEA, Vienna, in 100 g units

  3. 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.)

  4. Reference materials and measurement traceability

    International Nuclear Information System (INIS)

    Bingham, C.D.

    1980-01-01

    Nuclear materials safeguards within the U.S.A. are accomplished by the integration of activities involving physical protection, material control and material accountability. Material accountability requires both sound measurement technology and well-defined accounting procedures to provide final evidence that physical protection and materials control have achieved their purpose. 5 refs

  5. Production of Working Reference Materials for the Capability Evaluation Project

    Energy Technology Data Exchange (ETDEWEB)

    Phillip D. Noll, Jr.; Robert S. Marshall

    1999-03-01

    Nondestructive waste assay (NDA) methods are employed to determine the mass and activity of waste-entrained radionuclides as part of the National TRU (Trans-Uranic) Waste Characterization Program. In support of this program the Idaho National Engineering and Environmental Laboratory Mixed Waste Focus Area developed a plan to acquire capability/performance data on systems proposed for NDA purposes. The Capability Evaluation Project (CEP) was designed to evaluate the NDA systems of commercial contractors by subjecting all participants to identical tests involving 55 gallon drum surrogates containing known quantities and distributions of radioactive materials in the form of sealed-source standards, referred to as working reference materials (WRMs). Although numerous Pu WRMs already exist, the CEP WRM set allows for the evaluation of the capability and performance of systems with respect to waste types/configurations which contain increased amounts of {sup 241}Am relative to weapons grade Pu, waste that is dominantly {sup 241}Am, as well as wastes containing various proportions of depleted uranium. The CEP WRMs consist of a special mixture of PuO{sub 2}/AmO{sub 2} (IAP) and diatomaceous earth (DE) or depleted uranium (DU) oxide and DE and were fabricated at Los Alamos National Laboratory. The IAP WRMS are contained inside a pair of welded inner and outer stainless steel containers. The DU WRMs are singly contained within a stainless steel container equivalent to the outer container of the IAP standards. This report gives a general overview and discussion relating to the production and certification of the CEP WRMs.

  6. 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

  7. 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)

  8. 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)

  9. Certified reference materials for radionuclides in Bikini Atoll sediment (IAEA-410) and Pacific Ocean sediment (IAEA-412)

    DEFF Research Database (Denmark)

    Pham, M. K.; van Beek, P.; Carvalho, F. P.

    2016-01-01

    The preparation and characterization of certified reference materials (CRMs) for radionuclide content in sediments collected offshore of Bikini Atoll (IAEA-410) and in the open northwest Pacific Ocean (IAEA-412) are described and the results of the certification process are presented. The certified...... radionuclides include: 40K, 210Pb (210Po), 226Ra, 228Ra, 228Th, 232Th, 234U, 238U, 239Pu, 239+240Pu and 241Am for IAEA-410 and 40K, 137Cs, 210Pb (210Po), 226Ra, 228Ra, 228Th, 232Th, 235U, 238U, 239Pu, 240Pu and 239+240Pu for IAEA-412. The CRMs can be used for quality assurance and quality control purposes...

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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)

  15. 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.

  16. 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.

  17. The diffusion coefficient for 239Pu, 241Am, 99Tc and 137Cs in highly compacted buffer materials

    International Nuclear Information System (INIS)

    Zhou Kanghan; Li Guoding

    1998-01-01

    Based on one-dimension diffusion model, the diffusion coefficients of Pu, Am, Tc and Cs in highly compacted sodium-bentonite generally used as buffer materials in geologic disposal system for high-level radioactive waste have been determined at room temperature in the atmosphere of nitrogen. The results show that the diffusion coefficients of Am, Pu and Tc and about 10 -13 ∼10 -15 m 2 /s, and that of Cs about 10 -12 m 2 /s. The diffusion coefficients of these elements decrease with the increasing of the dry density of buffer materials. From the relationship of diffusion coefficient, retardation coefficient and dry density of bentonite, it has been concluded that Am and Pu transfer predominately by diffusion in solid phase, however, Cs and Tc by diffusion in pore water

  18. 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

  19. 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).

  20. Safety analysis report: packages 238Pu oxide shipping cask (packaging of fissile and other radioactive materials). Final report

    International Nuclear Information System (INIS)

    Evans, J.E.; Gates, A.A.

    1975-06-01

    Plutonium-238 (as PuO 2 powder) is shipped in triple-container stainless steel shipping casks in compliance with ERDA Manual Chapter 0529 (ERDAM 0529), Safety Standards for the Packaging of Fissile and Other Radioactive Materials. (U.S.)

  1. Safety analysis report: packages. Pu oxide and Am oxide shipping cask (Packaging of fissile and other radioactive materials). Final report

    International Nuclear Information System (INIS)

    Chalfant, G.G.

    1980-05-01

    The PuO 2 cask or SP 5320-2 and 3 cask is designed for surface shipment of americium or plutonium. The cask design was physically tested to demonstrate that it met the criteria specified in US ERDA Manual Chapter 0529, and Chapter I, Interstate Commerce Commission. The package has been assessed for transport of up to 357 grams of plutonium (403 grams PuO 2 powder) and up to 176 grams of americium (200 grams AmO 2 powder), having a maximum decay heat of 203 watts. Criticality evaluation alone would allow the shipment as Fissile Class II but the radiation level of the cask, measured at the time of shipment, may exceed 50 mrem/h at the surface and require shipment as Fissile Class III. Sample calculations address only the more restrictive of the two materials, which in most cases is 238 PuO 2

  2. 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

  3. 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)

  4. 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

  5. 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

  6. Certified reference material for radionuclides in fish flesh sample IAEA-414 (mixed fish from the Irish Sea and North Sea)

    DEFF Research Database (Denmark)

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

    2006-01-01

    A certified reference material (CRM) for radionuclides in fish sample IAEA-414 (mixed fish from the Irish Sea and North Seas) is described and the results of the certification process are presented. Nine radionuclides (K-40, Cs-137, Th-232, U-234, U-235, U-238, Pu-238, Pu239+240 and Am-241) were...... ratios are also included. The CRM can be used for quality assurance/quality control of the analysis of radionuclides in fish sample, for the development and validation of analytical methods and for training purposes. The material is available from IAEA, Vienna, in 100 g units. (c) 2006 Elsevier Ltd. All...

  7. 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

  8. Isotope ratios of 240Pu/239Pu in soil samples from different areas

    International Nuclear Information System (INIS)

    Muramatsu, Yasuyuki; Yoshida, Satoshi; Yamazaki, Shinnosuke

    2003-01-01

    Plutonium concentrations and 240 Pu/ 239 Pu atom ratios in soil samples from Japan and other areas in the world (including IAEA standard reference materials) were determined by ICP-MS. The range of 240 Pu/ 239 Pu atom ratios observed in 21 Japanese soil samples was 0.155 - 0.194 and the average was 0.180 ± 0.011, which is comparable to the global fallout value. A low ratio of about 0.05, which is derived from Pu-bomb, was found in samples from Nishiyama (Nagasaki) and Mururoa Atoll (IAEA-368), while a high ratio of about 0.31 was found in a sample from Bikini Atoll (Marshall Islands). The ratio for Irish Sea sediment (IAEA-135) was 0.21, which was higher than the global fallout value, suggesting the influence by the contamination from the Sellafield facility. The 240 Pu/ 239 Pu atom ratios in soils from the Chernobyl area were determined, and the ratio was found to be very high (about 0.4), indicating the high burn-up grade of the reactor fuel. These results show that the 240 Pu/ 239 Pu ratio can be used as a finger print to identify the source of the contamination. (author)

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

    International Nuclear Information System (INIS)

    El-Mongy, S.A.

    2000-01-01

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

  10. 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. ...

  11. 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

  12. 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.

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. The NIST natural-matrix radionuclide standard reference material program for ocean studies

    International Nuclear Information System (INIS)

    Inn, K.G.W.; Zhichao Lin; Zhongyu Wu; MacMahon, C.; Filliben, J.J.; Krey, P.; Feiner, M.; Harvey, J.

    2001-01-01

    In 1997, the Low-level Working Group of the International Committee on Radionuclide Metrology met in Boston, MA (USA) to define the characteristics of a new set of environmental radioactivity reference materials. These reference materials were to provide the radiochemist with the same analytical challenges faced when assaying environmental samples. It was decided that radionuclide bearing natural materials should be collected from sites where there had been sufficient time for natural processes to redistribute the various chemically different species of the radionuclides. Over the succeeding years, the National Institute of Standards and Technology (NIST), in cooperation with other highly experienced laboratories, certified and issued a number of these as low-level radioactivity Standard Reference Materials (SRMs) for fission and activation product and actinide concentrations. The experience of certifying these SRMs has given NIST the opportunity to compare radioanalytical methods and learn of their limitations. NIST convened an international workshop in 1994 to define the natural-matrix radionuclide SRM needs for ocean studies. The highest priorities proposed at the workshop were for sediment, shellfish, seaweed, fish flesh and water matrix SRMs certified for mBq per sample concentrations of 90 Sr, 137 Cs and 239 Pu + 240 Pu. The most recent low-level environmental radionuclide SRM issued by NIST, Ocean Sediment (SRM 4357) has certified and uncertified values for the following 22 radionuclides: 40 K, 90 Sr, 129 I, 137 Cs, 155 Eu, 210 Pb, 210 Po, 212 Pb, 214 Bi, 226 Ra, 228 Ra, 228 Th, 230 Th, 232 Th, 234 U, 235 U, 237 Np, 238 U, 238 Pu, 239 Pu + 240 Pu, and 241 Am. The uncertainties for a number of the certified radionuclides are non-symmetrical and relatively large because of the non-normal distribution of reported values. NIST is continuing its efforts to provide the ocean studies community with additional natural matrix radionuclide SRMs. The freeze

  18. Characterizing fallout material using Cs and Pu atom ratios in environmental samples from the FDNPP fallout zone

    Science.gov (United States)

    Richards, David; Dunne, James; Martin, Peter; Scott, Tom; Yamashiki, Yosuke; Coath, Chris; Chen, Hart

    2017-04-01

    Here we report the use of combined of Cs and Pu isotope measurements to investigate the extensive plumes of radioactive fallout from the disaster at Fukishima Daiichi nuclear power plant (FNDPP) in March 2011. Among the aims of our study are improved assessment of the physico-chemical nature and changing distribution of land-based fallout. 135Cs/137Cs and 134Cs/137Cs atom ratios are indicative of conditions that relate to the nuclear fission reactions responsible for producing the respective radiocaesium isotopes, and offer much more in terms of forensic and chronological analysis than monitoring 137Cs alone. We briefly present methods to quantify the atom ratios of Cs and Pu isotopes in soil, lichen and moss samples from FDNPP catchment using mass spectrometry (ThermoTRITON for Cs and ThermoNEPTUNE for Pu). High precision data from Fukushima are presented (e.g decay corrected 135Cs/137Cs atom ratio = 0.384 ± 0.001 (n = 5) for roadside dust from Iitate region), and these are in agreement with prelimary estimates by others. We also confirm results for IAEA-330, a spinach sample collected from Polesskoe, Ukraine and subject to contamination from the Chernobyl accident. In addition to Cs isotopes, we adopt Pu isotopes to add a further dimension to the forensic analysis. We discuss the corrections required for background levels prior to the disaster, possibility for multiple components of fallout and complicating factors associated with remobilisation during the clean-up operation. In parallel with this work on digests and leaches from bulk environmental samples, we are refining methods for particle identification, isolation and characterisation using a complementary sequence of cutting-edge materials and manipulation techniques, including combined electron microscopy, focused ion beam techniques (Dualbeam), nano/micro manipulators and nano-scale imaging x-ray photoelectron spectroscopy (NanoESCA) and microCT.

  19. 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

  20. [The molecular composition and spectral properties of polysaccharide isolated from pu-erh tea and its material].

    Science.gov (United States)

    Gong, Jia-shun; Hu, Xiao-jing; Peng, Chun-xiu; Zhou, Hong-jie

    2010-07-01

    Pu-erh tea, a kind of well-known tea from the ancient time, is originally produced in the Yunnan Lanchan River basin through a special solid state fermentation by fungi. It uses sun-dried green tea as its starting materials. To investigate the variation of composition and spectral properties of polysaccharide during solid state fermentation of pu-erh tea by using Saccharomyces cerevisiae as preponderant starter and using sun-dried green tea as materials in the present study. The results showed that the content of water soluble polysaccharide was increased, and the activity of hydrolase such as cellulase, pectinase and glucomylase were also enhanced. The content of neutral sugar increased with the ferment time increasing and the M(w) of raw polysaccharide showed significant difference during fermentation. The main polysaccharide TPS2 and TPS1 were isolated and purified from pu-erh tea and its materials by DEAE-52 and Sephadex G-150 column chromatography. TPS2 contains the higher content of uronic acid, but TPS1 contains the higher contents of neutral sugar and protein. Monosaccharide analysis by GC-MS revealed that TPS1 and TPS2 were composed of arabinose, galactose, glucose, rhamnose, xylose and mannose with molar ratios of 24.2 : 23.6 : 5.9 : 3.2 : 1.8 : 1.1 and 19.3 : 26.9 : 3.2 : 2.7 : 1.3 : 5.5, respectively. The average molecular weight of TPS1 and TPS2 was 1.68 x 10(4) and 1.21 x 10(4) Daltons, respectively. UV scanning spectrum showed that TPS1 and TPS2 had no characteristic absorption between 200 and 400 nm wavelength, it suggested that they contain trace protein. IR spectrum of TPS1 and TPS2 demonstrated that pyranoid rings were contained in them. As shown in the image of atomic force microscope, the molecular appearance of TPS1 and TPS2 resembled islands and apparently consisted of conglomerations. The height of conglomerations of TPS2 was about 40 nm and the length or width was 0.5-0.8 microm, while the height of conglomerations of TPS1 was about 4nm and

  1. Pu-239 and Pu-240 inventories and Pu-240/ Pu-239 atom ratios in the water column off Sanriku, Japan.

    Science.gov (United States)

    Yamada, Masatoshi; Zheng, Jian; Aono, Tatsuo

    2013-04-01

    A magnitude 9.0 earthquake and subsequent tsunami occurred in the Pacific Ocean off northern Honshu, Japan, on 11 March 2011 which caused severe damage to the Fukushima Dai-ichi Nuclear Power Plant. This accident has resulted in a substantial release of radioactive materials to the atmosphere and ocean, and has caused extensive contamination of the environment. However, no information is available on the amounts of radionuclides such as Pu isotopes released into the ocean at this time. Investigating the background baseline concentration and atom ratio of Pu isotopes in seawater is important for assessment of the possible contamination in the marine environment. Pu-239 (half-life: 24,100 years), Pu-240 (half-life: 6,560 years) and Pu-241 (half-life: 14.325 years) mainly have been released into the environment as the result of atmospheric nuclear weapons testing. The atom ratio of Pu-240/Pu-239 is a powerful fingerprint to identify the sources of Pu in the ocean. The Pu-239 and Pu-240 inventories and Pu-240/Pu-239 atom ratios in seawater samples collected in the western North Pacific off Sanriku before the accident at Fukushima Dai-ichi Nuclear Power Plant will provide useful background baseline data for understanding the process controlling Pu transport and for distinguishing additional Pu sources. Seawater samples were collected with acoustically triggered quadruple PVC sampling bottles during the KH-98-3 cruise of the R/V Hakuho-Maru. The Pu-240/Pu-239 atom ratios were measured with a double-focusing SF-ICP-MS, which was equipped with a guard electrode to eliminate secondary discharge in the plasma and to enhance overall sensitivity. The Pu-239 and Pu-240 concentrations were 2.07 and 1.67 mBq/m3 in the surface water, respectively, and increased with depth; a subsurface maximum was identified at 750 m depth, and the concentrations decreased with depth, then increased at the bottom layer. The total Pu-239+240 inventory in the entire water column (depth interval 0

  2. 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

  3. 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

  4. 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)

  5. 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.

  6. 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

  7. 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.

  8. 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

  9. 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

  10. 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

  11. 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

  12. Material control system simulator program reference manual

    Energy Technology Data Exchange (ETDEWEB)

    Hollstien, R.B.

    1978-01-24

    A description is presented of a Material Control System Simulator (MCSS) program for determination of material accounting uncertainty and system response to particular adversary action sequences that constitute plausible material diversion attempts. The program is intended for use in situations where randomness, uncertainty, or interaction of adversary actions and material control system components make it difficult to assess safeguards effectiveness against particular material diversion attempts. Although MCSS may be used independently in the design or analysis of material handling and processing systems, it has been tailored toward the determination of material accountability and the response of material control systems to adversary action sequences.

  13. Material control system simulator program reference manual

    International Nuclear Information System (INIS)

    Hollstien, R.B.

    1978-01-01

    A description is presented of a Material Control System Simulator (MCSS) program for determination of material accounting uncertainty and system response to particular adversary action sequences that constitute plausible material diversion attempts. The program is intended for use in situations where randomness, uncertainty, or interaction of adversary actions and material control system components make it difficult to assess safeguards effectiveness against particular material diversion attempts. Although MCSS may be used independently in the design or analysis of material handling and processing systems, it has been tailored toward the determination of material accountability and the response of material control systems to adversary action sequences

  14. Detection of Pu in Pacific Ocean water with AMS related to the Fukushima accident

    Energy Technology Data Exchange (ETDEWEB)

    Hain, Karin; Faestermann, Thomas; Fimiani, Leticia; Guzman, Jose Manuel; Korschinek, Gunther; Kortmann, Florian; Lierse v Gostomski, Christoph; Ludwig, Peter [TUM (Germany); Golser, Robin; Steier, Peter [Universitaet Wien (Austria); Yamada, Masatoshi [Hirosaki University (Japan)

    2016-07-01

    The concentration of plutonium (Pu) and its isotopic ratios were determined by accelerator mass spectrometry (AMS) in Pacific Ocean water samples. The isotopic ratios {sup 240}Pu/{sup 239}Pu and {sup 241}Pu/{sup 239}Pu can be used to identify a possible release of Pu into the ocean by the Fukushima accident. {sup 241}Pu from fallout of nuclear weapon testings has already significantly decayed. {sup 241}Am, the daughter nuclide of {sup 241}Pu, causes isobaric background on {sup 241}Pu in mass-spectrometric measurements. Therefore, Am and Pu had to be separated chemically using extraction chromatography. The method was verified by analyzing certified reference material. 12 sea water samples, collected at different depths, were prepared at the Radiochemie Muenchen. The concentration of Pu was measured with AMS at the Maier-Leibnitz-Laboratory in Munich and the Vienna Environmental Research Laboratory (VERA). After a short motivation related to the Fukushima accident, the chemical separation method will be presented. Preliminary results of the distribution of Pu in ocean water will be discussed.

  15. Experience of quality control for material accountancy analysis in Pu fuel facility

    International Nuclear Information System (INIS)

    Sumi, Mika; Satoh, Mitsuhiro; Ohnishi, Sumitaka; Suzuki, Toru

    2003-01-01

    Destructive analysis for material accountancy purpose should maintain higher precision referring the International Target Value (ITV). Quality control for the analysis is effective tool to maintain the analytical precision in routine analysis as well as to improve its performance. Since isotope dilution mass spectrometry for the determination of Plutonium and Uranium content and its isotopic composition has launched in the laboratory of Plutonium Fuel Center (PFC) of JNC, comprehensive quality control system has gradually growing up, which currently consists of bias detecting, random error monitoring and human error preventing system. Preventing analysis bias is the most important to maintain long-term performance of measurement. To make bias detecting capability robust, PFC is participating to several intercomparison programs regarding DA samples. Random error monitoring system is another important system to maintain high performance of each routine analysis operation, which composes functions to detect abnormal dispersion of each result and to confirm the state of health of operation of mass spectrometers by measurement of standard materials. To avoid human error during operation process, introduction of computer control system as much extent as possible is practical approach. In this paper, the comprehensive quality control system is introduced and the experiences gained so far are summarized for discussion. (author)

  16. 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)

  17. Determination of 241Pu in nuclear waste slurries: a comparative study using LSC and ICP-MS.

    Science.gov (United States)

    Jäggi, M; Röllin, S; Alvarado, J A Corcho; Eikenberg, J

    2012-02-01

    (241)Pu was determined in slurry samples from a nuclear reactor decommissioning project at the Paul Scherrer Institute (Switzerland). To validate the results, the (241)Pu activities of five samples were determined by LSC (TriCarb and Quantulus) and ICP-MS, with each instrument at a different laboratory. In lack of certified reference materials for (241)Pu, the methods were further validated using the (241)Pu information values of two reference sediments (IAEA-300 and IAEA-384). Excellent agreement with the results was found between LSC and ICP-MS in the nuclear waste slurries and the reference sediments. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. Decontamination of soils and materials containing medium-fired PuO{sub 2} using inhibited fluorides with polymer filtration technology

    Energy Technology Data Exchange (ETDEWEB)

    Temer, D.J.; Villarreal, R.; Smith, B.F. [Los Alamos National Lab., NM (United States)

    1997-10-01

    The decontamination of soils and/or materials from medium-fired plutonium oxide (PuO{sub 2}) with an effective and efficient decontamination agent that will not significantly dissolve the matrix requires a new and innovative technology. After testing several decontamination agents and solutions for dissolution of medium-fired PuO{sub 2}, the most successful decontamination solutions were fluoride compounds, which were effective in breaking the Pu-oxide bond but would not extensively dissolve soil constituents and other materials. The fluoride compounds, tetra fluoboric acid (HBF{sub 4}) and hydrofluorosilicic acid (H{sub 2}F{sub 6}Si), were effective in dissolving medium-fired PuO{sub 2}, and did not seem to have the potential to dissolve the matrix. In both compounds, the fluoride atom is attached to a boron or silicon atom that inhibits the reactivity of the fluoride towards other compounds or materials containing atoms less attracted to the fluoride atom in an acid solution. Because of this inhibition of the reactivity of the fluoride ion, these compounds are termed inhibited fluoride compounds or agents. Both inhibited fluorides studied effectively dissolved medium-fired PuO{sub 2} but exhibited a tendency to not attack stainless steel or soil. The basis for selecting inhibited fluorides was confirmed during leaching tests of medium-fired PuO{sub 2} spiked into soil taken from the Idaho National Engineering Laboratory (INEL). When dissolved in dilute HNO{sub 3}, HCl, or HBr, both inhibited fluoride compounds were effective at solubilizing the medium-fired PuO{sub 2} from spiked INEL soil.

  19. 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

  20. 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

  1. 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

  2. Np Analysis in IAT-Samples Containing <10 Microgram Pu

    International Nuclear Information System (INIS)

    Ludwig, R.; Raab, W.; Dashdondog, J.; Balsley, S.

    2008-01-01

    A method for the determination of neptunium to plutonium in safeguards samples containing less than 10 microgram Pu is presented. The chemical treatment and the optimized measurement conditions for gamma spectrometry are reported. This method is based on thermal ionization mass spectrometry (TIMS) after chemical treatment and separation and was validated with mixtures of U, Pu and Np certified reference materials and using the 237 Np standard addition method, followed by separation of the waste fraction and gamma spectrometric analysis. The highest sensitivity, precision and accuracy in the determination of the Np:Pu ratio at microgram levels of Pu is achieved by evaluating 241 Pu and 233 Pa after measuring the adsorbent with a well-type gamma detector 3 weeks after chemical treatment. The repeatability of determining the Np:Pu ratio is estimated to be 5%, the maximum uncertainty as determined from comparing the 4 measurement modes is within ± 10% for samples containing 3 μg Pu, while being within ± 20% for 0.4 μg Pu. (authors)

  3. Np Analysis in IAT-Samples Containing <10 Microgram Pu

    Energy Technology Data Exchange (ETDEWEB)

    Ludwig, R.; Raab, W.; Dashdondog, J.; Balsley, S. [IAEA, Safeguards Analytical Laboratory, Wagramer Str. 5, P.O. Box 100, A-1400 Vienna (Austria)

    2008-07-01

    A method for the determination of neptunium to plutonium in safeguards samples containing less than 10 microgram Pu is presented. The chemical treatment and the optimized measurement conditions for gamma spectrometry are reported. This method is based on thermal ionization mass spectrometry (TIMS) after chemical treatment and separation and was validated with mixtures of U, Pu and Np certified reference materials and using the {sup 237}Np standard addition method, followed by separation of the waste fraction and gamma spectrometric analysis. The highest sensitivity, precision and accuracy in the determination of the Np:Pu ratio at microgram levels of Pu is achieved by evaluating {sup 241}Pu and {sup 233}Pa after measuring the adsorbent with a well-type gamma detector 3 weeks after chemical treatment. The repeatability of determining the Np:Pu ratio is estimated to be 5%, the maximum uncertainty as determined from comparing the 4 measurement modes is within {+-} 10% for samples containing 3 {mu}g Pu, while being within {+-} 20% for 0.4 {mu}g Pu. (authors)

  4. 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).

  5. 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.

  6. 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.

  7. 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.

  8. 40 CFR 86.1 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... Chromatography, 1994 SAE Handbook—SAE International Cooperative Engineering Program, Volume 1: Materials, Fuels... Method for Analysis of Natural Gas by Gas Chromatography, IBR approved for §§ 86.113-94, 86.513-94, 86...) Gases and Propane Concentrates by Gas Chromatography, IBR approved for §§ 86.113-94, 86.1213-94, 86.1313...

  9. 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

  10. 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)

  11. 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.

  12. 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.

  13. 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)

  14. 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.

  15. 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)

  16. 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

  17. 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 ...

  18. 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

  19. 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

  20. 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

  1. 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)

  2. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

    Science.gov (United States)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

    2014-02-01

    This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation. © 2013 Elsevier B.V. All rights reserved.

  3. 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%.

  4. 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

  5. Analytical method for the determination of Np and Pu in sea water by AMS with respect to the Fukushima accident

    Energy Technology Data Exchange (ETDEWEB)

    Hain, K., E-mail: karin.hain@mytum.de [Physics Department, Technische Universität München, James-Franck-Str.1, 85748 Garching (Germany); Faestermann, T.; Famulok, N.; Fimiani, L.; Gómez-Guzmán, J.M.; Korschinek, G. [Physics Department, Technische Universität München, James-Franck-Str.1, 85748 Garching (Germany); Kortmann, F.; Lierse von Gostomski, Ch. [Radiochemie München, Technische Universität München, Walther-Meißner-Str.3, 85748 Garching (Germany); Ludwig, P. [Physics Department, Technische Universität München, James-Franck-Str.1, 85748 Garching (Germany); Shinonaga, T. [Helmholtz Zentrum München, German Research Center for Environmental Health, Institute of Radiation Protection, Ingolstädter Landstrasse 1, 855764 Neuherberg (Germany)

    2015-10-15

    A chemical separation procedure for plutonium (Pu) and neptunium (Np) was developed using extraction chromatography, mass spectrometry and radiometric analysis to determine their concentrations and isotopic ratios in sea water. {sup 241}Am, which causes isobaric background to {sup 241}Pu in mass spectrometric measurements, was successfully separated from the Pu fraction by this method. Water samples which were spiked with {sup 242}Pu and {sup 237}Np or {sup 239}Np, respectively, were used for chemical yield determination. The chemical yields of Pu and Np, which were determined by alpha and gamma spectrometry at the Radiochemie München (RCM), of more than 85% were obtained. The developed method was applied to analyze the concentration of Pu and Np in the certified reference material, IAEA-443, by Accelerator Mass Spectrometry (AMS) at the Maier–Leibnitz-Laboratory (MLL) to check the applicability of the method to sea water samples. The concentrations of {sup 240}Pu, {sup 241}Pu and {sup 237}Np obtained in this study are in agreement with the certified and literature values within the uncertainties. Due to strong isotopic interference of {sup 239}Pu with {sup 238}U, it was not possible to analyze the concentration of {sup 239}Pu. Some modifications of the chemical separation method to suppress the uranium (U) fraction are under consideration. This method can be used for the analysis of Pu and Np in Pacific Ocean water samples collected after the Fukushima accident.

  6. 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

  7. 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)

  8. Determination of Pu and U by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Muramatsu, Y.; Yoshida, S. [National Inst. of Radiological Sciences, Chiba (Japan)

    2002-06-01

    In order to understand the distribution and behaviour of long-lived radionuclides in the terrestrial environment, we have developed analytical methods for {sup 238}U, {sup 232}Th and {sup 239},{sup 240}Pu and determined them in several environmental samples. ICP-MS was applied to the analyses. Concentrations of {sup 238}U and {sup 232}Th were determined in variety of soils, plants and environmental waters. The mean concentration of U and Th in 77 soils, collected several parts of Japan, were 2.3 and 7.0 ppm (dry wt). Red and yellow soils, which are mainly found in western Japan, have high concentrations of Th, suggesting the contribution from granitic rocks. Higher concentration of U in agricultural soils than forest soils suggested the possible accumulation of this element from phosphate fertilizer. The soil-to-plant transfer factors (concentration ratios between plants and soils) of U and Th were estimated from the analytical results of these nuclides in soils and in several crops. The factors for U were about 0.0005 in leaf vegetables, 0.0002 in root vegetables, 0.0001 in potatoes and 0.00001 in rice (polished). For Th, the factors were about 0.0005 in leaf vegetables, 0.0008 in root vegetables, 0.0005 in potatoes and 0.00003 in rice (polished). For the analysis of plutonium, chromatographic resin, Dowex 1x8, was examined for their applicability in the separation of Pu from the matrix elements. Sufficient decontamination factors (10{sup 4}-10{sup 5}) for many matrix elements including U, which interferes in the detection of mass 239, were obtained in both resins. Analytical results of {sup 239+240}Pu in standard reference materials (IAEA-135, -SOIL-6, -368 and -134) indicated that the accuracy of this method was satisfactory. Data on the {sup 240}Pu/{sup 239}Pu atom ratios in these reference materials, which are rare in the literature, were also obtained. Soil samples from the Marshall Islands showed a large variation of the {sup 240}Pu/{sup 239}Pu atom ratios

  9. Rapid determination of 239Pu in urine samples using molecular recognition technology product AnaLigRPu-02 gel

    International Nuclear Information System (INIS)

    Silvia Dulanska; Boris Remenec; Jan Bilohuscin; Miroslav Labaska; Bianka Horvathova; Andrej Matel

    2013-01-01

    This paper describes the use of IBC's AnaLig R Pu-02 molecular recognition technology product to effectively and selectively pre-concentrate, separate and recover plutonium from urine samples. This method uses two-stage column separations consisting of two different commercial products, Eichrom's Pre-filter Material and AnaLig R Pu-02 resin from IBC Advanced Technologies. By eliminating the co-precipitation techniques and the ashing steps to remove residual organics, the analysis time was reduced significantly. The method was successfully tested by adding known activities of reference solutions of 242 Pu and 239 Pu to urine samples. (author)

  10. 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

  11. 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)

  12. The field migration tests of 237Np, 238Pu, 241Am and 90Sr in aerated loess, aquifer and engineering barrier materials

    International Nuclear Information System (INIS)

    Li Shushen; Wang Zhiming; Zhao Yingjie; Fan Zhiwen; Liu Chunli; An Yongfeng; Yang Yue'e; Wu Qinghua

    2003-01-01

    This paper introduces the field migration tests of 237 Np, 238 Pu, 241 Am and 90 Sr in aerated loess, aquifer and engineering barrier materials. The tests in the aerated loess and engineering barrier materials were carried out under both natural and artificial sprinkling (15 mm/d) conditions. The tests in aquifer were carried out in both assemblies packed with undisturbed aquifer media and a definite undisturbed area. The results indicate that after 3 years tests no significant migrations were seen for all nuclides in engineering barrier materials under two kinds of conditions and in aerated loess under natural conditions. For the aerated loess under artificial sprinkling conditions, 2.7 cm (center of mass) migration in the area directly below the sand tracer layer (named as area 1) and 13 cm (peak) migration in the area outside the area 1 for 90 Sr were observed; There was no migration for 237 Np, 238 Pu and 241 Am. It was discovered that the sand layer used as carrier of nuclide tracer has barrier effect on unsaturated water and an influence on nuclide migration. This has been demonstrated by the inter comparison experiment with both sand and loess as tracer carrier. In the tracer tests of undisturbed aquifer area there was no significant migration of 237 Np, 238 Pu, 241 Am and 90 Sr after 1023 days. In the assembly 8 there was no significant migration for 238 Pu and 241 Am and a small backward migration 0.95 cm for 237 Np and 4.7 cm migration (center of mass) for 90 Sr were observed. The tests also indicate that there is no significant difference of nuclide migration in ordinary and degraded cement

  13. 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%

  14. 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

  15. [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%.

  16. 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.

  17. 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)

  18. 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.)

  19. 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)

  20. 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

  1. 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)

  2. Fission track analysis of Pu in small specimens of biological material: Technical progress report, August 1, 1987--July 31, 1988

    International Nuclear Information System (INIS)

    Wrenn, M.E.

    1988-01-01

    The objective of this research is to develop a highly specific and ultrasensitive method capable of detecting 100 aCi/liter of 239 Pu in human urine. The method using neutron induced fission track analysis is to be made free of interference from uranium, the only naturally occurring element with an isotope which fissions with thermal neutrons. A simplified flow diagram for the method is shown in Figure 1. Briefly 239 Pu is coprecipitated quantitatively from urine with rhodozonic acid. The precipitate containing the 239 Pu is dissolved in HCl and is sequentially passed through two ion exchange columns and reduced in volume. The element is then deposited in a circular area on a thick polycarbonate detector and a thinner detector is placed over the circular deposit. The plastic detectors are then irradiated to a high thermal neutron fluence in a research reactor. The detectors are etched in a caustic solution for controlled times and temperatures in order to develop the fission tracks. Images of tracks are formed both on the thin and thick plastic detectors. Total tracks in the thinner detector are measured with a locally developed spark counter and in the thick plastic are measured by counting with a microscope. The results will be made quantitative by constructing a calibration curve for 239 Pu. 3 refs., 9 figs., 3 tabs

  3. 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.

  4. 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

  5. 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

  6. 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

  7. 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...

  8. 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…

  9. 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.)

  10. INAA and flame AAS of various vegetable reference materials

    International Nuclear Information System (INIS)

    Djingova, R.; Arpadjan, S.; Kuleff, I.

    1991-01-01

    INAA and flame AAS have been used for the analysis of a large number of vegetable reference materials. Out of all determined elements (28 by INAA and 11 by AAS) nine are common for both methods (Ca, Cd, Co, Cu, Fe, Mg, Mn, Na, Zn) and for these the possibilities of the two methods have been compared. (orig.)

  11. 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

  12. 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

  13. 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)

  14. 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

  15. Preparation of additional supplies of 244Pu

    International Nuclear Information System (INIS)

    Bigelow, J.E.; Newman, E.; Alexander, C.W.

    1985-01-01

    In the mid-1970s, gram quantities of the man-made isotope 244 Pu were produced in high purity for basic research as a by-product of a program to prepare gram quantities of 252 Cf. Because 244 Pu is not produced in appreciable quantities in standard power reactor fuel, this nuclide has become extremely useful in the application of isotope dilution mass spectrometry (IDMS), a high-precision analytical technique, to problems of plutonium accountability in support of international safeguards agreements. Although only a small amount (a fraction of a microgram) is needed for each analysis, the present supply of certified nuclear reference standard SRM-996 is expected to last only an additional 3 to 5 years. Three options for producing additional supplies of this rare and valuable material were examined. The options encompassed the production of from 1 to 8.5 g during time spans of from 3 to 10 years. Unit costs ranged from $2300 to $7200 per mg of plutonium of >97% 244 Pu. While the paper concludes that the short-term option can be pursued along with further study of the longer-term options, this should not be regarded as an offer or a commitment on the part of the US Department of Energy (USDOE) to furnish the described material

  16. Preparation of additional supplies of 244Pu

    International Nuclear Information System (INIS)

    Bigelow, J.E.; Newman, E.; Alexander, C.W.

    1985-01-01

    In the mid-1970s, gram quantities of the man-made isotope 244 Pu were produced in high purity for basic research as a by-product of a program to prepare gram quantities of 252 Cf. Because 244 Pu is not produced in appreciable quantities in standard power reactor fuel, this nuclide has become extremely useful in the application of isotope dilution mass spectrometry (IDMS), a high-precision analytical technique, to problems of plutonium accountability in support of international safeguards agreements. Although only a small amount (a fraction of a microgram) is needed for each analysis, the present supply of certified nuclear reference standard SRM-996 is expected to last only an additional 3 to 5 years. Three options for producing additional supplies of this rare and valuable material were examined. The options encompassed the production of from 1 to 8.5 g during time spans of from 3 to 10 years. Unit costs ranged from $2300 to $7200 per mg of plutonium of >97% 244 Pu. While the paper concludes that the short-term option can be pursued along with further study of the longer-term options, this should not be regarded as an offer or a commitment on the part of the U.S. Department of Energy (USDOE) to furnish the described material. (author)

  17. Migration of plutonium from freshwater ecosystem at Hanford. [/sup 238/Pu, /sup 239/Pu, /sup 240/Pu

    Energy Technology Data Exchange (ETDEWEB)

    Emery, R. M.; Klopfer, D. C.; McShane, M. C.

    1977-09-01

    A reprocessing waste pond at Hanford has been inventoried to determine quantities of plutonium (Pu) that have been accumulated since its formation in 1944. Expressions of export were developed from these inventory data and from informed assumptions about the vectors which act to mobilize material containing Pu. This 14-acre pond provides a realistic illustration of the mobility of Pu in a lentic ecosystem. The ecological behavior of Pu in this pond is similar to that in other contaminated aquatic systems having widely differing limnological characteristics. Since its creation, this pond has received about one Ci of /sup 239/,/sup 240/Pu and /sup 238/Pu, most of which has been retained by its sediments. Submerged plants, mainly diatoms and Potamogeton, accumulate >95% of the Pu contained in biota. Emergent insects are the only direct biological route of export, mobilizing about 5 x 10/sup 3/ nCi of Pu annually, which is also the estimated maximum quantity of the Pu exported by waterfowl, birds and mammals collectively. There is no apparent significant export by wind, and it is not likely that Pu has migrated to the ground water below U-Pond via percolation. Although this pond has a rapid flushing rate, a eutrophic nutrient supply with a diverse biotic profile, and interacts with an active terrestrial environment, it appears to effectively bind Pu and prevent it from entering pathways to man and other life.

  18. Developing Potential New Reference Materials for Light Isotopes in Foodstuffs

    Science.gov (United States)

    Frew, Russell; Van Hale, Robert; Clarke, Dianne; Abrahim, Aiman; Resch, Christian; Mayr, Leopold; Cannavan, Andrew; Gröning, Manfred

    2013-04-01

    Measurements of subtle variations in stable isotope ratios provide the means for verifying food integrity in numerous ways. Adulterants usually have different isotopic composition so their presence in a food is readily detectable. Stable isotope measurements can also be used to determine the region of production of the food. In most cases the ability of stable isotope measurements to verify, or otherwise reject, the authenticity of the food is greatly enhanced by comparison of a result to a reference database. The more high-quality data in the database, the more statistical power is afforded by the comparison. A serious weakness at present is the lack of reference materials in food matrices available to the community. Thus researchers have to rely on in-house standards for calibration and quality assurance. The result is that there are numerous datasets published that may be internally consistent but it is exceedingly difficult to combine these datasets into a cohesive database. This is particularly important for measurements of the hydrogen isotopes. Here we present a survey of the stable isotope (^2H, ^13C and ^15N) composition of 12 Reference Materials from the International Atomic Energy Agency catalogue. All but one of these materials are plant matter and have been developed as reference materials for other applications such as radionuclide or trace element measurements. Thus they have been verified as suitable materials in terms of stability and homogeneity for those tests. The purpose of this work is to ascertain if they are similarly suitable as stable isotope reference materials. The results from our survey show that there is a wide range in elemental and isotopic composition among these materials. For example, the ^15N values range from-13.5‰ to +18.6‰ and the nitrogen elemental composition range is from 0.7% to 9.7%. The ^13C values range from -20‰ to -40‰ and the carbon elemental composition ranges from 15% to 47%. We are now in the process of

  19. Certification of a uranium dioxide reference material for chemical analyses

    International Nuclear Information System (INIS)

    Le Duigou, Y.

    1984-01-01

    This report, issued by the Central Bureau for Nuclear Measurements (CBNM), describes the characterization of a uranium dioxide reference material with accurately determined uranium mass fraction for chemical analyses. The preparation, conditioning, homogeneity tests and the analyses performed on this material are described in Annex 1. The evaluation of the individual impurity results, total of impurities and uranium mass fraction are given in Annex 2. Information on a direct determination of uranium by titration is given in Annex 3. The uranium mass fraction (881.34+-0.13) g.kg -1 calculated in Annex 2 is given on the certificate

  20. 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)

  1. Radiolysis of Salts and Long-Term Storage Issues for Both Pure and Impure PuO{sub 2} Materials in Plutonium Storage Containers

    Energy Technology Data Exchange (ETDEWEB)

    Lav Tandon

    2000-05-01

    The Material Identification and Surveillance (MIS) project sponsored a literature search on the effects of radiation on salts, with focus on alkali chlorides. The goal of the survey was to provide a basis for estimating the magnitude of {alpha} radiation effects on alkali chlorides that can accompany plutonium oxide (PuO{sub 2}) into storage. Chloride radiolysis can yield potentially corrosive gases in plutonium storage containers that can adversely affect long-term stability. This literature search was primarily done to provide a tutorial on this topic, especially for personnel with nonradiation chemistry backgrounds.

  2. Elaboration and characterisation of plutonium waste reference materials

    International Nuclear Information System (INIS)

    Perolat, J.P.

    1990-01-01

    The Analysis Methods Establishment Commission (CETAMA) has set up a program for the elaboration and characterisation of plutonium waste reference materials. The object of this program is to give laboratories the possibility to test and calibrate apparatus used in non-destructive methods for the analysis of plutonium waste. The different parameters of this program are presented: - characterisation of plutonium, - type and number of containers, - plutonium distribution inside the different containers, - description of the matrix

  3. 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

  4. 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)

  5. 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

  6. Characterization of Ricin and R. communis Agglutinin Reference Materials

    Science.gov (United States)

    Worbs, Sylvia; Skiba, Martin; Söderström, Martin; Rapinoja, Marja-Leena; Zeleny, Reinhard; Russmann, Heiko; Schimmel, Heinz; Vanninen, Paula; Fredriksson, Sten-Åke; Dorner, Brigitte G.

    2015-01-01

    Ricinus communis intoxications have been known for centuries and were attributed to the toxic protein ricin. Due to its toxicity, availability, ease of preparation, and the lack of medical countermeasures, ricin attracted interest as a potential biological warfare agent. While different technologies for ricin analysis have been established, hardly any universally agreed-upon “gold standards” are available. Expert laboratories currently use differently purified in-house materials, making any comparison of accuracy and sensitivity of different methods nearly impossible. Technically challenging is the discrimination of ricin from R. communis agglutinin (RCA120), a less toxic but highly homologous protein also contained in R. communis. Here, we established both highly pure ricin and RCA120 reference materials which were extensively characterized by gel electrophoresis, liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS), and matrix-assisted laser desorption ionization–time of flight approaches as well as immunological and functional techniques. Purity reached >97% for ricin and >99% for RCA120. Different isoforms of ricin and RCA120 were identified unambiguously and distinguished by LC-ESI MS/MS. In terms of function, a real-time cytotoxicity assay showed that ricin is approximately 300-fold more toxic than RCA120. The highly pure ricin and RCA120 reference materials were used to conduct an international proficiency test. PMID:26703723

  7. Characterization of Ricin and R. communis Agglutinin Reference Materials

    Directory of Open Access Journals (Sweden)

    Sylvia Worbs

    2015-11-01

    Full Text Available Ricinus communis intoxications have been known for centuries and were attributed to the toxic protein ricin. Due to its toxicity, availability, ease of preparation, and the lack of medical countermeasures, ricin attracted interest as a potential biological warfare agent. While different technologies for ricin analysis have been established, hardly any universally agreed-upon “gold standards” are available. Expert laboratories currently use differently purified in-house materials, making any comparison of accuracy and sensitivity of different methods nearly impossible. Technically challenging is the discrimination of ricin from R. communis agglutinin (RCA120, a less toxic but highly homologous protein also contained in R. communis. Here, we established both highly pure ricin and RCA120 reference materials which were extensively characterized by gel electrophoresis, liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS, and matrix-assisted laser desorption ionization–time of flight approaches as well as immunological and functional techniques. Purity reached >97% for ricin and >99% for RCA120. Different isoforms of ricin and RCA120 were identified unambiguously and distinguished by LC-ESI MS/MS. In terms of function, a real-time cytotoxicity assay showed that ricin is approximately 300-fold more toxic than RCA120. The highly pure ricin and RCA120 reference materials were used to conduct an international proficiency test.

  8. Neutron activation analysis for certification of standard reference materials

    International Nuclear Information System (INIS)

    Capote Rodriguez, G.; Perez Zayas, G.; Hernandez Rivero, A.; Ribeiro Guevara, S.

    1996-01-01

    Neutron activation analysis is used extensively as one of the analytical techniques in the certification of standard reference materials. Characteristics of neutron activation analysis which make it valuable in this role are: accuracy multielemental capability to asses homogeneity, high sensitivity for many elements, and essentially non-destructive method. This paper report the concentrations of 30 elements (major, minor and trace elements) in four Cuban samples. The samples were irradiated in a thermal neutron flux of 10 12- 10 13 n.cm 2. s -1. The gamma ray spectra were measured by HPGe detectors and were analyzed using ACTAN program development in Center of Applied Studies for Nuclear Development

  9. Reference material for trace analysis by radioanalytical methods: Bowen's Kale

    International Nuclear Information System (INIS)

    Wainerdi, R.E.

    1979-01-01

    A fairly large volume of published data on 'Bowen's Kale' has been examined critically in order to develop recommendations for the use of this preparation as a 'reference material' in the standardisation and evaluation of the reliability of analytical procedures. Values are now recommended for the contents of twelve elements present in major to trace concentrations in 'Bowen's Kale'. 'Indicated values' for another 16 elements are provided. Values for 15 more elements are listed with no recommendation. The criteria adopted in categorising elements into these groups are discussed. (author)

  10. Certification of standard reference materials employing neutron activation analysis

    International Nuclear Information System (INIS)

    Capote Rodriguez, G.; Hernandez Rivero, A.; Molina Insfran, J.; Ribeiro Guevara, S.; Santana Encinosa, C.; Perez Zayas, G.

    1997-01-01

    Neutron activation analysis (Naa) is used extensively as one of the analytical techniques in the certification of standard reference materials (Srm). Characteristics of Naa which make it valuable in this role are: accuracy; multielemental capability; ability to assess homogeneity; high sensitivity for many elements, and essentially non-destructive method. This paper reports the concentrations of thirty elements (major, minor and trace elements) in four Cuban Srm's. The samples were irradiated in a thermal neutron flux of 10 12 -10 13 neutrons.cm -2 .s -1 . The gamma-ray spectra were measured by HPGe detectors and were analysed using ACTAN program, developed in CEADEN. (author) [es

  11. Characterization of the NIST shellfish Standard Reference Material 4358

    International Nuclear Information System (INIS)

    Nour, S.; Inn, K.G.W.; Filliben, J.; Gaast van der, H.; Men, L.C.; Calmet, D.; Altzitzoglou, T.; Povinec, P.; Takata, Y.; Wisdom, M.

    2013-01-01

    A new shellfish Standard Reference Material 4358 was developed by the National Institute of Standards and Technology through an international interlaboratory comparison that involved twelve laboratories-participants from nine countries. The results from the participants were statistically evaluated, and the most robust certified values were based on the median of laboratories’ reported means and the uncertainties derived using the bootstrap method. Massic activity certified values were established for fourteen radionuclides, five activity ratios, and informational massic activity values for eight more radionuclides and two activity ratios. (author)

  12. Japanese tea leaves: a possible biological standard reference material

    International Nuclear Information System (INIS)

    Fuwa, Keiichiro; Notsu, Kenji; Tsunoda, Kin-ichi; Kato, Hideaki; Yamamoto, Yuko.

    1978-01-01

    Japanese Tea Leaves, prepared by pulverizing with an agate ball mill and sieving with a Saran fiber sieve (50 mesh) were assessed as a possible biological standard reference material for elemental analysis. The metal content of the tea leaves was determined independently at two laboratories using atomic absorption and flame emission spectrometry. Neutron activation analysis was also performed to determine the content (21 elements) of Tea Leaves. For some elements the result from the various methods were compared. The characteristics of Tea Leaves are discussed and the elemental composition is compared to that of Orchard Leaves (NBS SRM, 1571). The most significant characteristic of Tea Leaves was the high manganese content. (auth.)

  13. Need for organic reference materials in marine science

    Energy Technology Data Exchange (ETDEWEB)

    Wells, D.E.

    1988-12-01

    The reference materials (RMs) available for organic trace analysis (OTA) and the development programmes of the RM producers are reviewed. The need for a wider range of determinants, matrices and classes of RMs, particularly the more widespread use of laboratory RMs (LRMs) is discussed. Additional certified RMs should include phenolic surfactant degradation products, chlorophenolics from the wood and paper industries, and organobromines from fire retardants. RMs as molecular markers of geogenic, pyrogenic and biogenic sources; chlorophylls and xanthophylls as a measure of marine productivity and natural shellfish toxins are proposed.

  14. 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.)

  15. Preparation, characterization and certification of uranium isotope reference materials

    International Nuclear Information System (INIS)

    Oliveira Junior, Olivio Pereira de

    2006-01-01

    This work describes the preparation, characterization and certification of a set of uranium isotope reference materials ranging from 0.5 to 20.0 % of 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( 235 U)/n( 238 U) was certified in the materials produced to expanded uncertainties ranging from 0.02 to 0.10 % and the ratios n( 234 U)/n( 238 U) and n( 236 U)/n( 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)

  16. Electrodynamics in Arbitrary Reference Frames and in Arbitrary Material Media

    International Nuclear Information System (INIS)

    Horzela, A.; Kapuscik, E.; Widomski, M.

    1999-01-01

    Full text: The investigation of electromagnetic phenomena in material media still belongs to the most difficult tasks of electrodynamics. Complexity and variability of material media practically exclude effective applications of methods and computational techniques elaborated in the framework of standard microscopic electrodynamics with classical vacuum as a ground state. In order to obtain satisfactorily exact descriptions of electromagnetic properties of complex material media one is enforced to use methods and approximations which are difficult to control. Moreover, they usually break covariance properties and the results obtained are valid in one reference frame which choice remains subjective and model dependent. Some time ago we have proposed a reformulation of Maxwell electrodynamics which opens new ways in study of electromagnetic processes in material media. The formalism gets rid of assumptions characteristic for vacuum electrodynamics only and it avoids the usage of constitutive relations as primary relations put on quantities needed for a complete description of an electromagnetic system. Fundamental properties of all electromagnetic quantities are their uniquely defined transformation rules and their analysis allows to determine the possible relations between them. Within such a scheme it is possible to introduce constitutive relations which do not have analogies in macroscopic classical electrodynamics. They may be used in description of microscopic electromagnetic processes in a different way than it is done in the framework of quantum electrodynamics. (author)

  17. Consensus values for NIST biological and environmental Standard Reference Materials

    International Nuclear Information System (INIS)

    Roelandts, I.; Gladney, E.S.

    1998-01-01

    The National Institute of Standards and Technology (NIST, formerly the National Bureau of Standards or NBS) has produced numerous Standard Reference Materials (SRM) for use in biological and environmental analytical chemistry. The value listed on the ''NIST Certificate of Analysis'' is the present best estimate of the ''true'' concentration of that element and is not expected to deviate from that concentration by more than the stated uncertainty. However, NIST does not certify the elemental concentration of every constituent and the number of elements reported in the NIST programs tends to be limited.Numerous analysts have published concentration data on these reference materials. Major journals in analytical chemistry, books, proceedings and ''technical reports'' have been surveyed to collect these available literature values. A standard statistical approach has been employed to evaluate the compiled data. Our methodology has been developed in a series of previous papers. Some subjective criteria are first used to reject aberrant data. Following these eliminations, an initial arithmetic mean and standard deviation (S.D.) are computed from remaining data for each element. All data now outside two S.D. from the initial mean are dropped and a second mean and S.D. recalculated. These final means and associated S.D. are reported as ''consensus values'' in our tables. (orig.)

  18. Reference Material IAEA 434: Naturally Occurring Radionuclides in Phosphogypsum

    International Nuclear Information System (INIS)

    2010-01-01

    Phosphogypsum is generated as a by-product of the phosphoric acid based fertilizer industry. The discharge of phosphogypsum on earth surface deposits is a potential source of enhanced natural radiation and heavy metals, and the resulting environmental impact should be considered carefully to ensure safety and compliance with environmental regulations. In addition, phosphogypsum can be used to make several building materials and it is used in agriculture as a conditioner to maintain soil productivity in areas where soils are poor and erode easily. A reliable determination of naturally occurring radionuclides in phosphogypsum is necessary to comply with the radiation protection and environmental regulations. The IAEA-434 will assist laboratories in the IAEA Member States in validating their analytical methods for the determination of naturally occurring radionuclides in phosphogypsum and to control the quality of the produced analytical results. Reference values for the massic activities and associated standard uncertainties were established for: Pb-210, Ra-226, Th-230, U-234 and U-238. During sample production and certification, the requirements for reference material production and certification as stated in ISO guides 34 and 35 were taken into account. This report summarizes the preparation and certification process

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  20. Criticality Data for Spherical 235U, 239Pu, and 237Np Systems Reflector-Moderated by Low Capturing-Moderator Materials

    International Nuclear Information System (INIS)

    Loaiza, David J.; Stratton, William

    2004-01-01

    The critical dimensions of spherical systems moderated and reflected by low-capturing materials such as D 2 O, BeO, Be, and C were investigated. A parametric study of the critical mass of enriched uranium, plutonium, and neptunium is examined and tabulated. The results obtained expand on the understanding of reflector-moderated critical systems, and they show regions of unstable criticality for 235 U and 239 Pu reflected cores at intermediate densities. This instability is illustrated by calculations of the positive reactivity coefficient of volume expansion. The coefficient is positive, not negative, in the intermediate density region for 235 U and 239 Pu systems. For 237 Np cores reflected by the same moderator, the effect is negligible. The critical dimensions were calculated with the DANTSYS codes using the Hansen-Roach cross-section libraries. This study is both a summary of mostly unpublished calculations and new calculations. Experimental data for these configurations are extremely limited. These are examined in the text when applicable

  1. A comparison of chemical reference materials for solution calorimeters.

    Science.gov (United States)

    Ramos, Rita; Gaisford, Simon; Buckton, Graham; Royall, Paul G; Yff, Barbara T S; O'Neill, Michael A A

    2005-08-11

    Solution calorimeters are based on semi-adiabatic or isothermal heat-conduction principles and differ in the way they record data. They also have different measuring sensitivities and require different quantities of solute and solvent. As such, the choice of chemical test substance is not straightforward. Usually the dilution of KCl is recommended; it is possible to purchase a reference sample of KCl that has a certified enthalpy of solution and this standard material is usually used to test semi-adiabatic instruments. Here, we review the suitability of a range of chemical test substances (KCl, sucrose and Tris) for an isothermal heat-conduction solution calorimeter. It was found that KCl was not the best test material because its relatively high enthalpy of solution (DeltasolH) necessitated the use of small samples (2 mg), resulting in a relatively large standard deviation (sigman-1) in the values recorded (DeltasolH=17.14+/-0.49 kJ mol-1); furthermore, KCl data must be corrected to account for the effect of dilution, although the correction was found to be small (0.07 kJ mol-1) under the experimental conditions employed here. Sucrose appears to be a much more robust test material for isothermal heat-conduction instruments because its lower enthalpy of solution allows the use of much larger samples (20 mg), which minimises experimental errors. The DeltasolH value returned (6.14+/-0.08 kJ mol-1) is in excellent agreement with the literature. It is also cheap, readily available and requires minimal preparation although its widespread use would require the preparation of a certified reference sample.

  2. HANFORD Pu-238 DRUM INTEGRITY ASSESSMENT

    International Nuclear Information System (INIS)

    CANNELL, G.R.

    2004-01-01

    Hanford is presently retrieving contact-handled, transuranic (CH-TRU) waste drums from the site's Low-Level Burial Grounds (LLBG) for processing and disposition. A subgroup of these drums (12 total), referred to as Pu-238 drums, has some unique characteristics that may impact the current drum handling and processing activities. These characteristics include content, shielding, thermal, pressurization and criticality issues. An effort to evaluate these characteristics, for the purpose of developing a specific plan for safe retrieval of the Pu-238 drums, is underway. In addition to the above evaluation, the following integrity assessment of the inner container material and/or confinement properties, with primary emphasis on the Source Capsule (primary confinement barrier) and Shipping Container has been performed. Assessment included review of the inner container materials and the potential impact the service history may have had on material and/or confinement properties. Several environmental degradation mechanisms were considered with the objective of answering the following question: Is it likely the container material and/or confinement properties have been significantly altered as a result of service history?

  3. Anthropogenic Pu distribution in Tropical East Pacific

    International Nuclear Information System (INIS)

    Kinoshita, Norikazu; Sumi, Takahiro; Takimoto, Kiyotaka; Nagaoka, Mika; Yokoyama, Akihiko; Nakanishi, Takashi

    2011-01-01

    The geographical distribution of the anthropogenic radionuclides 238 Pu and 239+240 Pu in the Tropical East Pacific in 2003 was studied from the viewpoint of material migration. We measured the contents of Pu isotopes in seawater and in sediment from the sea bottom. The distributions of Pu isotopes, together with those of coexisting nitrate and phosphate species and dissolved oxygen, are discussed in relation to the potential temperature and potential density (sigma-θ). The Pu contents in sediment samples were compared with those in the seawater. Horizontal migration across the Equator from north to south was investigated at depths down to ∼ 800 m in the eastern Pacific. The Pu distribution at 0-400 m correlated well with the distribution of potential temperature. Maximum Pu levels were observed in the subsurface layer at 600-800 m, corresponding to the depth where sigma-θ ∼ 27.0. It is suggested that the Pu distribution depends on the structure of the water mass and the particular temperature and salinity. The water column/sediment column inventory ratio and the vertical distribution of Pu may reflect the efficiency of scavenging in the relevant water areas. Research Highlights: → Geographical distributions of Pu isotopes were investigated from viewpoint of material migration. → Horizontal migration from north to south was found at depths down to ∼800 m in the eastern Pacific. → Pu distribution at 0-400 m was correlated with water temperature. → The distribution at 600-800 m correlated with water mass structure. → Pu in seawater and sediment gave information about efficiency of scavenging.

  4. 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.

  5. Safety requirements for the Pu carriers

    International Nuclear Information System (INIS)

    Mishima, H.

    1993-01-01

    Ministry of Transport of Japan has now set about studying requirements for Pu carriers to ensure safety. It was first studied what the basic concept of safe carriage of Pu should be, and the basic ideas have been worked out. Next the requirements for the Pu carriers were studied based on the above. There are at present no international requirements of construction and equipment for the nuclear-material carriers, but MOT of Japan has so far required special construction and equipment for the nuclear-material carriers which carry a large amount of radioactive material, such as spent fuel or low level radioactive waste, corresponding to the level of the respective potential hazard. The requirements of construction and equipment of the Pu carriers have been established considering the difference in heat generation between Pu and spent fuel, physical protection, and so forth, in addition to the above basic concept. (J.P.N.)

  6. Scalar material reference systems and loop quantum gravity

    International Nuclear Information System (INIS)

    Giesel, K; Thiemann, T

    2015-01-01

    In the past, the possibility to employ (scalar) material reference systems in order to describe classical and quantum gravity directly in terms of gauge invariant (Dirac) observables has been emphasized frequently. This idea has been picked up more recently in loop quantum gravity with the aim to perform a reduced phase space quantization of the theory, thus possibly avoiding problems with the (Dirac) operator constraint quantization method for a constrained system. In this work, we review the models that have been studied on the classical and/or the quantum level and parametrize the space of theories considered so far. We then describe the quantum theory of a model that, to the best of our knowledge, has only been considered classically so far. This model could arguably be called the optimal one in this class of models considered as it displays the simplest possible true Hamiltonian, while at the same time reducing all constraints of general relativity. (paper)

  7. Iodine in different food articles and standard reference materials

    International Nuclear Information System (INIS)

    Dermelj, M.; Slejkovec, Z.; Byrne, A.R.; Stegnar, P.; Stibilj, V.; Rossbach, M.

    1990-01-01

    The greater part of essential iodine enters living organisms via the food chain. Nevertheless, quantitative data on its concentration in diets, food articles and also in available SRMs are very poor and scarce. This and WHO recommendations on daily allowances of iodine for man via food articles caused an added demand for accurate and reliable determination of iodine in these samples. From this point of view the purpose of the present was to analyse and to establish the concentration levels of total iodine in some food articles, diets, SRMs and candidate reference materials by the use of rapid radiochemical separation, developed in our laboratory. The results were checked by the analysis of SRMs with available certified values for iodine and good agreement is evident. (orig.)

  8. Neutron activation analysis of new botanical reference materials. Pt. 2

    International Nuclear Information System (INIS)

    Kucera, J.; Soukal, L.

    1993-01-01

    The certified, information, and other values of elemental contents were compared with results of neutron activation analysis (NAA) for the new Czechoslovak botanical reference materials (RMs) Green Algae 12-02-02, Lucerne 12-02-03, Wheat Bread Fluor 12-02-04, and Rye Bread Flour 12-02-05. These were prepared by the Institute of Radioecology and Applied Nuclear Techniques (IRANT), Kosice, and statistically evaluated after interlaboratory comparisons. For the majority of elements, a very good agreement was found between the IRANT values and the results of NAA. In several cases, however, significant differences were detected; possible analytical reasons for the differences and the suitability of a purely statistical evaluation of intercomparison results without analytical considerations for RM certification are discussed. (orig.)

  9. Development of the NBS beryllium isotopic standard reference material

    International Nuclear Information System (INIS)

    Inn, K.G.W; Fassett, J.D.; Coursey, B.M.; Walker, R.L.; Raman, S.

    1987-01-01

    The National Bureau of Standards, in conjunction with the Oak Ridge National Laboratory and the Accelerator Mass Spectrometry community, is in the process of developing a beryllium isotopic solution Standard Reference Material. The master 10 Be/ 9 Be solution was characterized isotopically by resonance-ionization and secondary-ion mass-spectrometric-based techniques, and radioactivity measurements were by liquid scintillation counting. The master solution was gravimetrically diluted with 9 Be to a final 10 Be/ 9 Be atomic ratio of 3 x 10 -11 . The preliminary data indicate a half life for 10 Be of 1.3 million years, and AMS measurements are within 10% of the known beryllium isotopic ratio

  10. Bias detection and certified reference materials for random measurands

    Science.gov (United States)

    Rukhin, Andrew L.

    2015-12-01

    A problem that frequently occurs in metrology is the bias checking of data obtained by a laboratory against the specified value and uncertainty estimate given in the certificate of analysis. The measurand—a property of a certified reference material (CRM)—is supposed to be random with a normal distribution whose parameters are given by the certificate specifications. The laboratory’s data from subsequent measurements of the CRM (a CRM experiment) are summarized by the sample mean value and its uncertainty which is commonly based on a repeatability standard deviation. New confidence intervals for the lab’s bias are derived. Although they may lack intuitive appeal, those obtained by using higher order asymptotic methods, compared and contrasted in this paper, are recommended.

  11. INAA Application for Trace Element Determination in Biological Reference Material

    Science.gov (United States)

    Atmodjo, D. P. D.; Kurniawati, S.; Lestiani, D. D.; Adventini, N.

    2017-06-01

    Trace element determination in biological samples is often used in the study of health and toxicology. Determination change to its essentiality and toxicity of trace element require an accurate determination method, which implies that a good Quality Control (QC) procedure should be performed. In this study, QC for trace element determination in biological samples was applied by analyzing the Standard Reference Material (SRM) Bovine muscle 8414 NIST using Instrumental Neutron Activation Analysis (INAA). Three selected trace element such as Fe, Zn, and Se were determined. Accuracy of the elements showed as %recovery and precision as %coefficient of variance (%CV). The result showed that %recovery of Fe, Zn, and Se were in the range between 99.4-107%, 92.7-103%, and 91.9-112%, respectively, whereas %CV were 2.92, 3.70, and 5.37%, respectively. These results showed that INAA method is precise and accurate for trace element determination in biological matrices.

  12. The ETH Zurich AMS facilities: Performance parameters and reference materials

    Energy Technology Data Exchange (ETDEWEB)

    Christl, M., E-mail: mchristl@phys.ethz.ch [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland); Vockenhuber, C.; Kubik, P.W.; Wacker, L.; Lachner, J.; Alfimov, V.; Synal, H.-A. [Laboratory of Ion Beam Physics, ETH Zurich, 8093 Zurich (Switzerland)

    2013-01-15

    The current performance of all three AMS systems in operation at ETH Zurich, the 6 MV HVEC EN-Tandem facility 'TANDEM', the 0.5 MV NEC Pelletron 'TANDY', and the 0.2 MV system 'MICADAS' is summarized. Radionuclides routinely measured with these AMS systems include {sup 10}Be, {sup 14}C, {sup 26}Al, {sup 36}Cl, {sup 41}Ca, {sup 129}I and the actinides. The reference materials used for the normalization of the AMS measurements at the ETH Zurich AMS facilities are presented. This paper therefore is a comprehensive status report of all three AMS systems currently operated by the Laboratory of Ion Beam Physics (LIP) at ETH Zurich and documents their performance and operation parameters.

  13. IAEA reference materials for quality assurance of marine radioactivity measurements

    International Nuclear Information System (INIS)

    Povinec, P.P.; Pham, M.K.

    2001-01-01

    The IAEA's Marine Environment Laboratory has been assisting laboratories in Analytical Quality Control Services (AQCS) for the analysis of radionuclides in the marine environment since the early seventies. AQCS through world-wide and regional intercomparison exercises and the provision of reference methods and reference materials (RM) have been recognized as an important component of quality assurance/quality control. A total of 43 intercomparison exercises were organized and 37 RM were produced for marine radioactivity studies. All important marine matrices were covered, e.g., seawater, marine sediments of different chemical compositions, fish, shellfish and seaplants. RM were prepared from samples collected at contaminated sites (e.g., the Irish Sea, the Baltic Sea, the Arabian Sea, Mururoa and Bikini Atolls, etc.) as well as from sites affected only by global fallout (e.g., the Pacific Ocean). Available RM are listed in the IAEA biennial catalogue and can be purchased at a minimal price. An overview of prepared RM for radionuclides in marine matrices is presented and discussed in more detail. (author)

  14. New Carbonate Standard Reference Materials for Boron Isotope Geochemistry

    Science.gov (United States)

    Stewart, J.; Christopher, S. J.; Day, R. D.

    2015-12-01

    The isotopic composition of boron (δ11B) in marine carbonates is well established as a proxy for past ocean pH. Yet, before palaeoceanographic interpretation can be made, rigorous assessment of analytical uncertainty of δ11B data is required; particularly in light of recent interlaboratory comparison studies that reported significant measurement disagreement between laboratories [1]. Well characterised boron standard reference materials (SRMs) in a carbonate matrix are needed to assess the accuracy and precision of carbonate δ11B measurements throughout the entire procedural chemistry; from sample cleaning, to ionic separation of boron from the carbonate matrix, and final δ11B measurement by multi-collector inductively coupled plasma mass spectrometry. To date only two carbonate reference materials exist that have been value-assigned by the boron isotope measurement community [2]; JCp-1 (porites coral) and JCt-1 (Giant Clam) [3]. The National Institute of Standards and Technology (NIST) will supplement these existing standards with new solution based inorganic carbonate boron SRMs that replicate typical foraminiferal and coral B/Ca ratios and δ11B values. These new SRMs will not only ensure quality control of full procedural chemistry between laboratories, but have the added benefits of being both in abundant supply and free from any restrictions associated with shipment of biogenic samples derived from protected species. Here we present in-house δ11B measurements of these new boron carbonate SRM solutions. These preliminary data will feed into an interlaboratory comparison study to establish certified values for these new NIST SRMs. 1. Foster, G.L., et al., Chemical Geology, 2013. 358(0): p. 1-14. 2. Gutjahr, M., et al., Boron Isotope Intercomparison Project (BIIP): Development of a new carbonate standard for stable isotopic analyses. Geophysical Research Abstracts, EGU General Assembly 2014, 2014. 16(EGU2014-5028-1). 3. Inoue, M., et al., Geostandards and

  15. Computing and physical methods to calculate Pu

    International Nuclear Information System (INIS)

    Mohamed, Ashraf Elsayed Mohamed

    2013-01-01

    Main limitations due to the enhancement of the plutonium content are related to the coolant void effect as the spectrum becomes faster, the neutron flux in the thermal region tends towards zero and is concentrated in the region from 10 Ke to 1 MeV. Thus, all captures by 240 Pu and 242 Pu in the thermal and epithermal resonance disappear and the 240 Pu and 242 Pu contributions to the void effect became positive. The higher the Pu content and the poorer the Pu quality, the larger the void effect. The core control in nominal or transient conditions Pu enrichment leads to a decrease in (B eff.), the efficiency of soluble boron and control rods. Also, the Doppler effect tends to decrease when Pu replaces U, so, that in case of transients the core could diverge again if the control is not effective enough. As for the voiding effect, the plutonium degradation and the 240 Pu and 242 Pu accumulation after multiple recycling lead to spectrum hardening and to a decrease in control. One solution would be to use enriched boron in soluble boron and shutdown rods. In this paper, I discuss and show the advanced computing and physical methods to calculate Pu inside the nuclear reactors and glovebox and the different solutions to be used to overcome the difficulties that effect, on safety parameters and on reactor performance, and analysis the consequences of plutonium management on the whole fuel cycle like Raw materials savings, fraction of nuclear electric power involved in the Pu management. All through two types of scenario, one involving a low fraction of the nuclear park dedicated to plutonium management, the other involving a dilution of the plutonium in all the nuclear park. (author)

  16. Use of neutron activation in dietary reference material analysis

    Energy Technology Data Exchange (ETDEWEB)

    Woittiez, J R.W.; Iyengar, G V

    1988-12-01

    Results for a number of trace elements in a total human diet material (USDIET-1), obtained by the application of both INAA and RNAA are presented. Several dietary reference materials such as NBS SRM 1577A, and BCR CRM Single Cell Protein were also analyzed, and these results are also given. Combining measurements on short and long lived radionuclides, the INAA approach is useful for the determination of about 20 elements. In order to expand the elemental coverage or improve detection limits, RNAA was also explored in two modes: separation of radionuclides using organic ion exchange resins and the use of hydrated manganese dioxide. This combination is applicable to 15 trace elements. For example, using RNAA, the following results were obtained for USDIET-1: Cd=31.8, Mo=280, Cr=71, Ag=4, As=117 and Sb=9.4 ..mu..g/kg. In the INAA mode, special attention was given to Al, F and Se. The F content of USDIET-1 was found to be 840 mg/kg, a rather high value, resulting from handling USDIET-1 by Teflon tools. By applying INAA and RNAA under two different laboratory conditions, it has been demonstrated that, even for the so-called difficult to determine elements like Cr, As or Mo, consistent results can be obtained. Thus, NAA promises to be a strong tool for human nutritional studies.

  17. Reactor neutron activation analysis on reference materials from intercomparison runs

    International Nuclear Information System (INIS)

    Pantelica, A.; Salagean, M.

    2003-01-01

    A review of using the Instrumental Neutron Activation Analysis (INAA) technique in our laboratory to determine major, minor and trace elements in mineral and biological samples from international intercomparison runs organised by IAEA Vienna, IAEA-MEL Monaco, 'pb-anal' Kosice, INCT Warszawa and IPNT Krakow is presented. Neutron irradiation was carried out at WWR-S reactor in Bucharest (short and long irradiation) during 1982-1997 and at TRIGA reactor in Pitesti (long irradiation) during the later period. The following type of materials were analysed: soils, marine sediments, uranium phosphate ore, water sludge, copper flue dust, whey powder, yeast, cereal flour (rye and wheat), marine animal tissue (mussel, garfish and tuna fish), as well as vegetal tissue (seaweed, cabbage, spinach, alfalfa, algae, tea leaves and herbs). The following elements could be, in general, determined: Ag, As, Au, Ba, Br, Ca, Ce, Co, Cr, Cs, Eu, Fe, Hf, Hg, K, La, Lu, Mo, Na, Nd, Ni, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, U, W, Yb and Zn of long-lived radionuclides, as well as Al, Ca, Cl, Cu, Mg, Mn, and Ti of short-lived radionuclides. Data obtained in our laboratory for various matrix samples presented and compared with the intercomparison certified values. The intercomparison exercises offer to the participating laboratories the opportunity to test the accuracy of their analytical methods as well as to acquire valuable Reference Materials/ standards for future analytical applications. (authors)

  18. Nuclear microprobe analysis of the standard reference materials

    International Nuclear Information System (INIS)

    Jaksic, M.; Fazinic, S.; Bogdanovic, I.; Tadic, T.

    2002-01-01

    Most of the presently existing Standard Reference Materials (SRM) for nuclear analytical methods are certified for the analyzed mass of the order of few hundred mg. Typical mass of sample which is analyzed by PIXE or XRF methods is very often below 1 mg. By the development of focused proton or x-ray beams, masses which can be typically analyzed go down to μg or even ng level. It is difficult to make biological or environmental SRMs which can give desired homogeneity at such low scale. However, use of fundamental parameter quantitative evaluation procedures (absolute method), minimize needs for SRMs. In PIXE and micro PIXE setup at our Institute, fundamental parameter approach is used. For exact calibration of the quantitative analysis procedure just one standard sample is needed. In our case glass standards which showed homogeneity down to micron scale were used. Of course, it is desirable to use SRMs for quality assurance, and therefore need for homogenous materials can be justified even for micro PIXE method. In this presentation, brief overview of PIXE setup calibration is given, along with some recent results of tests of several SRMs

  19. 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

  20. Laboratory Reference Spectroscopy of Icy Satellite Candidate Surface Materials (Invited)

    Science.gov (United States)

    Dalton, J. B.; Jamieson, C. S.; Shirley, J. H.; Pitman, K. M.; Kariya, M.; Crandall, P.

    2013-12-01

    The bulk of our knowledge of icy satellite composition continues to be derived from ultraviolet, visible and infrared remote sensing observations. Interpretation of remote sensing observations relies on availability of laboratory reference spectra of candidate surface materials. These are compared directly to observations, or incorporated into models to generate synthetic spectra representing mixtures of the candidate materials. Spectral measurements for the study of icy satellites must be taken under appropriate conditions (cf. Dalton, 2010; also http://mos.seti.org/icyworldspectra.html for a database of compounds) of temperature (typically 50 to 150 K), pressure (from 10-9 to 10-3 Torr), viewing geometry, (i.e., reflectance), and optical depth (must manifest near infrared bands but avoid saturation in the mid-infrared fundamentals). The Planetary Ice Characterization Laboratory (PICL) is being developed at JPL to provide robust reference spectra for icy satellite surface materials. These include sulfate hydrates, hydrated and hydroxylated minerals, and both organic and inorganic volatile ices. Spectral measurements are performed using an Analytical Spectral Devices FR3 portable grating spectrometer from .35 to 2.5 microns, and a Thermo-Nicolet 6500 Fourier-Transform InfraRed (FTIR) spectrometer from 1.25 to 20 microns. These are interfaced with the Basic Extraterrestrial Environment Simulation Testbed (BEEST), a vacuum chamber capable of pressures below 10-9 Torr with a closed loop liquid helium cryostat with custom heating element capable of temperatures from 30-800 Kelvins. To generate optical constants (real and imaginary index of refraction) for use in nonlinear mixing models (i.e., Hapke, 1981 and Shkuratov, 1999), samples are ground and sieved to six different size fractions or deposited at varying rates to provide a range of grain sizes for optical constants calculations based on subtractive Kramers-Kronig combined with Hapke forward modeling (Dalton and

  1. Reference materials for molecular diagnostics: Current achievements and future strategies.

    Science.gov (United States)

    Jing, Rongrong; Wang, Huimin; Ju, Shaoqing; Cui, Ming

    2018-06-01

    Molecular diagnoses have become more widespread in many areas of laboratory medicine where qualitative or quantitative approaches are used to detect nucleic acids. The increasing number of assay methods and the targets for molecular diagnostics contribute to variability in the test results among clinical laboratories. Thus, reference materials (RMs) are required to enhance the comparability of results. This review focuses on the definition of RMs as well as the production and characteristics of higher order RMs from different organizations and their future strategies. We describe the recent progress in RMs, including the definition of RMs by the Joint Committee for Guides in Metrology, as well as the production and characteristics of higher order RMs by international official bodies. There is an urgent need for RMs in nucleic acid testing, especially higher order RMs. To advance the harmonization and standardization of clinical nucleic acid detection, cooperation between the above organizations is proposed and different approaches to higher order RMs development are also needed. Copyright © 2018 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  2. LA-ICP-MS of magnetite: Methods and reference materials

    Science.gov (United States)

    Nadoll, P.; Koenig, A.E.

    2011-01-01

    Magnetite (Fe3O4) is a common accessory mineral in many geologic settings. Its variable geochemistry makes it a powerful petrogenetic indicator. Electron microprobe (EMPA) analyses are commonly used to examine major and minor element contents in magnetite. Laser ablation ICP-MS (LA-ICP-MS) is applicable to trace element analyses of magnetite but has not been widely employed to examine compositional variations. We tested the applicability of the NIST SRM 610, the USGS GSE-1G, and the NIST SRM 2782 reference materials (RMs) as external standards and developed a reliable method for LA-ICP-MS analysis of magnetite. LA-ICP-MS analyses were carried out on well characterized magnetite samples with a 193 nm, Excimer, ArF LA system. Although matrix-matched RMs are sometimes important for calibration and normalization of LA-ICP-MS data, we demonstrate that glass RMs can produce accurate results for LA-ICP-MS analyses of magnetite. Cross-comparison between the NIST SRM 610 and USGS GSE-1G indicates good agreement for magnetite minor and trace element data calibrated with either of these RMs. Many elements show a sufficiently good match between the LA-ICP-MS and the EMPA data; for example, Ti and V show a close to linear relationship with correlation coefficients, R2 of 0.79 and 0.85 respectively. ?? 2011 The Royal Society of Chemistry.

  3. Reference Materials: Critical Importance to the Infant Formula Industry.

    Science.gov (United States)

    Wargo, Wayne F

    2017-09-01

    Infant formula is one of the most regulated foods in the world. It has advanced in complexity over the years as a result of numerous research innovations. To ensure product safety and quality, analytical technologies have also had to advance to keep pace. Given the rigorous performance demands expected of these methods and the ever-growing array of complex matrixes, there is the potential for gaps to exist in current Official MethodsSM and other recognized international methods for infant formula and adult nutritionals. Food safety concerns, particularly for infants, drive the need for extensive testing by manufacturers and regulators. The net effect is the potential for an increase in time- and resource-consuming regulatory disputes. In an effort to mitigate such costly activities, AOAC INTERNATIONAL, under the direction of the Infant Formula Council of America-a trade association of manufacturers and marketers of formulated nutritional products-agreed to establish voluntary consensus Standard Method Performance Requirements, and, ultimately, to identify and publish globally recognized, fit-for-purpose standard methods. To accomplish this task, nutritional reference materials (RMs), representing all major commercially available nutritional formulations, were (and continue to be) a critical necessity. In this paper, various types of RMs will be defined, followed by review and discussion of their importance to the infant formula industry.

  4. A comparative study of nitride purity and Am fabrication losses in PuN materials by the powder and internal gelation production routes

    Energy Technology Data Exchange (ETDEWEB)

    Hedberg, Marcus, E-mail: marhed@chalmers.se; Ekberg, Christian

    2016-12-15

    Fabrication of plutonium containing fuels through the internal gelation method has mostly been studied in mixed metal systems such as U, Pu or Zr,Pu. In this work production of undiluted PuN has been performed by carbothermal reduction on both oxide powder and Pu microspheres produced by the internal gelation method. Nitride purities reached using the different methods have been studied together with final densities achieved during pellet fabrication as well as losses of ingrown Am during the different production steps. Formation of Pu microspheres was successfully performed using the internal gelation method, although extensive microsphere fracturing occurred during thermal treatment. Final densities of PuN pellets produced by cold pressing and sintering reached 70–80% of theoretical density. Am losses during the carbothermal reduction step was on average about 3.7%. After sintering about 11% of Am was lost in total through the entire production process if sintering in N{sub 2} + 5% H{sub 2} atmosphere while about 50% of the Am in total was lost when using Ar as sintering atmosphere. - Highlights: • Internal gelation Pu based sols was performed. • Nitride formation by carbothermal reduction on Pu microspheres and powders was performed. • Pelletization and sintering of pellets was performed. • Am losses were measured throughout the production steps.

  5. Speciation analysis of 129I, 137Cs, 232Th, 238U, 239Pu and 240Pu in environmental soil and sediment

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hansen, Violeta; Hou, Xiaolin

    2012-01-01

    The environmental mobility and bioavailability of radionuclides are related to their physicochemical forms, namely species. We here present a speciation analysis of important radionuclides including 129I (also 127I), 137Cs, 232Th, 238U and plutonium isotopes (239Pu and 240Pu) in soil (IAEA-375......) and sediment (NIST-4354) standard reference materials and two fresh sediment samples from Øvre Heimdalsvatnet Lake, Norway. A modified sequential extraction protocol was used for the speciation analysis of these samples to obtain fractionation information of target radionuclides. Analytical results reveal...

  6. Artificial radioactivity in the environmental samples as IAEA reference materials

    International Nuclear Information System (INIS)

    Salagean, M.; Pantelica, A.

    1998-01-01

    . Uncontaminated by nuclear activities: IAEA-327, Podsolic soil collected in 1990 from the Moscow region and considered uncontaminated by radionuclides of the Chernobyl accident or by other nuclear activities. The results obtained by our laboratory are in good agreement with the certified IAEA data. Generally, the concentration of the artificial radionuclides in the investigated samples is higher than that expected from the influence of global fallout in the intercomparison materials distributed before Chernobyl accident. Concerning the nature of these investigated IAEA reference materials, very high values for the concentration levels of cesium radionuclides especially in IAEA-373 (grass) and IAEA-375 (soil) samples collected in the vicinity of Chernobyl Power Station after the nuclear accident in 1986 were found. High levels of radioactivities for the artificial radionuclides were also determined in the samples collected in the neighbourhood of the nuclear installations, especially in marine sediment (IAEA-135). It is of interest to point out the high concentration of cesium radionuclides in IAEA-300 sediment collected in 1992 in the Baltic Sea in comparison with the IAEA-306 sediment collected also in the Baltic Sea in 1986. It seems to be an increase of the Baltic Sea artificial radioactivity by accumulation in time. Marine sediment constitutes an important component of marine ecosystem since it represents the final sink for any releases of wastes into the sea. These certified radioactive materials are very useful to all laboratories engaged in the radioactive pollution investigations on environmental samples. (authors)

  7. 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

  8. 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.

  9. 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.)

  10. Local atomic structure of α-Pu

    International Nuclear Information System (INIS)

    Espinosa, F. J.; Villella, P.; Lashley, J. C.; Conradson, S. D.; Cox, L. E.; Martinez, R.; Martinez, B.; Morales, L.; Terry, J.; Pereyra, R. A.

    2001-01-01

    The local atomic structure of α-Pu was investigated using x-ray absorption fine structure (XAFS) spectroscopy. XAFS spectra were obtained for a zone-refined α-Pu and the results were compared to 32-year-old and Ce-doped (0.34 at.%) samples. X-ray diffraction (XRD) patterns were also measured for the zone-refined and 32-year-old materials. The extent of the Bragg peaks showed that amorphization of the 32-year-old sample had not occurred despite the prolonged exposure to self-radiation. Analogous to metastable δ-Pu alloys, the local atomic structure around Pu for the zone-refined material shows the possible presence of noncrystallographic Pu-Pu distances. Conversely, the Ce and the 32-year-old sample show no evidence for such noncrystallographic distances. Disorder in the Pu local environment was found to be impurity dependent. The Ce-doped sample presented a larger Pu-Pu nearest neighbor disorder than the aged sample, although the total amount of Am, U, and He impurities was actually higher in the aged sample. The local environment around U and Ce impurities is consistent with these elements being in substitutional lattice sites. In addition, U and Ce do not introduce significant lattice distortion to their nearest neighbors. This is consistent with disorder being more related to the perturbation of the coupling between the electronic and crystal structure, or the Peierls--Jahn-Teller distortion that generates the monoclinic α-Pu structure, and less to strain fields produced in the vicinity of the impurities

  11. Reference Materials in LIS Instruction: A Delphi Study

    Science.gov (United States)

    Rabina, Debbie

    2013-01-01

    This paper presents the results of a Delphi study conducted over a two-month period in 2011. The purpose of the study was to identify reference sources that should be covered in basic reference courses taught in LIS programs in the United States. The Delphi method was selected for its appropriateness in soliciting expert opinions and assessing the…

  12. Chemical speciation of Pu in natural waters

    International Nuclear Information System (INIS)

    Nelson, D.M.; Larsen, R.P.; Penrose, W.R.

    1983-01-01

    The behavior of plutonium in natural waters is determined to a major degree by the chemical forms which are present. We have characterized the ambient Pu in a number of surface waters with regard to its oxidation state and association with natural colloidal organic carbon compounds using a combination of field measurements and laboratory experiments. Both of these factors are shown to have a profound effect on the adsorption of Pu to natural sediments, since both complexation with organic matter and oxidation compete with adsorption. The concentration of organic carbon in the water is the key variable influencing both oxidation state and organic binding. The adsorption process conforms to the laws applicable to a reversible equilibrium with values of the distribution coefficient, K/sub D/, measured in laboratory experiments being similar to those observed for ambient Pu. Experiments using natural waters and sediments in which the Pu concentration was varied show the forms present at typical ambient concentrations (10 -17 - 10 -14 M) are the same as those found at concentrations up to 10 -7 M. Moreover, the affinity for sediments did not change with concentration indicating the binding sites for Pu had not become saturated. Thus, the behavior observed for Pu at ultratrace concentrations should remain unchanged throughout this concentration range. The studies in this report all deal with Pu in exchangeable (and hence source independent) forms and should therefore reflect the behavior toward which the plutonium from any source will tend with time. 13 references, 7 figures, 10 tables

  13. Determination of {sup 241}Pu in nuclear waste slurries: A comparative study using LSC and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Jaeggi, M., E-mail: maya.jaeggi@psi.ch [Department Logistics for Radiation Safety and Security, Radioanalytics, CH-5232 Villligen PSI (Switzerland); Roellin, S., E-mail: Stefan.Roellin@babs.admin.ch [Federal Office for Civil Protection, SPIEZ Laboratory, CH-3700 Spiez (Switzerland); Corcho Alvarado, J.A., E-mail: Corcho-Alvarado@chuv.ch [Institute of Radiation Physics, University Hospital and University of Lausanne, Rue du Grand-Pre 1, 1007 Lausanne (Switzerland); Eikenberg, J., E-mail: jost.eikenberg@psi.ch [Department Logistics for Radiation Safety and Security, Radioanalytics, CH-5232 Villligen PSI (Switzerland)

    2012-02-15

    {sup 241}Pu was determined in slurry samples from a nuclear reactor decommissioning project at the Paul Scherrer Institute (Switzerland). To validate the results, the {sup 241}Pu activities of five samples were determined by LSC (TriCarb and Quantulus) and ICP-MS, with each instrument at a different laboratory. In lack of certified reference materials for {sup 241}Pu, the methods were further validated using the {sup 241}Pu information values of two reference sediments (IAEA-300 and IAEA-384). Excellent agreement with the results was found between LSC and ICP-MS in the nuclear waste slurries and the reference sediments. - Highlights: Black-Right-Pointing-Pointer Good agreement between the {sup 241}Pu activity of 5 slurry samples, using 3 measurement techniques. Black-Right-Pointing-Pointer {sup 241}Pu information values of two IAEA samples agreed well for the 3 measurement techniques. Black-Right-Pointing-Pointer Low detection limits were achieved; 1.8 Bq/kg (Quantulus), 2 Bq/kg (ICP-MS) and 3.5 Bq/kg (TriCarb).

  14. 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.

  15. Electronic Correlation Strength of Pu

    DEFF Research Database (Denmark)

    Svane, A.; C. Albers, R.; E. Christensen, N.

    2013-01-01

    A new electronic quantity, the correlation strength, is defined as a necessary step for understanding the properties and trends in strongly correlated electronic materials. As a test case, this is applied to the different phases of elemental Pu. Within the GW approximation we have surprisingly...... found a "universal" scaling relationship, where the f-electron bandwidth reduction due to correlation effects is shown to depend only upon the local density approximation (LDA) bandwidth and is otherwise independent of crystal structure and lattice constant....

  16. Economical Production of Pu-238

    Energy Technology Data Exchange (ETDEWEB)

    Steven D. Howe; Douglas Crawford; Jorge Navarro; Terry Ring

    2013-02-01

    All space exploration missions traveling beyond Jupiter must use radioisotopic power sources for electrical power. The best isotope to power these sources is plutonium-238. The US supply of Pu-238 is almost exhausted and will be gone within the next decade. The Department of Energy has initiated a production program with a $10M allocation from NASA but the cost is estimated at over $100 M to get to production levels. The Center for Space Nuclear Research has conceived of a potentially better process to produce Pu-238 earlier and for significantly less cost. The new process will also produce dramatically less waste. Potentially, the front end costs could be provided by private industry such that the government only had to pay for the product produced. Under a NASA Phase I NIAC grant, the CSNR has evaluated the feasibility of using a low power, commercially available nuclear reactor to produce at least 1.5 kg of Pu-238 per year. The impact on the neutronics of the reactor have been assessed, the amount of Neptunium target material estimated, and the production rates calculated. In addition, the size of the post-irradiation processing facility has been established. In addition, a new method for fabricating the Pu-238 product into the form used for power sources has been identified to reduce the cost of the final product. In short, the concept appears to be viable, can produce the amount of Pu-238 needed to support the NASA missions, can be available within a few years, and will cost significantly less than the current DOE program.

  17. Statistical signal processing and artificial intelligence applications in the nondestructive assay of U/Pu bearing materials

    International Nuclear Information System (INIS)

    Aumeier, S.E.; Forsmann, J.H.

    1997-01-01

    Over the years a number of techniques have been developed to determine the quantity and distribution of radiative isotopes contained in given assay samples through the measurement and analysis of penetrating characteristic radiations. An active technique of particular utility when assaying samples containing very small quantities of fissionable material or when high gamma ray backgrounds are encountered is the delayed neutron nondestructive assay (DN-NDA) technique. Typically, analysis of the delayed neutron signal involves relating the gross delayed neutron count observed following neutron irradiation of an assay sample to total fissionable material present via a linear calibration curve. In this way, the technique is capable of yielding the mass of a single dominant fissionable isotope or the total fissionable mass contained in a sample. Using this approach the only way to determine the mass of individual fissionable isotopes contained in a sample is to correlate total fissionable mass to individual isotopics via calculations or other means, yielding an indirect measure of isotopics. However, there is isotope specific information in the temporal delayed neutron signal due to differences in the delayed neutron precursor yields resulting from the fissioning of different isotopes. The authors present the results of an analysis to evaluate the feasibility of using Kalman filters and genetic algorithms to determine multiple specific fissionable isotopic masses contained in an assay sample from a cumulative delayed neutron signal measured following neutron irradiation of the sample

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-11-15

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

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

    Science.gov (United States)

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

    2008-11-01

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

  1. 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

  2. 10 CFR 431.303 - Materials incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ... this material at NARA, call 202-741-6030 or go to http://www.archives.gov/federal_register/code_of... through Friday, except Federal holidays, or go to: http://www1.eere.energy.gov/buildings/appliance... and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, (610) 832-9500, or http://www...

  3. Investigation of the oxidation states of Pu isotopes in a hydrochloric acid solution

    Energy Technology Data Exchange (ETDEWEB)

    Lee, M.H. [Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute, P. O. Box 105, Yuseong, Daejeon 305-353 (Korea, Republic of)], E-mail: mhlee@kaeri.re.kr; Kim, J.Y.; Kim, W.H.; Jung, E.C.; Jee, K.Y. [Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute, P. O. Box 105, Yuseong, Daejeon 305-353 (Korea, Republic of)

    2008-12-15

    The characteristics of the oxidation states of Pu in a hydrochloric acid solution were investigated and the results were applied to a separating of Pu isotopes from IAEA reference soils. The oxidation states of Pu(III) and Pu(IV) were prepared by adding hydroxylamine hydrochloride and sodium nitrite to a Pu stock solution, respectively. Also, the oxidation state of Pu(VI) was adjusted with concentrated HNO{sub 3} and HClO{sub 4}. The stability of the various oxidation states of plutonium in a HCl solution with elapsed time after preparation were found to be in the following order: Pu(III){approx}Pu(VI)>Pu(IV)>Pu(V). The chemical recoveries of Pu(IV) in a 9 M HCl solution with an anion exchange resin were similar to those of Pu(VI). This method for the determination of Pu isotopes with an anion exchange resin in a 9 M HCl medium was applied to IAEA reference soils where the activity concentrations of {sup 239,240}Pu and {sup 238}Pu in IAEA-375 and IAEA-326 were consistent with the reference values reported by the IAEA.

  4. 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 ...

  5. 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

  6. 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

  7. 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)

  8. Distribution of 238Pu and 239240Pu in aquatic macrophytes from a midwestern watershed

    International Nuclear Information System (INIS)

    Wayman, C.W.; Bartelt, G.E.; Alberts, J.J.

    1977-01-01

    Aquatic macrophytes were collected in the Great Miami River, Ohio, above and below Miamisburg and in the canal and ponds, near the Mound Laboratory, which contain sediments of a high activity (approximately 10 3 to 10 6 times) relative to the river sediments. Macrophytes collected in the river below Miamisburg have higher activities of 238 Pu than those collected from above the city. Macrophytes from the canal and ponds contain high specific activities of 238 Pu and 239 , 240 Pu with the exception of cattails grown in the ponds. Concentration factors are reported and discussed with reference to possible modes of plutonium accumulation and distribution within the plants

  9. 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

  10. 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.

  11. Alternative buffer material. Status of the ongoing laboratory investigation of reference materials and test package 1

    International Nuclear Information System (INIS)

    Svensson, Daniel; Dueck, Ann; Nilsson, Ulf; Olsson, Siv; Sanden, Torbjoern; Lydmark, Sara; Jaegerwall, Sara; Pedersen, Karsten; Hansen, Staffan

    2011-07-01

    Bentonite clay is part of the Swedish KBS-3 design of final repositories for high level radioactive waste. Wyoming bentonite with the commercial name MX-80 (American Colloid Co) has long been the reference for buffer material in the KBS-3 concept. Extending the knowledge base of alternative buffer materials will make it possible to optimize regarding safety, availability and cost. For this reason the field experiment Alternative Buffer Material (ABM) was started at Aespoe Hard Rock Laboratory during 2006. The experiment includes three medium-scale test packages, each consisting of a central steel tube with heaters, and a buffer of compacted clay. Eleven different clays were chosen for the buffers to examine effects of smectite content, interlayer cations and overall iron content. Also bentonite pellets with and without additional quartz are being tested. The buffer in package 1 had been subjected to wetting by formation water and heating for more than two years (at 130 deg C for ∼ 1 year) when it was retrieved and analyzed. The main purposes of the project were to characterise the clays with respect to hydro-mechanical properties, mineralogy and chemical composition and to identify any differences in behaviour or long term stability. The diversity of clays and the heater of steel also make the experiment suitable for studies of iron-bentonite interactions. This report concerns the work accomplished up to now and is not to be treated as any final report of the project

  12. Alternative buffer material. Status of the ongoing laboratory investigation of reference materials and test package 1

    Energy Technology Data Exchange (ETDEWEB)

    Svensson, Daniel [Swedish Nuclear Fuel and Waste Management Co., Stockholm (Sweden); Dueck, Ann; Nilsson, Ulf; Olsson, Siv; Sanden, Torbjoern [Clay Technology AB, Lund (Sweden); Lydmark, Sara; Jaegerwall, Sara; Pedersen, Karsten [Microbial Analytics Sweden AB, Moelnlycke (Sweden); Hansen, Staffan [LTH Lund Univ., Lund (Sweden)

    2011-07-15

    Bentonite clay is part of the Swedish KBS-3 design of final repositories for high level radioactive waste. Wyoming bentonite with the commercial name MX-80 (American Colloid Co) has long been the reference for buffer material in the KBS-3 concept. Extending the knowledge base of alternative buffer materials will make it possible to optimize regarding safety, availability and cost. For this reason the field experiment Alternative Buffer Material (ABM) was started at Aespoe Hard Rock Laboratory during 2006. The experiment includes three medium-scale test packages, each consisting of a central steel tube with heaters, and a buffer of compacted clay. Eleven different clays were chosen for the buffers to examine effects of smectite content, interlayer cations and overall iron content. Also bentonite pellets with and without additional quartz are being tested. The buffer in package 1 had been subjected to wetting by formation water and heating for more than two years (at 130 deg C for {approx} 1 year) when it was retrieved and analyzed. The main purposes of the project were to characterise the clays with respect to hydro-mechanical properties, mineralogy and chemical composition and to identify any differences in behaviour or long term stability. The diversity of clays and the heater of steel also make the experiment suitable for studies of iron-bentonite interactions. This report concerns the work accomplished up to now and is not to be treated as any final report of the project.

  13. 10 CFR 431.323 - Materials incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ... National Standard for Lamp Ballasts—Ballasts for High-Intensity Discharge Lamps—Methods of Measurement... AND INDUSTRIAL EQUIPMENT Metal Halide Lamp Ballasts and Fixtures Test Procedures § 431.323 Materials... National Standard for electric lamps: Single-Ended Metal Halide Lamps, approved May 5, 2004, IBR approved...

  14. The preparation of four biological reference materials for QUASIMEME

    NARCIS (Netherlands)

    Leeuwen, van S.P.J.; Pieters, H.; Boer, de J.

    2004-01-01

    Four biological materials have been prepared for use in QUASIMEME interlaboratory studies including a shrimp sample for metal analysis (QM01-1) and two mussel (QO01-3 and QO02-2) and one mackerel sample (QO02-1) for organic contaminant analysis.

  15. 10 CFR 431.293 - Materials incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ....293 Energy DEPARTMENT OF ENERGY ENERGY CONSERVATION ENERGY EFFICIENCY PROGRAM FOR CERTAIN COMMERCIAL.../code_of_federal_regulations/ibr_locations.html. This material is also available for inspection at U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy, Building Technologies Program, 6th...

  16. 10 CFR 431.63 - Materials incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ... Energy DEPARTMENT OF ENERGY ENERGY CONSERVATION ENERGY EFFICIENCY PROGRAM FOR CERTAIN COMMERCIAL AND..._of_federal_regulations/ibr_locations.html. Also, this material is available for inspection at U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy, Building Technologies Program, 6th...

  17. 10 CFR 431.85 - Materials incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ... Energy DEPARTMENT OF ENERGY ENERGY CONSERVATION ENERGY EFFICIENCY PROGRAM FOR CERTAIN COMMERCIAL AND..._locations.html. Also, this material is available for inspection at U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy, Building Technologies Program, 6th Floor, 950 L'Enfant Plaza, SW...

  18. Alpha damage in non-reference waste form matrix materials

    International Nuclear Information System (INIS)

    Burnay, S.G.

    1987-05-01

    Although bitumen is the matrix material currently used for European α-bearing intermediate level waste streams, polymer and polymer-modified cement matrices could have advantages over bitumen for such wastes. Two organic matrix systems have been studied - an epoxide resin, and an epoxide modified cement. Alpha irradiations were carried out by incorporating 241 Am at approx. 0.9 Ci/l. Comparisons have been made with unirradiated material and with materials which had been γ-irradiated to the same dose as the α-irradiated samples. Measurements were made of dimensional changes, mechanical properties and the leaching behaviour of 241 Am and 137 Cs. A limited amount of swelling (< 3%) was observed in α-irradiated epoxide resin; none was observed in the epoxide modified cement. Gamma irradiation to 300 kGy has no significant effect on the mechanical properties of either system. However, alpha irradiation to the same dose produced significant changes in flexural strength, an increase for the polymer and a decrease for the polymer-cement. Leaching in these systems was found to be a diffusion-controlled process; alpha irradiation to approx. 250 kGy has little effect on the leaching behaviour of either system. (author)

  19. 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.

  20. 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

  1. Multicenter evaluation of the commutability of a potential reference material for harmonization of enzyme activities

    NARCIS (Netherlands)

    Scharnhorst, V.; Apperloo, J.J.; Baadenhuijsen, H.; Vader, H.L.

    2014-01-01

    Standardization of laboratory results allows for the use of common reference intervals and can be achieved via calibration of field methods with secondary reference materials. These harmonization materials should be commutable, i.e., they produce identical numerical results independent of assay

  2. Neutron activation analysis of trace elements in IAEA reference materials

    International Nuclear Information System (INIS)

    Cheema, M.N.; Hasany, S.M.; Hanif, I.; Chaudhry, M.S.; Qureshi, I.H.

    1978-09-01

    Analytical Chemistry Group of Nuclear Chemistry Division at PINSTECH has been participating in IAEA Intercomparison programme of analytical quality control since 1972. So far fifteen samples of a variety of materials received from the Agency have been analyzed for different minor and trace elements. Mostly destructive and non-destructive neutron activation analysis techniques have been used for elemental analysis. In this report the description of the samples and the experimental procedures employed have been mentioned. The results of elemental analysis have been reported and compared with IAEA values which are based on the average computed from the results of different participating laboratories. (authors)

  3. Fabrication of 12% 240Pu calorimetry standards

    International Nuclear Information System (INIS)

    Long, S.M.; Hildner, S.; Gutierrez, D.; Mills, C.; Garcia, W.; Gurule, C.

    1995-01-01

    Throughout the DOE complex, laboratories are performing calorimetric assays on items containing high burnup plutonium. These materials contain higher isotopic range and higher wattages than materials previously encountered in vault holdings. Currently, measurement control standards have been limited to utilizing 6% 240 Pu standards. The lower isotopic and wattage value standards do not complement the measurement of the higher burnup material. Participants of the Calorimetry Exchange (CALEX) Program have identified the need for new calorimetric assay standards with a higher wattage and isotopic range. This paper describes the fabrication and verification measurements of the new CALEX standard containing 12% 240 Pu oxide with a wattage of about 6 to 8 watts

  4. Anaerobic Biotransformation and Mobility of Pu and Pu-EDTA

    International Nuclear Information System (INIS)

    Bolton, H. Jr.; Rai, D.; Xun, L.

    2005-01-01

    The complexation of radionuclides (e.g., plutonium (Pu) and 60 Co) by codisposed ethylenediaminetetraacetate (EDTA) has enhanced their transport in sediments at DOE sites. Our previous NABIR research investigated the aerobic biodegradation and biogeochemistry of Pu(IV)-EDTA. Plutonium(IV) forms stable complexes with EDTA under aerobic conditions and an aerobic EDTA degrading bacterium can degrade EDTA in the presence of Pu and decrease Pu mobility. However, our recent studies indicate that while Pu(IV)-EDTA is stable in simple aqueous systems, it is not stable in the presence of relatively soluble Fe(III) compounds (i.e., Fe(OH) 3 (s)--2-line ferrihydrite). Since most DOE sites have Fe(III) containing sediments, Pu(IV) in likely not the mobile form of Pu-EDTA in groundwater. The only other Pu-EDTA complex stable in groundwater relevant to DOE sites would be Pu(III)-EDTA, which only forms under anaerobic conditions. Research is therefore needed in this brand new project to investigate the biotransformation of Pu and Pu-EDTA under anaerobic conditions. The biotransformation of Pu and Pu-EDTA under various anaerobic regimes is poorly understood including the reduction kinetics of Pu(IV) to Pu(III) from soluble (Pu(IV)-EDTA) and insoluble Pu(IV) as PuO2(am) by metal reducing bacteria, the redox conditions required for this reduction, the strength of the Pu(III)-EDTA complex, how the Pu(III)-EDTA complex competes with other dominant anoxic soluble metals (e.g., Fe(II)), and the oxidation kinetics of Pu(III)-EDTA. Finally, the formation of a stable soluble Pu(III)-EDTA complex under anaerobic conditions would require degradation of the EDTA complex to limit Pu(III) transport in geologic environments. Anaerobic EDTA degrading microorganisms have not been isolated. These knowledge gaps preclude the development of a mechanistic understanding of how anaerobic conditions will influence Pu and Pu-EDTA fate and transport to assess, model, and design approaches to stop Pu

  5. Mechanism based evaluation of materials behavior and reference curves

    International Nuclear Information System (INIS)

    Toerroenen, K.; Saario, T.; Wallin, K.; Forsten, J.

    1984-01-01

    The safety assessment of nuclear pressure vessels and piping requires a quantitative estimation of defect growth by stable and unstable manner during service. This estimation is essential for determining whether the defect detected during inspection should be repaired or whether the size of the defect even after its expected growth is small enough to leave the integrity of the vessel unaffected. The most important stable defect growth mechanism is that of environmentally assisted cyclic crack growth. Recent results indicate that it is markedly affected by sulfur content and/or manganese sulfide morphology and distribution. This implies that an essential improvement in component safety has been gained by currently applied steelmaking practices, which result in extra low sulfur content, generally below 0.01 wt%, and in round shape and small size of inclusions, through, e.g., calcium treatment, hence considerably reducing the effect of environment on crack growth rate. This further implies that the ASME Section XI reference curves for environmentally accelerated cyclic crack growth are conservative for steels produced by current steelmaking practices. (orig./WL)

  6. 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.

  7. 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.

  8. 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)

  9. Determination of technetium-99 in environmental standard reference materials by ICP-MS

    International Nuclear Information System (INIS)

    Tagami, K.; Uchida, S.

    2000-01-01

    Technetium-99 is an artificial radionuclide which is produced in the fission of 235 U or 239 Pu with a relatively high fission yield of ca. 6%. Because of its long half-life of 2.1 x 10 5 y, 99 Tc has been accumulating in the environment, and thus, is considered to present a potential risk for humans. It is important for dose assessments to identify the behavior of the nuclide in the environment. Analysis data of global fallout 99 Tc in environmental samples would give useful information for predicting the nuclide's behavior; however, due to its low concentration and analytical difficulties, not much data are available. Besides, no environmental standard reference material (SRM) for 99 Tc is available. If we could get suitable SRMs for 99 Tc analysis, it would be easier to determine the concentration of 99 Tc in environmental samples. The purpose of this study was to investigate the possibility of several SRMs to be used as references for low-level 99 Tc. For this, ICP-MS was used for 99 Tc determination. In recent years, ICP-MS has been used for 99 Tc measurements instead of radioactivity counting methods. The samples used were as follows: A) IAEA-373 (a grass sample collected on grassland near Chernobyl Nuclear Power Reactor, Ukraine), B) IAEA-375 (a soil sample collected on a field near Chernobyl Nuclear Power Reactor, Russia), C) IAEA-135 (a sea sediment sample affected by Sellafield, UK), D) five seaweed samples of which the concentration levels are different from each other (collected around the coast near Sellafield, UK). Throughout the chemical separation, 95m Tc was used as a yield monitor. The sample was incinerated for at least 2 h at 450degC. After 99 Tc extraction from the sample at 90degC for 3 h with 4M HNO 3 , the sample was filtered and the residue on the filter was washed with deionized water. The solution was diluted to ca. 0.1M HNO 3 then passed through TEVA resin column (EIChroM Industries, Inc.) to extract Tc onto the resin. Then Tc was

  10. Determination of Pu in soil samples

    International Nuclear Information System (INIS)

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

    2016-10-01

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

  11. Induced radioactivity evaluation for reference materials by European scientific cooperation

    International Nuclear Information System (INIS)

    Ventura, A.; Reffo, G.; Avrigeanu, V.; Antonov, A.N.; Grypeos, M.; Trkov, A.

    1997-01-01

    The global objective of this research is to apply the latest theoretical achievements for calculation of nuclear quantities on the request lists of the current EC projects related to activation (European Activation File) and fusion (European Fusion File, Joint Evaluation File and Fusion Evaluated Nuclear Data Library). The main goal has concerned the (n,p) and (n,α) reaction cross sections, of first importance for prediction of radiation damage in fusion reactor stainless steel. The required development of adequate activation computer codes and data libraries are expected to provide improvement of the following types of nuclear data: - threshold and capture reactions leading to long-lived radionuclides; - other neutron-induced reactions producing the most critical activities in elements ranging from boron to bismuth; - charged-particle emission spectra of neutron-induced reactions and charged-particle induced reactions needed to treat the important sequential (x,n) reactions; - detailed error estimates of critical nuclear data, in order to specify the uncertainty levels of current predictions for radiological properties of potential low-activation materials

  12. 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

  13. Physics of the fuel cycle. Evaluation of methods, uncertainties and estimation of the material balance for fuels UO2 and UO2-PuO2

    International Nuclear Information System (INIS)

    Monier, C.

    1997-09-01

    The research works of this thesis are aimed to evaluate the methods and the associated uncertainties for the material balances estimation of the burn-up UO 2 and MOX fuels which intervene in the fuel cycle physics. The studies carried out are used to qualify the cycle 'package' DARWIN for the PWRs material balances estimation. The elaboration and optimisation of the calculation routes are carried out following a very specific methodology, aimed at estimating the bias introduced by the modelizations simplification by a comparison with almost exact reference modelizations. Depending on the precision goals and the informations, the permissible approximation will be determined. Two calculation routes have been developed and the qualified by applying them to the used fuels isotopic analysis interpretation: one 'industry-oriented' calculation route which can calculate full UO 2 assemblies material balances with a 2 % precision on the main actinides, respecting the industrial specifications. This route must run with a reasonable calculation time and stay user-friendly; one reference calculation route for the precise interpretation of fuel samples made of pieces of burn-up MOX rods. Aiming to provide material balances with the best possible precision, this route does not have the same specifications concerning its use and its calculation time performance. (author)

  14. Redefining design criteria for Pu-238 gloveboxes

    International Nuclear Information System (INIS)

    Acosta, S.V.

    1998-01-01

    Enclosures for confinement of special nuclear materials (SNM) have evolved into the design of gloveboxes. During the early stages of glovebox technology, established practices and process operation requirements defined design criteria. Proven boxes that performed and met or exceeded process requirements in one group or area, often could not be duplicated in other areas or processes, and till achieve the same success. Changes in materials, fabrication and installation methods often only met immediate design criteria. Standardization of design criteria took a big step during creation of ''Special-Nuclear Materials R and D Laboratory Project, Glovebox standards''. The standards defined design criteria for every type of process equipment in its most general form. Los Alamos National Laboratory (LANL) then and now has had great success with Pu-238 processing. However with ever changing Environment Safety and Health (ES and H) requirements and Ta-55 Facility Configuration Management, current design criteria are forced to explore alternative methods of glovebox design fabrication and installation. Pu-238 fuel processing operations in the Power Source Technologies Group have pushed the limitations of current design criteria. More than half of Pu-238 gloveboxes are being retrofitted or replaced to perform the specific fuel process operations. Pu-238 glovebox design criteria are headed toward process designed single use glovebox and supporting line gloveboxes. Gloveboxes that will house equipment and processes will support TA-55 Pu-238 fuel processing needs into the next century and extend glovebox expected design life

  15. 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

  16. Three New Offset {delta}{sup 11}B Isotope Reference Materials for Environmental Boron Isotope Studies

    Energy Technology Data Exchange (ETDEWEB)

    Rosner, M. [BAM Federal Institute for Materials Research and Testing, Berlin (Germany); IsoAnalysis UG, Berlin (Germany); Vogl, J. [BAM Federal Institute for Materials Research and Testing, Berlin (Germany)

    2013-07-15

    The isotopic composition of boron is a well established tool in various areas of science and industry. Boron isotope compositions are typically reported as {delta}{sup 11}B values which indicate the isotopic difference of a sample relative to the isotope reference material NIST SRM 951. A significant drawback of all of the available boron isotope reference materials is that none of them covers a natural boron isotope composition apart from NIST SRM 951. To fill this gap of required {delta}{sup 11}B reference materials three new solution boric acid reference materials were produced, which cover 60 per mille of the natural boron isotope variation (-20 to 40 per mille {delta}{sup 11}B) of about 100 per mille . The new reference materials are certified for their {delta}{sup 11}B values and are commercially available through European Reference Materials (http://www.erm-crm.org). The newly produced and certified boron isotope reference materials will allow straightforward method validation and quality control of boron isotope data. (author)

  17. Efforts to save 244Pu in Mark 18A targets for use in international safeguards measurements

    International Nuclear Information System (INIS)

    Goldberg, Steven A.; Cappis, John; Clarke, Stephanie; Whitesel, Robert

    2001-01-01

    Full text: The Office of Arms Control and Nonproliferation and the Office of Security and Emergency Operations are working collaboratively to evaluate the disposition of a large quantity of the 244 Pu isotope contained in 65 Mark ISA targets at the Savannah River Site (SRS). 244 Pu is used as a standard reference material for plutonium analytical measurements required for both domestic and international safeguards. 244 Pu is particularly valuable for high accuracy measurements of plutonium in small samples containing trace quantities of plutonium (environmental analysis) and for measurements of material through-put in bulk processing facilities handling large volumes of plutonium and plutonium-bearing materials. In October 2000, an assessment team was tasked by the U.S. Department of Energy (DOE) Under Secretary to evaluate pathways and costs for the chemical separation and isotopic enrichment of the 244 Pu identified in the targets. Even though the target materials have recently been designated as a National Resource, they are scheduled for waste disposal unless funds can be identified and assigned to the project. Background information on the Mark ISA targets and a review of the assessment process are presented below to inform other organizations and governments of current efforts to examine potential disposition options and to solicit international cooperation for the extraction of the 244 Pu. Background - The United States possesses the bulk of the world's supply of the rare isotope 244 Pu. This isotope was produced by extremely long neutron irradiation of 242 Pu in a high-flux reactor during experiments used primarily to create isotopes of medical interest. In its separated enriched form, 244 Pu is regarded as the most accurate and desirable spike for safeguards, forensics, and environmental analysis of plutonium, allowing the simultaneous measurement of a sample for isotopic abundances and elemental concentration. Such measurements are a critical component of

  18. Two spruce shoot candidate reference materials from the German environmental specimen bank

    International Nuclear Information System (INIS)

    Backhaus, F.; Bagschik, U.; Burow, M.; Froning, M.; Mohl, C.; Ostapczuk, P.; Rossbach, M.; Schladot, J.D.; Stoeppler, M.; Waidmann, E.; Byrne, A.R.; Zeisler, R.

    1994-01-01

    Two new materials are introduced that might serve as useful aids for the harmonisation of analytical results. Spruce shoots, cryogenically homogenized and characterized for 50 elements from two sampling sites of the German Environmental Specimen Bank (ESB) are presented as possible third generation reference materials that might also act as calibrating materials in speciation analysis. (author)

  19. 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.)

  20. 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)

  1. 239Pu standards for quantitative neutron-induced autoradiography

    International Nuclear Information System (INIS)

    Smith, J.M.; Atherton, D.R.; Wronski, T.J.; Jee, W.S.S.

    1977-01-01

    The present study deals with the preparation of 239 Pu standards for neutron bone tissue autoradiography and the calibration of these standards with respect to uranium reference standards. Known concentrations of 239 Pu were prepared in methyl methacrylate and Bioplastic casting resin bars. Wafers sawed from these bars served as standards. Solid state nuclear tract detectors (Lexan polycarbonate) were used to record fission fragment tracks after the standards were exposed to a thermal neutron flux. The original bars were found to contain a uniform distribution of 239 Pu. To confirm the concentration of 239 Pu in the wafers, the induced track density from the 239 Pu standards was compared with that from uranium reference standards. The average fission fragment detection efficiency for all of the standards was 0.51

  2. Pu Anion Exchange Process Intensification

    International Nuclear Information System (INIS)

    Taylor-Pashow, Kathryn M. L.

    2017-01-01

    This research is focused on improving the efficiency of the anion exchange process for purifying plutonium. While initially focused on plutonium, the technology could also be applied to other ion-exchange processes. Work in FY17 focused on the improvement and optimization of porous foam columns that were initially developed in FY16. These foam columns were surface functionalized with poly(4-vinylpyridine) (PVP) to provide the Pu specific anion-exchange sites. Two different polymerization methods were explored for maximizing the surface functionalization with the PVP. The open-celled polymeric foams have large open pores and large surface areas available for sorption. The fluid passes through the large open pores of this material, allowing convection to be the dominant mechanism by which mass transport takes place. These materials generally have very low densities, open-celled structures with high cell interconnectivity, small cell sizes, uniform cell size distributions, and high structural integrity. These porous foam columns provide advantages over the typical porous resin beads by eliminating the slow diffusion through resin beads, making the anion-exchange sites easily accessible on the foam surfaces. The best performing samples exceeded the Pu capacity of the commercially available resin, and also offered the advantage of sharper elution profiles, resulting in a more concentrated product, with less loss of material to the dilute heads and tails cuts. An alternate approach to improving the efficiency of this process was also explored through the development of a microchannel array system for performing the anion exchange.

  3. Pu Anion Exchange Process Intensification

    Energy Technology Data Exchange (ETDEWEB)

    Taylor-Pashow, Kathryn M. L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-10-06

    This research is focused on improving the efficiency of the anion exchange process for purifying plutonium. While initially focused on plutonium, the technology could also be applied to other ion-exchange processes. Work in FY17 focused on the improvement and optimization of porous foam columns that were initially developed in FY16. These foam columns were surface functionalized with poly(4-vinylpyridine) (PVP) to provide the Pu specific anion-exchange sites. Two different polymerization methods were explored for maximizing the surface functionalization with the PVP. The open-celled polymeric foams have large open pores and large surface areas available for sorption. The fluid passes through the large open pores of this material, allowing convection to be the dominant mechanism by which mass transport takes place. These materials generally have very low densities, open-celled structures with high cell interconnectivity, small cell sizes, uniform cell size distributions, and high structural integrity. These porous foam columns provide advantages over the typical porous resin beads by eliminating the slow diffusion through resin beads, making the anion-exchange sites easily accessible on the foam surfaces. The best performing samples exceeded the Pu capacity of the commercially available resin, and also offered the advantage of sharper elution profiles, resulting in a more concentrated product, with less loss of material to the dilute heads and tails cuts. An alternate approach to improving the efficiency of this process was also explored through the development of a microchannel array system for performing the anion exchange.

  4. 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)

  5. Normalization Methods and Selection Strategies for Reference Materials in Stable Isotope Analyes. Review

    Energy Technology Data Exchange (ETDEWEB)

    Skrzypek, G. [West Australian Biogeochemistry Centre, John de Laeter Centre of Mass Spectrometry, School of Plant Biology, University of Western Australia, Crawley (Australia); Sadler, R. [School of Agricultural and Resource Economics, University of Western Australia, Crawley (Australia); Paul, D. [Department of Civil Engineering (Geosciences), Indian Institute of Technology Kanpur, Kanpur (India); Forizs, I. [Institute for Geochemical Research, Hungarian Academy of Sciences, Budapest (Hungary)

    2013-07-15

    Stable isotope ratio mass spectrometers are highly precise, but not accurate instruments. Therefore, results have to be normalized to one of the isotope scales (e.g., VSMOW, VPDB) based on well calibrated reference materials. The selection of reference materials, numbers of replicates, {delta}-values of these reference materials and normalization technique have been identified as crucial in determining the uncertainty associated with the final results. The most common normalization techniques and reference materials have been tested using both Monte Carlo simulations and laboratory experiments to investigate aspects of error propagation during the normalization of isotope data. The range of observed differences justifies the need to employ the same sets of standards worldwide for each element and each stable isotope analytical technique. (author)

  6. Determination of trimethyllead reference material using high performance liquid chromatography-inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lu Hai; Wei Chao; Wang Jun; Chao Jingbo; Zhou Tao; Chen Dazhou

    2005-01-01

    A high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) was combined, and the chromatography conditions were optimized. The stability and homogeneity of a trimethyllead reference material were determined using this method. (authors)

  7. 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)

  8. 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....

  9. Pu Denaturing by Transmutation of MA in FBR Multi-cycle

    Energy Technology Data Exchange (ETDEWEB)

    Meiliza, Yoshitalia; Saito, Masaki; Sagara, Hiroshi [Tokyo Institute of Technology, 2-12-1-N1-1 Ookayama, Meguro-ku, Tokyo, 1528550 (Japan)

    2009-06-15

    Pu accumulation and its recycling is important in the term of energy resources, however one of the most sensitive issues is non-proliferation in the future fuel cycle based on fast breeder reactor (FBR). The present paper utilizes Protected Pu Production (P{sup 3}) concept for the production of {sup 238}Pu and {sup 242}Pu by Minor Actinides (MA) transmutation to enhance the proliferation resistance of Pu in the fuel. Increase in the {sup 238}Pu and {sup 242}Pu isotopic fraction creates a high rate of internal heat generation by alpha decay (DH) and/or a high neutron source of spontaneous fission (SFN) in Pu that would be encountered during manufacturing and maintaining of nuclear explosive device. The feasibility of denaturing of Pu by MA transmutation in medium size FBR has been studied from the viewpoint of even-mass number Pu accumulation during multi-cycle of Pu and MA. The proliferation resistance property of Pu is also evaluated based on the specific decay heat and spontaneous fission neutron, compared with the reference criteria. In present paper, the P{sup 3} technology based on multi-recycled Pu and MA is compared with the conventional technology based on multi-recycled Pu only. The detail of mass balance behavior is, however, beyond the scope of the present paper. (authors)

  10. 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)

  11. 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.

  12. 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)

  13. Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Kobayashi, K.; Kudo, K.

    1979-01-01

    Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultre-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B and C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS. (author)

  14. 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

  15. 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

  16. 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

  17. Internal Corrosion Analysis of Model 9975 Packaging Containing Pu or PuO2 During Shipping and Storage

    International Nuclear Information System (INIS)

    Vormelker, P.

    1999-01-01

    The Materials Consultation Group of SRTC has completed an internal corrosion analysis of the Model 9975 packaging assembly containing either Pu or PuO2 for storage in K Reactor under ambient conditions for a period of 12 years. The 12-year storage period includes two years for shipping and up to ten years for storage

  18. 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

  19. Interlaboratory Reproducibility of Droplet Digital Polymerase Chain Reaction Using a New DNA Reference Material Format.

    Science.gov (United States)

    Pinheiro, Leonardo B; O'Brien, Helen; Druce, Julian; Do, Hongdo; Kay, Pippa; Daniels, Marissa; You, Jingjing; Burke, Daniel; Griffiths, Kate; Emslie, Kerry R

    2017-11-07

    Use of droplet digital PCR technology (ddPCR) is expanding rapidly in the diversity of applications and number of users around the world. Access to relatively simple and affordable commercial ddPCR technology has attracted wide interest in use of this technology as a molecular diagnostic tool. For ddPCR to effectively transition to a molecular diagnostic setting requires processes for method validation and verification and demonstration of reproducible instrument performance. In this study, we describe the development and characterization of a DNA reference material (NMI NA008 High GC reference material) comprising a challenging methylated GC-rich DNA template under a novel 96-well microplate format. A scalable process using high precision acoustic dispensing technology was validated to produce the DNA reference material with a certified reference value expressed in amount of DNA molecules per well. An interlaboratory study, conducted using blinded NA008 High GC reference material to assess reproducibility among seven independent laboratories demonstrated less than 4.5% reproducibility relative standard deviation. With the exclusion of one laboratory, laboratories had appropriate technical competency, fully functional instrumentation, and suitable reagents to perform accurate ddPCR based DNA quantification measurements at the time of the study. The study results confirmed that NA008 High GC reference material is fit for the purpose of being used for quality control of ddPCR systems, consumables, instrumentation, and workflow.

  20. 239, 240, 241Pu fingerprinting of plutonium in western US soils using ICPMS: solution and laser ablation measurements

    International Nuclear Information System (INIS)

    Cizdziel, James V.; Ketterer, Michael E.; Farmer, Dennis; Faller, Scott H.; Hodge, Vernon F.

    2008-01-01

    -members. A rapid total dissolution procedure, followed by extraction chromatography and SF-ICPMS solution Pu analysis, generates excellent agreement with certified 239+240 Pu activities for standard reference materials NIST 4350b, NIST 4353, NIST 4357, and IAEA 385. 239+240 Pu activities and atom ratios determined by total dissolution reveal isotopic information in agreement with the LA-ICPMS dataset regarding the ubiquitous mixing of NTS and stratospheric fallout Pu sources in the regional environment. For several specific samples, the total dissolution method reveals that Pu is incompletely recovered by simpler HNO 3 -HCl leaching procedures, since some of the Pu originating from the NTS is contained in refractory siliceous particles. (orig.)

  1. A study of production of radioactive environmental reference materials used for proficiency testing program in Taiwan

    International Nuclear Information System (INIS)

    Peng, En-Chi; Wang, Jeng-Jong

    2013-01-01

    To realise radioactive environmental reference materials in Taiwan, seven environmental materials of soil, water, vegetation, meat, airborne particles (filter paper), milk and mushroom samples that are frequently encountered were used to establish the preparation of the reference materials. These seven environmental materials were collected, checked for freedom from radioactivity and prepared according to their properties. The preparation was carried out by using activity about 10–100 times that of the minimum detectable activity (MDA) in routine measurements in the radioactive standard used to spike the inactive material and this standard is traceable to national ionising radioactivity standards (TAF, 2004). To demonstrate sample traceability to the added standard, each sample was carefully measured and its uncertainty evaluated. Based on the recommendations of ISO Guide 35 for evaluation of reference materials and with the above assessment and verification procedures, the uncertainties (k=1) of the spike activity used in making reference materials were: 60 Co≤4.6%, 134 Cs≤4.7%, 137 Cs≤5.0%, total β≤0.6% and 3 H≤1.3%. - Highlights: • Seven kinds environmental materials were used to establish the production of the RMs. • Spiking the traceable standard radioactive source to the blank substance. • Each sample was carefully evaluated for its uncertainty. • The performance of the RMs was estimated with the Proficiency Testing program report. • The ability of the environment RMs in the configuration is quite good

  2. Certified reference materials for food packaging specific migration tests: development, validation and modelling

    NARCIS (Netherlands)

    Stoffers, N.H.

    2005-01-01

    Keywords:certified reference materials; diffusion; food contact materials; food packaging; laurolactam; migration modelling; nylon; specific migration This thesis compiles several research topics

  3. Development of in-plant reference material for composition of chinese cabbage with certified selenium content

    Directory of Open Access Journals (Sweden)

    D. A. Chupahin

    2014-01-01

    Full Text Available In-plant reference material for composition of Chinese cabbage with certified selenium content was developed for accuracy control of the results of selenium determination and within-laboratory quality control of analytical work in the analysis of food raw material.

  4. The preparation and certification of a South African phosphate concentrate for use as a reference material

    International Nuclear Information System (INIS)

    Hansen, R.G.

    1985-01-01

    This report describes the preparation, analysis, and certification of South African Reference Material (SARM) 32. The material is a phosphate concentrate from the Phalaborwa deposit, and was supplied by the Phosphate Development Corporation Ltd (Foskor). Eighteen laboratories in eight countries used a variety of analytical techniques to provide the analytical results

  5. Thallium determination in reference materials by isotope dilution mass spectrometry (IDMS) using thermal ionization

    International Nuclear Information System (INIS)

    Waidmann, E.; Hilpert, K.; Stoeppler, M.

    1990-01-01

    Using Isotope Dilution Mass Spectrometry (IDMS) with thermal ionization, thallium concentrations were determined in reference materials from NIST and BCR, from other sources, and reference materials from the German Environmental Specimen Bank 203 Tl spike solution is applied for the isotope dilution technique. Thallium concentrations in the investigated materials range from 2.67 μg Tl.kg -1 to 963 μg Tl.kg -1 with a relative standard deviation from 0.14 to 10%. The detection limit was 0.1 ng thallium for this work. (orig.)

  6. Report of the research co-ordination meeting on reference materials for microanalytical nuclear techniques

    International Nuclear Information System (INIS)

    1994-01-01

    Many microanalytical procedure require specific natural-matrix reference materials containing very low levels of trace elements and having a high degree of homogeneity. This proposed CRP will specifically address the question of quality control materials for these techniques. The participants of the meeting discussed the requirements for certified reference materials to by used in microanalysis with particular emphasis on the homogeneity issues. This publication contains summary of the discussions along with conclusions and recommendations made by the participants. The publication also contains 13 individual presentations delivered by the participants. Each of the individual papers has been provided with an abstract and indexed separately

  7. Report of the research co-ordination meeting on reference materials for microanalytical nuclear techniques

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-07-01

    Many microanalytical procedure require specific natural-matrix reference materials containing very low levels of trace elements and having a high degree of homogeneity. This proposed CRP will specifically address the question of quality control materials for these techniques. The participants of the meeting discussed the requirements for certified reference materials to by used in microanalysis with particular emphasis on the homogeneity issues. This publication contains summary of the discussions along with conclusions and recommendations made by the participants. The publication also contains 13 individual presentations delivered by the participants. Each of the individual papers has been provided with an abstract and indexed separately.

  8. Comparison of U-Pu-Mo, U-Pu-Nb, U-Pu-Ti and U-Pu-Zr alloys; Comparaison des alliages U-Pu-Mo, U-Pu-Nb, U-Pu-Ti, U-Pu-Zr

    Energy Technology Data Exchange (ETDEWEB)

    Boucher, R; Barthelemy, P [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1964-07-01

    The data concerning the U-Pu, U-Pu-Mo and U-Pu-Nb are recalled. The results obtained with U-Pu-Ti and U-Pu-Zr alloys containing 15-20 per cent Pu and 10 wt. per cent ternary element are reported. The transformation temperatures, the expansion coefficients, the nature of phases, the thermal cycling behaviour have been determined. A list of the principal properties of these different alloys is presented and the possibilities of their use as fast reactor's fuel element are considered. The U-Pu-Ti alloys seem to be quite promising: easiness of fabrication, large thermal stability, excellent behaviour in air, small quantity of zeta phase, temperature of solidus superior to 1100 deg. C. (authors) [French] On rappelle brievement les connaissances acquises sur les alliages U-Pu, U-Pu-Mo et U-Pu-Nb. On presente les resultats obtenus avec les alliages U-Pu-Ti et U-Pu-Zr pour des teneurs de 15 a 20 pour cent de plutonium et 10 pour cent en poids d'element ternaire. On a determine les temperatures de transformation, les coefficients de dilatation, la nature des phases, la conductibilite thermique a 20 deg. C, la tenue au cyclage thermique et diverses autres proprietes. Un tableau resume les principales proprietes des divers alliages. On considere les possibilites d'emploi de ces alliages comme combustibles de reacteur rapide. Les alliages U-Pu-Ti paraissent particulierement interessants: facilite d'elaboration, stabilite thermique etendue, tenue dans l'air excellente, faible quantite de la phase U-Pu zeta, temperature de fusion commencante superieure a 1100 deg. C. (auteurs)

  9. 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

  10. Critical outlook and trends for environmental reference materials at the Measurements & Testing Generic Activity (European Commission).

    Science.gov (United States)

    Quevauviller, P; Bennink, D; Bøwadt, S

    2001-05-01

    It is now well recognised that the quality control (QC) of all types of analyses, including environmental analyses depends on the appropriate use of reference materials. One of the ways to check the accuracy of methods is based on the use of Certified Reference Materials (CRMs), whereas other types of (not certified) Reference Materials (RMs) are used for routine quality control (establishment of control charts) and interlaboratory testing (e.g. proficiency testing). The perception of these materials, in particular with respect to their production and use, differs widely according to various perspectives (e.g. RM producers, routine laboratories, researchers). This review discusses some critical aspects of RM use and production for the QC of environmental analyses and describes the new approach followed by the Measurements & Testing Generic Activity (European Commission) to tackle new research and production needs.

  11. 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)

  12. 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

  13. Variations in Pu isotopic composition in soils from the Spitsbergen (Norway): Three potential pollution sources of the Arctic region.

    Science.gov (United States)

    Łokas, E; Anczkiewicz, R; Kierepko, R; Mietelski, J W

    2017-07-01

    Although the polar regions have not been industrialised, numerous contaminants originating from human activity are detectable in the Arctic environment. This study reports evidence of 240 Pu/ 239 Pu atomic ratios in the tundra and initial soils from different parts of west and central Spitsbergen and recognizes possible environmental inputs of non-global fallout Pu. The average atomic ratio of 240 Pu/ 239 Pu equal to 0.179 (ranging between 0.129 and 0.201) in tundra soils are comparable to the characteristic ratio for global fallout (0.180). However, the 240 Pu/ 239 Pu atomic ratios in the initial soils from proglacial zone of glaciers change within wide range between 0.1281 and 0.234 with the mean value of 0.169. By combining alpha and mass spectrometry, the three-sources model was used to identify the Pu sources in initial soils. Our study indicated that the main source of Pu is nuclear tests and that a second source with lower Pu ratio may come from weapons grade Pu (unexploded weapons grade Pu ie. material from bomb which didn't undergo nuclear explosions for example for security tests). Additionally, we found samples with high 238 Pu/ 239+240 Pu activity ratios and with typical global fallout 240 Pu/ 239 Pu atomic ratios, which are associated with separate sources of pure 238 Pu from the SNAP-9A satellite burn up in the atmosphere. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Vertical distribution of Pu radionuclides, 241Am and 99Sr in soil Samples from Romania

    International Nuclear Information System (INIS)

    Breban, D.; Mocanu, N.; Moreno-Bermudez, J.

    2002-01-01

    The investigated area is a natural alpine pasture located in the South chain of the Carpathian Mountains, which was found as one of the most contaminated areas in Romania after the Chernobyl accident.Radioactive concentrations of Pu radioisotopes, 2 41Am and 9 0Sr were determined in successive layers from 4 soil sections downward a depth of 6-8 cm, providing for the first time information on the effect of fallout acumulation of these radionuclides in soil samples from Romania. Pu and Am were separated by using a combined sequential procedure based on anion exchange and extraction chromatography. The measurements of 241Pu were performed by Liquid Scintillation Counting. 9 0Sr was determined by chemical separation of Sr using the classical precipitation method and Cerenkov counting of 9 0Y. For Quality Control IAEA reference materials were analyzed along with the samples. In a soil section of 8 cm depth radioactive inventories were approximately 500 Bq/m 2 for 2 41Pu, 115 Bq/m 2 for 2 39 +2 40Pu, 8 Bq/m 2 for 2 38Pu, 50 Bq/m2 for 2 41Am and 2500 Bq/m 2 for 9 0Sr. The data on each of the radioisotopes vertical distribution profile are compared between themselves and give an idea for their migration. On the basis of activity isotopic ratios in the soil depth profile, the origin of the contamination (Chernobyl accident and nuclear weapon test fallout) is discussed. The results are also compared to previous data on Cs-137

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-15

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

  16. Comparison of U-Pu-Mo, U-Pu-Nb, U-Pu-Ti and U-Pu-Zr alloys

    International Nuclear Information System (INIS)

    Boucher, R.; Barthelemy, P.

    1964-01-01

    The data concerning the U-Pu, U-Pu-Mo and U-Pu-Nb are recalled. The results obtained with U-Pu-Ti and U-Pu-Zr alloys containing 15-20 per cent Pu and 10 wt. per cent ternary element are reported. The transformation temperatures, the expansion coefficients, the nature of phases, the thermal cycling behaviour have been determined. A list of the principal properties of these different alloys is presented and the possibilities of their use as fast reactor's fuel element are considered. The U-Pu-Ti alloys seem to be quite promising: easiness of fabrication, large thermal stability, excellent behaviour in air, small quantity of zeta phase, temperature of solidus superior to 1100 deg. C. (authors) [fr

  17. 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

  18. High-precision isotopic characterization of USGS reference materials by TIMS and MC-ICP-MS

    Science.gov (United States)

    Weis, Dominique; Kieffer, Bruno; Maerschalk, Claude; Barling, Jane; de Jong, Jeroen; Williams, Gwen A.; Hanano, Diane; Pretorius, Wilma; Mattielli, Nadine; Scoates, James S.; Goolaerts, Arnaud; Friedman, Richard M.; Mahoney, J. Brian

    2006-08-01

    The Pacific Centre for Isotopic and Geochemical Research (PCIGR) at the University of British Columbia has undertaken a systematic analysis of the isotopic (Sr, Nd, and Pb) compositions and concentrations of a broad compositional range of U.S. Geological Survey (USGS) reference materials, including basalt (BCR-1, 2; BHVO-1, 2), andesite (AGV-1, 2), rhyolite (RGM-1, 2), syenite (STM-1, 2), granodiorite (GSP-2), and granite (G-2, 3). USGS rock reference materials are geochemically well characterized, but there is neither a systematic methodology nor a database for radiogenic isotopic compositions, even for the widely used BCR-1. This investigation represents the first comprehensive, systematic analysis of the isotopic composition and concentration of USGS reference materials and provides an important database for the isotopic community. In addition, the range of equipment at the PCIGR, including a Nu Instruments Plasma MC-ICP-MS, a Thermo Finnigan Triton TIMS, and a Thermo Finnigan Element2 HR-ICP-MS, permits an assessment and comparison of the precision and accuracy of isotopic analyses determined by both the TIMS and MC-ICP-MS methods (e.g., Nd isotopic compositions). For each of the reference materials, 5 to 10 complete replicate analyses provide coherent isotopic results, all with external precision below 30 ppm (2 SD) for Sr and Nd isotopic compositions (27 and 24 ppm for TIMS and MC-ICP-MS, respectively). Our results also show that the first- and second-generation USGS reference materials have homogeneous Sr and Nd isotopic compositions. Nd isotopic compositions by MC-ICP-MS and TIMS agree to within 15 ppm for all reference materials. Interlaboratory MC-ICP-MS comparisons show excellent agreement for Pb isotopic compositions; however, the reproducibility is not as good as for Sr and Nd. A careful, sequential leaching experiment of three first- and second-generation reference materials (BCR, BHVO, AGV) indicates that the heterogeneity in Pb isotopic compositions

  19. Biodegradation of PuEDTA and Impacts on Pu Mobility

    International Nuclear Information System (INIS)

    Xun, Luying; Bolton, Jr. Harvey

    2001-01-01

    Ethylenediaminetetraacetate (EDTA) and nitrilotriacetate (NTA) are synthetic chelating agents, which can form strong water-soluble complexes with radionuclides and metals and has been used to decontaminate and process nuclear materials. Synthetic chelating agents were co-disposed with radionuclides (e.g., 60Co, Pu) and heavy metals enhancing their transport in the subsurface. An understanding of EDTA biodegradation is essential to help mitigate enhanced radionuclide transport by EDTA. The objective of this research is to develop fundamental data on factors that govern the biodegradation of radionuclide-EDTA. These factors include the dominant EDTA aqueous species, the biodegradation of various metal-EDTA complexes, the uptake of various metal-EDTA complexes into the cell, the distribution and mobility of the radionuclide during and after EDTA biodegradation, and the enzymology and genetics of EDTA biodegradation

  20. 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)

  1. River bottom sediment from the Vistula as matrix of candidate for a new reference material.

    Science.gov (United States)

    Kiełbasa, Anna; Buszewski, Bogusław

    2017-08-01

    Bottom sediments are very important in aquatic ecosystems. The sediments accumulate heavy metals and compounds belonging to the group of persistent organic pollutants. The accelerated solvent extraction (ASE) was used for extraction of 16 compounds from PAH group from bottom sediment of Vistula. For the matrix of candidate of a new reference material, moisture content, particle size, loss on ignition, pH, and total organic carbon were determined. A gas chromatograph with a selective mass detector (GC/MS) was used for the final analysis. The obtained recoveries were from 86% (SD=6.9) for anthracene to 119% (SD=5.4) for dibenzo(ah)anthracene. For the candidate for a new reference material, homogeneity and analytes content were determined using a validated method. The results are a very important part of the development and certification of a new reference materials. Copyright © 2017 Elsevier Inc. All rights reserved.

  2. Combating illicit trafficking in nuclear and other radioactive material. Reference material

    International Nuclear Information System (INIS)

    2007-01-01

    This publication is intended for individuals and organizations that may be called upon to deal with the detection of and response to criminal or unauthorized acts involving nuclear or other radioactive material. It will also be useful for legislators, law enforcement agencies, government officials, technical experts, lawyers, diplomats and users of nuclear technology. This manual emphasizes the international initiatives for improving the security of nuclear and other radioactive material. However, it is recognized that effective measures for controlling the transfer of equipment, non-nuclear material, technology or information that may assist in the development of nuclear explosive devices, improvised nuclear devices (INDs) or other radiological dispersal devices (RDDs) are important elements of an effective nuclear security system. In addition, issues of personal integrity, inspection and investigative procedures are not discussed in this manual, all of which are essential elements for an effective overall security system. The manual considers a variety of elements that are recognized as being essential for dealing with incidents of criminal or unauthorized acts involving nuclear and other radioactive material. Depending on conditions in a specific State, including its legal and governmental infrastructure, some of the measures discussed will need to be adapted to suit that State's circumstances. However, much of the material can be applied directly in the context of other national programmes. This manual is divided into four main parts. Section 2 discusses the threat posed by criminal or unauthorized acts involving nuclear and other radioactive material, as well as the policy and legal bases underlying the international effort to restrain such activities. Sections 3 and 4 summarize the major international undertakings in the field. Sections 5-8 provide some basic technical information on radiation, radioactive material, the health consequences of radiation

  3. The use of high accuracy NAA for the certification of NIST botanical standard reference materials

    International Nuclear Information System (INIS)

    Becker, D.A.; Greenberg, R.R.; Stone, S.F.

    1992-01-01

    Neutron activation analysis is one of many analytical techniques used at the National Institute of Standards and Technology (NIST) for the certification of NIST Standard Reference Materials (SRMs). NAA competes favorably with all other techniques because of it's unique capabilities for high accuracy even at very low concentrations for many elements. In this paper, instrumental and radiochemical NAA results are described for 25 elements in two new NIST SRMs, SRM 1515 (Apple Leaves) and SRM 1547 (Peach Leaves), and are compared to the certified values for 19 elements in these two new botanical reference materials. (author) 7 refs.; 4 tabs

  4. Use of reference materials for quality control of elemental analysis by neutron activation with radiochemical separation

    International Nuclear Information System (INIS)

    Woittiez, J.R.W.

    1990-01-01

    This paper describes the use of certified reference materials to monitor the long-term quality of radiochemical separations. The practical limitations which determine the actual design of the quality control are discussed. The hypothesis that the high yield of the radiochemical separation will be constant with time has been checked and validated for the elements Zn, Fe, Co, Cd, Mo and to a lesser extent for W and Th using NBS SRM 1577A, BCR CRM 274 and IAEA RM A-11. This validation could not be made for the elements Cr, Au, and Ag. Especially for Cr there is a serious lack of appropiate certified reference materials. (orig.)

  5. 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.

  6. 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

  7. USTUR Whole Body Case 0262: 33-y Follow-up of PuO2 In A Skin Wound and Associated Axillary Node

    Energy Technology Data Exchange (ETDEWEB)

    James, Anthony C.; Sasser, Lyle B.; Stuit, Dorothy B.; Wood, T. G.; Glover, Samuel E.; Lynch, Timothy P.; Dagle, Gerald E.

    2008-01-28

    This whole body donation case (USTUR Registrant) involved two suspected plutonium oxide (Pu) inhalation intakes, each indicated by a measurable Pu alpha activity in a single urine sample, followed about 1.5 y later by a puncture wound to the thumb while working in a Pu glovebox. The study is concerned with modeling simultaneously the biokinetics of deposition and retention in the respiratory tract and at the wound site; and the biokinetics of Pu subsequently transferred to other body organs, until the donor's death. Urine samples taken after the wound incident had readily measurable Pu alpha activity over the next 14 y, before dropping below the minimum detectable excretion rate (<0.4 mBq per day). The Registrant died about 33 y after the wound intake, at the age of 71, from hepatocellular carcinoma with extensive metastases. At autopsy, all major soft tissue organs were harvested for analysis of their Pu-238, Pu-239+240 and Am-241 content. The amount of Pu-239+240 retained at the wound site was 68 ± 7 Bq (1 SD), measured by low-energy planar Ge spectrometry. A further 56.0 ± 1.2 Bq was retained in an associated axillary lymph node, measured by radiochemistry. Simultaneous mathematical analysis (modelling) of all in vivo urinary excretion data, together with the measured lung, thoracic lymph node, wound, axillary lymph node and systemic tissue contents at death, yielded estimated intake amounts of 757 and 1504 Bq, respectively, for the first and second inhalation incidents, and 204 Bq for the total wound intake. The inhaled Pu material was highly insoluble, with an estimated long-term absorption rate from the lungs of 2 E-5 per day. The Pu material deposited at the wound site was mixed: 14% was rapidly absorbed, 49% was absorbed at the rate of about 6E-5 per day, and the remainder ( 37%) was absorbed extremely slowly (at the rate of about 5E-6 per day). Thus, it was estimated that only 40% of the Pu initially deposited in the wound had been absorbed

  8. USTUR whole body case 0262: 33-y follow-up of PuO{sub 2} in a skin wound and associated axillary node

    Energy Technology Data Exchange (ETDEWEB)

    James, A.C.; Sasser, L.B.; Stuit, D.B.; Wood, T.G. [U.S. Transuranium and Uranium Registries, College of Pharmacy, Washington State University, 1845 Terminal Drive, Suite 201, Richland, WA 99354 (United States); Glover, S.E. [Department of Mechanical, Industrial and Nuclear Engineering, University of Cincinnati, 598 Rhodes Hall, Cincinnati, OH 45221 (United States); Lynch, T.P. [Pacific Northwest National Laboratory, PO Box 999, Richland, WA 99354 (United States); Dagle, G.E. [2543 Harris Avenue, Richland, WA 99354 (United States)

    2007-07-01

    This whole body donation case (USTUR Registrant) involved two suspected PuO{sub 2} inhalation intakes, each indicated by a measurable Pu alpha activity in a single urine sample, followed about 1 1/2 y later by a puncture wound to the thumb while working in a Pu glovebox. The study is concerned with modelling simultaneously the biokinetics of deposition and retention in the respiratory tract and at the wound site; and the biokinetics of Pu subsequently transferred to other body organs, until the donor's death. Urine samples taken after the wound incident had readily measurable Pu alpha activity over the next 14 y, before dropping below the minimum detectable excretion rate (<0.4 mBq d{sup -1}). The Registrant died about 33 y after the wound intake, at the age of 71, from hepatocellular carcinoma with extensive metastases. At autopsy, all major soft tissue organs were harvested for analysis of their {sup 238}Pu, {sup 239+240}Pu and {sup 241}Am content. The amount of {sup 239+240}Pu retained at the wound site was 68{+-}7 Bq (1 SD), measured by low-energy planar Ge spectrometry. A further 56.0{+-}1.2 Bq was retained in an associated axillary lymph node, measured by radiochemistry. Simultaneous mathematical analysis (modelling) of all in vivo urinary excretion data, together with the measured lung, thoracic lymph node, wound, axillary lymph node and systemic tissue contents at death, yielded estimated intake amounts of 757 and 1504 Bq, respectively, for the first and second inhalation incidents, and 204 Bq for the total wound intake. The inhaled Pu material was highly insoluble, with an estimated long-term absorption rate from the lungs of 2 x 10{sup -5} d{sup -1}. The Pu material deposited at the wound site was mixed: {approx}14% was rapidly absorbed, {approx}49% was absorbed at the rate of about 6 x 10{sup -5} d{sup -1}, and the remainder ({approx}37%) was absorbed extremely slowly (at the rate of about 5 x 10{sup -6} d{sup -1}). Thus, it was estimated that only

  9. 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)

  10. Certified reference materials for the determination of mineral oil hydrocarbons in water, soil and waste

    Energy Technology Data Exchange (ETDEWEB)

    Koch, M.; Liebich, A.; Win, T.; Nehls, I.

    2005-07-01

    The international research project HYCREF, funded by the European Commission in the 5{sup th} Framework programme, aimed to develop methods to prepare homogeneous and stable water-, soil- and waste reference materials contaminated with mineral oil hydrocarbons and to test certify the mineral oil content by gas chromatographic methods. As mineral oil products are important sources for environmental contaminations a high need exists for certified reference materials for their determination using the new gas chromatographic methods (soil: ISO/FDIS 16703, waste: ENpr 14039, water: ISO 9377-2). The experimental conditions and results for preparation and characterisation of a total of nine reference materials (3 water, 3 soil- and 3 waste materials) are described and discussed. Target values for the reference materials were defined at the beginning of the project in order to have clear quality criteria, which could be compared with the achieved results at the end of the project. These target specifications were related to the maximum uncertainty from test certification exercises (<5% for soil/waste and <10% for water), the maximum inhomogeneity between bottles (<3%) and minimum requirements for stability (>5 years for soil/waste and >2 years for water). The feasibility studies showed that solid materials (soil, waste) could be prepared sufficiently homogeneous and stable. The test certified values of the 6 solid materials comprise a wide range of mineral oil content from about 200-9000 mg/kg with expanded uncertainties between 5.7-13.1% using a coverage factor k (k=2). The development of new water reference materials - the so-called ''spiking pills'' for an offshore- and a land-based discharge water represents one of the most innovative aspects of the project. The spiking pill technology facilitates the application and storage and improves the material stability compared with aqueous materials. Additional to the preparation and test certification of

  11. Assessment of international reference materials for isotope-ratio analysis (IUPAC Technical Report)

    Science.gov (United States)

    Brand, Willi A.; Coplen, Tyler B.; Vogl, Jochen; Rosner, Martin; Prohaska, Thomas

    2014-01-01

    Since the early 1950s, the number of international measurement standards for anchoring stable isotope delta scales has mushroomed from 3 to more than 30, expanding to more than 25 chemical elements. With the development of new instrumentation, along with new and improved measurement procedures for studying naturally occurring isotopic abundance variations in natural and technical samples, the number of internationally distributed, secondary isotopic reference materials with a specified delta value has blossomed in the last six decades to more than 150 materials. More than half of these isotopic reference materials were produced for isotope-delta measurements of seven elements: H, Li, B, C, N, O, and S. The number of isotopic reference materials for other, heavier elements has grown considerably over the last decade. Nevertheless, even primary international measurement standards for isotope-delta measurements are still needed for some elements, including Mg, Fe, Te, Sb, Mo, and Ge. It is recommended that authors publish the delta values of internationally distributed, secondary isotopic reference materials that were used for anchoring their measurement results to the respective primary stable isotope scale.

  12. Sorption of Pu onto some kinds of clay

    International Nuclear Information System (INIS)

    Jia Haihong; Si Gaohua; Liu Wei; Yu Jing

    2010-01-01

    There are rich clay mines holding in one area, so it's necessary to know about these clays' sorption capacity to Pu, for building radioactive waste repository in the area. Distribution coefficients of Pu onto different clays were acquired in static method, with the result about 104. The size of clay is different, but the result of Kds is near. In addition, it's estimated how far Pu moves in the most rapid speed in the clay based on these Kids', disregarding the influence of Pu-colloid. In a word, as a kind of backfilling material clays in the area can effectively prevent Pu from moving to environment, and when designing the backfilling layer, it's not necessary to catch clays through NO.200 sieve, if only considering the influence of Kd. (authors)

  13. NDA PDP Program PuO2 increased particle size specification and design

    International Nuclear Information System (INIS)

    Marshall, R.S.; Taggart, D.P.; Becker, G.K.; Woon, W.Y.

    1996-01-01

    Provisions in the National TRU Program Quality Assurance Program Plan require an assessment of performance for nondestructive waste assay (NDA) systems employed in the program. This requirement is in part fulfilled through the use of Performance Demonstration programs. In order to optimize the quality and quantity of information acquired during a given Performance Demonstration Program cycle, the assessment employed is to be carefully specified and designed. The assessment must yield measurement system performance data meaningful with respect to NDA system capability to accommodate attributes of interest known to occur in actual waste forms. The design and specification of the increased particle size PuO 2 PDP working reference materials (WRMs) is directed at providing a straightforward mechanism to assess waste NDA system capability to account for biases introduced by large PuO 2 particles. The increased particle size PuO 2 PDP WRM design addresses actual waste form attributes associated with PuO 2 particle size and distributions thereof, the issue of a known and stable WRM configuration and equally important appropriate certification and tractability considerations

  14. A feasibility study for producing an egg matrix candidate reference material for the polyether ionophore salinomycin.

    Science.gov (United States)

    Ferreira, Rosana Gomes; Monteiro, Mychelle Alves; Pereira, Mararlene Ulberg; da Costa, Rafaela Pinto; Spisso, Bernardete Ferraz; Calado, Veronica

    2016-08-01

    The aim of this work was to study the feasibility of producing an egg matrix candidate reference material for salinomycin. Preservation techniques investigated were freeze-drying and spray drying dehydration. Homogeneity and stability studies of the produced batches were conducted according to ISO Guides 34 and 35. The results showed that all produced batches were homogeneous and both freeze-drying and spray drying techniques were suitable for matrix dehydrating, ensuring the material stability. In order to preserve the material integrity, it must be transported within the temperature range of -20 up to 25°C. The results constitute an important step towards the development of an egg matrix reference material for salinomycin is possible. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Evaluation of botanical reference materials for the determination of vanadium in biological samples

    International Nuclear Information System (INIS)

    Heydorn, K.; Damsgaard, E.

    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 chemical or radiochemical separations, and results for vanadium were compared with those found by purely instrumental neutron activation analysis. Significantly lower results indicate losses or incomplete dissolution, which makes SRM 1575 Pine Needles and SRM 1573 Tomato Leaves less satisfactory than SRM 1570 Spinach. 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. (author)

  16. Inhaled 239PuO2 in rats with pulmonary emphysema

    International Nuclear Information System (INIS)

    Lundgren, D.L.; Mauderly, J.L.; Hahn, F.F.

    1984-01-01

    The modifying effects of a pre-existing lung disease (emphysema) on the deposition, distribution, retention, and effects of inhaled 239 PuO 2 in the rat are being investigated. Preliminary observations indicated that the deposition and retention patterns for 239 Pu particles inhaled by rats with emphysema and control rats were similar, but the distribution of inhaled 239 Pu immediately after exposure was different. Respiratory function measured through one year after exposure to 239 Pu was consistent with emphysema and was not altered by the 239 Pu lung burden. Long-term observations are continuing. 4 references, 2 tables

  17. Importance of 241 Am Determination in the Characterization of PuO2 Standards for Calorimetric Assay.

    Energy Technology Data Exchange (ETDEWEB)

    Sampson, Thomas E.

    2005-01-01

    Plutonium dioxide (PuO{sub 2}) standards are often used both as heat standards and isotopic standards for calorimetric assay. Calorimetric assay is the combination of the power in watts measured in a calorimeter with the effective specific power (P{sub eff}) in watts/g Pu, determined either by nondestructive gamma-ray assay or by destructive mass spectrometry, to yield the total elemental plutonium mass in the sample. To use a PuO{sub 2} sample as a heat standard for calorimetry, one must determine both the plutonium mass and P{sub eff} with very small uncertainties and then calculate the sample watts from the known plutonium mass, specific powers, and isotopic composition. Well-characterized PuO{sub 2} standards have plutonium mass values determined by analytical chemistry with a precision and accuracy on the order of 0.1%-0.2% relative to the total mass of the sample. Mass spectrometry, typically used to determine the isotopic fractions of plutonium standards, is very accurate and precise for the major isotopes but is somewhat less precise for low-abundance isotopes. The characterization of the {sup 241}Am/Pu ratio in the standard is also of great importance because {sup 241}Am can contribute significantly to P{sub eff} and to the heat output of the standard. The determination of the {sup 241}Am/Pu ratio in a plutonium-bearing sample is a process that is less standardized than mass spectrometry. There are no certified reference materials (CRMs) traceable to the national measurement system for {sup 241}Am in plutonium, and routine analytical {sup 241}Am/Pu ratio measurements often exhibit uncertainties of several percent relative to the total plutonium or greater.

  18. Preparation and certification of a uranium isotope certified reference material JAERI-U5

    International Nuclear Information System (INIS)

    Tamura, Shuzo; Hashitani, Hiroshi

    1982-06-01

    The Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI had planned to prepare a new reference material, JAERI-U5 for uranium isotopic measurement since 1978. The reference material is composed of 6 samples of different enrichment in the range of 0.2 to 4.5 wt. percents of 235 U. The preparation includes dissolution of raw materials, blending of solutions, precipitation of ammonium diuranate, drying and ignition to U 3 O 8 . A mass-spectrometric collaborative analysis was carried out by well-trained two laboratories in this country, JAERI and PNC. The certified values were decided from the result of the collaborative work. As the measurements were based on NBS SRM's, JAERI-U5 should be called tertiary standard. The materials are packed in bottles of low-potassium-content glass for a possible use in non-destructive gamma-rays spectrometry. The reference material has been distributing from JAERI with a price of yen 140,000 per set (6 samples of 2 g of each) since 1979. (author)

  19. IAEA Reference Materials for Quality Assurance: A Study in the Quality Control of Marine Radioactivity

    International Nuclear Information System (INIS)

    Pham Mai Khanh; Bartocci, J.; Gastaud, J.; Nies, H.; Vasileva, E.; Betti, M.; Chamizo, E.; Gomez-Guzman, J.-M.

    2013-01-01

    The IAEA's Marine Environment Laboratories has assisted laboratories in Analytical Quality Control Services (AQCS) for the analysis of radionuclides in the marine environment since the early seventies. The AQCS programme, now named Reference Products for Environment and Trade, is recognized as an essential component of quality assurance and control and for the development and validation of analytical methods, through its worldwide and regional interlaboratory comparisons and the provision of reference methods and Reference Materials/Certified Reference Materials (RMs/CRMs). A total of 49 interlaboratory exercises were organized and 42 RMs/CRMs were produced for marine radioactivity studies. Different techniques such as radiometric methods with X ray, gamma spectrometry, alpha spectrometry, beta counter, liquid scintillation counter as well as mass spectrometry (ICP-MS, AMS, TIMS) are applied for the characterization during certification process. An overview of prepared Certified Reference Materials (CRMs) for radionuclides in marine matrices will be presented as well as lessons learned from interlaboratory comparisons (ICs) and Proficiency Tests (PTs). A characterization of a new CRM for radionuclides in IAEA-446, Baltic Sea seaweed (Fucus vesiculosus), as well as a specific case of using Accelerator Mass Spectrometry (AMS) technique to characterize I-129 in sea water (IAEA-418) and seaweed sample (IAEA-446), will be discussed. Available RMs/CRMs are listed and can be ordered and purchased through the IAEA website http://nucleus.iaea.org/rpst/. (author)

  20. IAEA Reference Materials for Quality Assurance: A Study in the Quality Control of Marine Radioactivity

    Energy Technology Data Exchange (ETDEWEB)

    Khanh, Pham Mai; Bartocci, J.; Gastaud, J.; Nies, H.; Vasileva, E.; Betti, M. [International Atomic Energy Agency, Environment Laboratory (Monaco); Chamizo, E.; Gomez-Guzman, J. -M. [Centro Nacional de Aceleradores, Seville (Spain)

    2013-07-15

    The IAEA's Marine Environment Laboratories has assisted laboratories in Analytical Quality Control Services (AQCS) for the analysis of radionuclides in the marine environment since the early seventies. The AQCS programme, now named Reference Products for Environment and Trade, is recognized as an essential component of quality assurance and control and for the development and validation of analytical methods, through its worldwide and regional interlaboratory comparisons and the provision of reference methods and Reference Materials/Certified Reference Materials (RMs/CRMs). A total of 49 interlaboratory exercises were organized and 42 RMs/CRMs were produced for marine radioactivity studies. Different techniques such as radiometric methods with X ray, gamma spectrometry, alpha spectrometry, beta counter, liquid scintillation counter as well as mass spectrometry (ICP-MS, AMS, TIMS) are applied for the characterization during certification process. An overview of prepared Certified Reference Materials (CRMs) for radionuclides in marine matrices will be presented as well as lessons learned from interlaboratory comparisons (ICs) and Proficiency Tests (PTs). A characterization of a new CRM for radionuclides in IAEA-446, Baltic Sea seaweed (Fucus vesiculosus), as well as a specific case of using Accelerator Mass Spectrometry (AMS) technique to characterize I-129 in sea water (IAEA-418) and seaweed sample (IAEA-446), will be discussed. Available RMs/CRMs are listed and can be ordered and purchased through the IAEA website http://nucleus.iaea.org/rpst/. (author)

  1. Two 238Pu inhalation incidents

    International Nuclear Information System (INIS)

    Fleming, R.R.; Hall, R.M.

    1978-06-01

    Two employees inhaled significant amounts of 238 Pu in separate unrelated contamination incidents in 1977. Both acute exposure incidents are described and the urine, feces, and in-vivo chest count data for each employee. Case B ( 238 PuNO 3 ) received 24 DTPA treatments beginning the day of the incident while, for medical reasons, Case A ( 238 PuO 2 ) received no therapy

  2. Normalization Methods and Selection Strategies for Reference Materials in Stable Isotope Analyses - Review

    International Nuclear Information System (INIS)

    Skrzypek, G.; Sadler, R.; Paul, D.; Forizs, I.

    2011-01-01

    A stable isotope analyst has to make a number of important decisions regarding how to best determine the 'true' stable isotope composition of analysed samples in reference to an international scale. It has to be decided which reference materials should be used, the number of reference materials and how many repetitions of each standard is most appropriate for a desired level of precision, and what normalization procedure should be selected. In this paper we summarise what is known about propagation of uncertainties associated with normalization procedures and propagation of uncertainties associated with reference materials used as anchors for the determination of 'true' values for δ''1''3C and δ''1''8O. Normalization methods Several normalization methods transforming the 'raw' value obtained from mass spectrometers to one of the internationally recognized scales has been developed. However, as summarised by Paul et al. different normalization transforms alone may lead to inconsistencies between laboratories. The most common normalization procedures are: single-point anchoring (versus working gas and certified reference standard), modified single-point normalization, linear shift between the measured and the true isotopic composition of two certified reference standards, two-point and multipoint linear normalization methods. The accuracy of these various normalization methods has been compared by using analytical laboratory data by Paul et al., with the single-point and normalization versus tank calibrations resulting in the largest normalization errors, and that also exceed the analytical uncertainty recommended for δ 13 C. The normalization error depends greatly on the relative differences between the stable isotope composition of the reference material and the sample. On the other hand, the normalization methods using two or more certified reference standards produces a smaller normalization error, if the reference materials are bracketing the whole range of

  3. IRMM Certified Reference Materials and k0-NAA: an important role for the future

    International Nuclear Information System (INIS)

    Robouch, P.; Arana, G.; Pauwels, J.; Pomm, S.

    1998-01-01

    The k 0 -Neutron Activation Analysis method was introduced at the Institute for Reference Materials and Measurements (IRMM) and the Belgian nuclear research centre (SCK CEN) in 1994. This analytical technique is routinely used at IRMM for the production control, homogeneity and stability tests and/or for certification of metallic, biological and environmental reference materials. The successful implementation of k 0 -NAA was proven at several certification exercises - such as ISS Antarctic Sediment, BCR Mussel Tissue and BCR Bovine Liver, SMU Bovine Blood - where all our results were accepted for certification. Responding to regulatory and/or scientific demands, IRMM is collaborating with national institutes to develop new high quality reference materials: (i) in the field of Neutron dosimetry: high purity nickel, Al-Ag or Zr-Au-Lu alloys; (ii) for environmental and industrial monitoring: Antarctic krill, doped plastics or catalytic converters; (iii) synthetic multi-element standard for the accreditation of k 0 -NAA laboratories. Far from being exhaustive, this list highlights the important role that k 0 -NAA will play in the certification of reference materials in the years 2000. (author)

  4. 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)

  5. Compilation of elemental concentration data for NBS Biological and Environmental Standard Reference Materials

    International Nuclear Information System (INIS)

    Gladney, E.S.

    1980-07-01

    Concentration data on up to 76 elementals in 19 NBS Standard Reference Materials have been collected from 325 journal articles and technical reports. These data are summarized into mean +- one standard deviation values and compared with available data from NBS and other review articles. Data are presented on the analytical procedures employed and all raw data are presented in appendixes

  6. Speciation of dimethylarsinyl-riboside derivatives (arsenosugars) in marine reference materials by HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt

    1995-01-01

    (cf. Table 2) were present in shellfish certified reference materials (CRMs) and in a lobster hepatopancreas CRM. The concentration of the two arsenosugars in the shellfish samples amounts to 18% of the total arsenic as compared to arsenobetaine at 9–13% and dimethylarsinate at 4–9% of the total...

  7. An independent accurate reference method for the determination of chromium in biological materials

    NARCIS (Netherlands)

    Lagerwaard, A.; Woittiez, J.R.W.; de Goeij, J.J.M.

    1994-01-01

    A method for the determination of Cr in biological materials with high accuracy is reported for use as an independent reference method. It is based on radiochemical neutron activation analysis (RNAA) in combination with an individual yield determination based on the online yield principle. A

  8. Doorways III: Teacher Reference Materials. On School-Related Gender-Based Violence Prevention and Response

    Science.gov (United States)

    US Agency for International Development, 2009

    2009-01-01

    The Doorways training program was designed by the U.S. Agency for International Development (USAID)-funded Safe Schools Program (Safe Schools) to enable teachers, community members and students to prevent and respond to school-related gender-based violence (SRGBV). This booklet, "Doorways III: Teacher Reference Materials on School-Related…

  9. Instrumental neutron and photon activation analyses of selected geochemical reference materials

    Czech Academy of Sciences Publication Activity Database

    Mizera, Jiří; Řanda, Zdeněk

    2010-01-01

    Roč. 284, č. 1 (2010), s. 157-163 ISSN 0236-5731 R&D Projects: GA AV ČR IAA300130706 Institutional research plan: CEZ:AV0Z10480505 Keywords : neutron activation analysis * photon activation analysis * geochemical reference materials Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 0.777, year: 2010

  10. Instrumental neutron and photon activation analyses of selected geochemical reference materials

    Czech Academy of Sciences Publication Activity Database

    Mizera, Jiří; Řanda, Z.

    2010-01-01

    Roč. 284, č. 1 (2010), s. 157-163 ISSN 0236-5731 Institutional research plan: CEZ:AV0Z30460519 Keywords : neutron activation analysis * photon activation analysis * geochemical reference materials Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders OBOR OECD: Analytical chemistry Impact factor: 0.777, year: 2010

  11. Reference material certification of chinese cabbage composition for selenium, nitrogen, phosphorus and potassium content

    Directory of Open Access Journals (Sweden)

    D. A. Chupakhin

    2016-01-01

    Full Text Available Rationale. The reference material of composition with the established metrological characteristics including a certified value and an expanded uncertainty is necessary to ensure an effective accuracy and precision control of results of element composition determination in food ingredients and products. This paper represents the development of a reference material of food crop composition for selenium, nitrogen, phosphorus and potassium content. Methods. To identify the selenium the hybrid atomic absorption method was used, to identify the nitrogen and phosphorus the photometric method was used, to determine the potassium flame-photometric method was used. When determining the metrological characteristics of the reference material the Russian national instructions and recommendations MI 3174-2009 and P 50.2.058-2007 were applied. Results. Based on the research findings the reference material of Chinese cabbage composition with a certified value and an expanded uncertainty was developed: for selenium 0.044 ± 0.017 mg/kg; for nitrogen 4.09 ± 0.27 %; for phosphorus 0.69 ± 0.14 %; for potassium 2.87 ± 0.22 %.

  12. Determination of trace elements in standard reference materials by the ko-standardization method

    International Nuclear Information System (INIS)

    Smodis, B.; Jacimovic, R.; Stegnar, P.; Jovanovic, S.

    1990-01-01

    The k o -standardization method is suitable for routine multielement determinations by reactor neutron activation analysis (NAA). Investigation of NIST standard reference materials SRM 1571 Orchard Leaves, SRM 1572 Citrus leaves, and SRM 1573 Tomato Leaves showed the systematic error of 12 certified elements determined to be less than 8%. Thirty-four elements were determined in NIST proposed SRM 1515 Apple Leaves

  13. Intercomparison of enriched stable isotope reference materials for medical and biological studies

    International Nuclear Information System (INIS)

    Parr, R.M.; Clements, S.A.

    1991-01-01

    This report summarizes the results of an intercomparison exercise organized by the IAEA during the latter part of 1988 and 1989. Data are presented for 13 different kinds of enriched stable isotope reference material containing 2 H, 13 C, 15 N and 18 O. Results were submitted by forty participants in twenty countries. 2 refs, 13 figs, 18 tabs

  14. Analysis of marine sediment and lobster hepatopancreas reference materials by instrumental photon activation

    International Nuclear Information System (INIS)

    Landsberger, S.; Davidson, W.F.

    1985-01-01

    By use of instrumental photon activation analysis, twelve trace (As, Ba, Cr, Co, Mn, Ni, Pb, Sb, Sr, U, Zn, and Zr) and eight minor (C, Na, Mg, Co, K, Ca, Tl, and Fe) elements were determined in a certified marine sediment standard reference material as well as eight trace (Mn, Ni, Cu, Zn, As, Sr, Cd, and Pb) and four minor (Na, Mg, Cl, and Ca) elements in a certified marine tissue (lobster hepatopancreas) standard reference material. The precision and accuracy of the present results when compared to the accepted values clearly demonstrate the reliability of this nondestructive technique and its applicability to marine environmental or marine geochemical studies. 24 references, 4 figures, 3 tables

  15. Biodegradation of PuEDTA and Impacts on Pu Mobility

    International Nuclear Information System (INIS)

    Bolton, H. Jr.; Rai, D.; Xun, L.

    2004-01-01

    The contamination of many DOE sites by Pu presents a long-term problem because of its long half-life (240,000 yrs) and the low drinking water standard ( -12 M). EDTA was co-disposed with radionuclides (e.g., Pu, 60 Co), formed strong complexes, and enhanced radionuclide transport at several DOE sites. Biodegradation of EDTA should decrease Pu mobility. One objective of this project was to determine the biodegradation of EDTA in the presence of PuEDTA complexes. The aqueous system investigated at pH 7 (10 -4 M EDTA and 10 -6 M Pu) contained predominantly Pu(OH) 2 EDTA 2- . The EDTA was degraded at a faster rate in the presence of Pu. As the total concentration of both EDTA and PuEDTA decreased (i.e., 10 -5 M EDTA and 10 -7 M PuEDTA), the presence of Pu decreased the biodegradation rate of the EDTA. It is currently unclear why the concentration of Pu directly affects the increase/decrease in rate of EDTA biodegradation. The soluble Pu concentration decreased, in agreement with thermodynamic predictions, as the EDTA was biodegraded, indicating that biodegradation of EDTA will decrease Pu mobility when the Pu is initially present as Pu(IV)EDTA. A second objective was to investigate how the presence of competing metals, commonly encountered in geologic media, will influence the speciation and biodegradation of Pu(IV)-EDTA. Studies on the solubilities of Fe(OH) 3 (s) and of Fe(OH) 3 (s) plus PuO 2 (am) in the presence of EDTA and as a function of pH showed that Fe(III) out competes the Pu(IV) for the EDTA complex, thereby showing that Pu(IV) will not form stable complexes with EDTA for enhanced transport of Pu in Fe(III) dominated subsurface systems. A third objective is to investigate the genes and enzymes involved in EDTA biodegradation. BNC1 can use EDTA and another synthetic chelating agent nitrilotriacetate (NTA) as sole carbon and nitrogen sources. The same catabolic enzymes are responsible for both EDTA and NTA degradation except that additional enzymes are

  16. Certification of a plutonium dioxide reference material for elemental analyses (EC-NRM 210)

    International Nuclear Information System (INIS)

    Le Duigou, Y.

    1990-01-01

    A new EC plutonium reference material is made available in the form of 5g samples of plutonium dioxide powder. Before weighing the material must be calcined at 1 250 0 C for two hours. The plutonium content (880.26 ± 0.44) g.kg -1 has been derived from plutonium measurements performed by three different laboratories each applying a different oxydo-reductive method. The results of the plutonium measurement, the statistical evaluation of the uncertainty of the plutonium content together with information on the impurities present in the material are given in the report

  17. Experimental Benchmarking of Pu Electronic Structure

    International Nuclear Information System (INIS)

    Tobin, J.G.; Moore, K.T.; Chung, B.W.; Wall, M.A.; Schwartz, A.J.; Ebbinghaus, B.B.; Butterfield, M.T.; Teslich, N.E. Jr.; Bliss, R.A.; Morton, S.A.; Yu, S.W.; Komesu, T.; Waddill, G.D.; van der Laan, G.; Kutepov, A.L.

    2008-01-01

    The standard method to determine the band structure of a condensed phase material is to (1) obtain a single crystal with a well defined surface and (2) map the bands with angle resolved photoelectron spectroscopy (occupied or valence bands) and inverse photoelectron spectroscopy (unoccupied or conduction bands). Unfortunately, in the case of Pu, the single crystals of Pu are either nonexistent, very small and/or having poorly defined surfaces. Furthermore, effects such as electron correlation and a large spin-orbit splitting in the 5f states have further complicated the situation. Thus, we have embarked upon the utilization of unorthodox electron spectroscopies, to circumvent the problems caused by the absence of large single crystals of Pu with well-defined surfaces. Our approach includes the techniques of resonant photoelectron spectroscopy, x-ray absorption spectroscopy, electron energy loss spectroscopy, Fano Effect measurements, and Bremstrahlung Isochromat Spectroscopy, including the utilization of micro-focused beams to probe single-crystallite regions of polycrystalline Pu samples.

  18. Certification of a meat reference material based on a collaborative study

    Directory of Open Access Journals (Sweden)

    Claudia Marcela Salazar Arzate

    2013-01-01

    Full Text Available Through a collaborative project, comparison studies were carried out to improve measurement capabilities of participating laboratories, supporting them to produce, characterize and distribute reference materials in the food sector. The project was planned in four annual stages (milk, water, meat and grains. The third stage aimed specifically to quantify and certify the nutritional content of the parameters (nitrogen, fat, sodium and potassium of a batch candidate as Certified Reference Material (CRM of canned beef. This study was conducted in collaboration between several National Metrology Institutes (NMIs and/or collaborating laboratories, which, once identified the possible causes of variability or bias in the measurements, as well as the opportunities of improvement, achieved the certification of the material beef. The CRM was distributed among the participants to cover the needs of the food industry of meat products and testing laboratories in their respective countries.

  19. Aluminium-gold reference material for the k0-standardisation of neutron activation analysis

    International Nuclear Information System (INIS)

    Ingelbrecht, C.; Peetermans, F.; Corte, F. de; Wispelaere, A. de; Vandecasteele, C.; Courtijn, E.; Hondt, P. d'

    1991-01-01

    Gold is an excellent comparator material for the k 0 -standardisation of neutron activation analysis because of its convenient and well defined nuclear properties. The most suitable form for a reference material is a dilute aluminium-gold alloy, for which the self-shielding effect for neutrons is small. Castings of composition Al-0.1 wt.% Au were prepared by crucible-less levitation melting, which gives close control of ingot composition with minimal contamination of the melt. The alloy composition was checked using induction-coupled plasma source emission spectrometry. The homogeneity of the alloy was measured by neutron activation analysis and a relative standard deviation of the gold content of 0.30% was found (10 mg samples). Metallography revealed a homogeneous distribution of AuAl 2 particles. The alloy was certified as Reference Materials CBNM-530, with certified gold mass fraction 0.100±0.002 wt.%. (orig.)

  20. 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.

  1. Determination of cadmium, lead and zinc in a candidate reference materials using isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Munoz, Luis; Gras, Nuri; Quejido, Alberto; Fernandez, Marta

    2001-01-01

    The growing demands placed on analytical laboratories to ensure the reliability of their results, due to the introduction of systems of quality and to the increasing use of metrology in chemical measurements has led most laboratories to validate their methodologies and to control them statistically. One of the techniques used most often for these purposes is based on the use of reference materials. The proper use of these materials means that laboratory results may be traced to the International System of Units, analytical methodologies can be validated, instruments calibrated and chemical measurements harmonized. One of the biggest challenges in developing reference materials is that of certifying their properties, a process that has been defined as assigning a concentration value that is as close as possible to the true value together with its uncertainty. Organizations that produce reference materials use several options for their certification process, and among these is the use of a primary method. Among the primary methods recognized by the International Office of Weights and Measures is the Isotope Dilution Mass Spectrometry technique. The Chilean Nuclear Energy Commission, through its Reference Materials Program, has prepared a reference material of clam tissue, which has been chemically defined by different analytical methodologies applied in different national and international laboratories. This work describes the methodology developed with the CIEMAT for determining the elements lead, cadmium and zinc in the clam tissue reference material using the primary technique of Isotope Dilution Mass Spectrometry. The calculation is described for obtaining the spike amounts to be added to the sample and the procedure is explained for carrying out the isotopic exchange. The isotopic relationships 204 Pb/ 205 Pb, 111 Cd/ 114 Cd and 66 Zn/ 67 Zn were determined in an atomic emission spectrometer with a plasma source with the following characteristics: plasma

  2. Solubility of reactor fuels in the mouse lung with respect to their U/Pu and 238Pu/239Pu ratios

    International Nuclear Information System (INIS)

    Talbot, R.J.; Baker, S.T.

    1989-01-01

    The studies reported were designed to assess the comparative in vivo solubilities of a range of plutonium containing reactor fuels. To simulate these fuels, mixed U/Pu oxides were prepared and calcined at 1600 0 C. A plutonium content of 3% w/w was chosen as typical of water-cooled reactor fuel. Higher concentrations of plutonium (10, 20 and 30%) were included to simulate fast reactor fuel. As it is known that 238 PuO 2 , with high specific activity, is translocated more rapidly from lung than 239 PuO 2 , the effect of isotopic composition of plutonium in simulated reactor fuels was also investigated. For this purpose, both the water-cooled and fast-reactor fuels were prepared with plutonium containing 2% of 238 Pu by weight. The resulting oxides had about 6 times the specific activity of those prepared with 239 Pu. Groups of mice were killed at 1, 3, 6, 12 and 18 months after inhaling aerosols of the simulated reactor fuels. After 3 months, measurements of Pu retention in the lung showed no marked differences between materials. After 6 months, measurements of plutonium deposited in the liver and skeleton showed that mixed U/Pu oxides were more soluble in vivo than 239 PuO 2 . Their solubility was inversely related to their plutonium content. The addition of 238 Pu to the plutonium resulted in enhanced translocation of plutonium from the lung, in the cases of water-cooled reactor fuel by a factor of two. (author)

  3. Reference methods and materials. A programme of support for regional and global marine pollution assessments

    International Nuclear Information System (INIS)

    1990-01-01

    This document describes a programme of comprehensive support for regional and global marine pollution assessments developed by the United Nations Environment Programme (UNEP) in cooperation with the International Atomic Energy Agency (IAEA) and the Intergovernmental Oceanographic Commission (IOC) and with the collaboration of a number of other United Nations Specialized agencies including the Food and Agriculture Organisation (FAO), the World Meteorological Organisation (WMO), the World Health Organisation (WHO) and the International Maritime Organisation (IMO). Two of the principle components of this programme, Reference Methods and Reference materials are given special attention in this document and a full Reference Method catalogue is included, giving details of over 80 methods currently available or in an advanced stage of preparation and testing. It is important that these methods are seen as a functional component of a much wider strategy necessary for assuring good quality and intercomparable data for regional and global pollution monitoring and the user is encouraged to read this document carefully before employing Reference Methods and Reference Materials in his/her laboratory. 3 figs

  4. 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

  5. CETAMA contribution to safeguards and nuclear forensic analysis based on nuclear reference materials

    International Nuclear Information System (INIS)

    Roudil, D.; Rigaux, C.; Rivier, C.; Hubinois, J.C.; Aufore, L.

    2012-01-01

    Measurement quality is crucial for the safety of nuclear facilities: nuclear reference materials (CRM) and interlaboratory programs (ILC), beyond the assessment of analytical measurement quality, play an important role. In the nuclear field, the CETAMA proposes suitable scientific and technical developments, in particular the preparation and certification of CRM used either as analytical standards or as reference samples for ILCs. The growing emphasis on nuclear forensic measurements will require some re-certification of old CRMs. But the future analytical challenges of meeting nuclear fuel cycle needs and of ensuring safeguard performance improvements will also concern the future CRMs. (authors)

  6. Polycyclic aromatic hydrocarbons (PAHs) in a coal tar standard reference material - SRM 1597a updated

    Energy Technology Data Exchange (ETDEWEB)

    Wise, Stephen A.; Poster, Dianne L.; Rimmer, Catherine A.; Schubert, Patricia; Sander, Lane C.; Schantz, Michele M. [National Institute of Standards and Technology (NIST), Analytical Chemistry Division, Gaithersburg, MD (United States); Leigh, Stefan D. [National Institute of Standards and Technology (NIST), Statistical Engineering Division, Gaithersburg, MD (United States); Moessner, Stephanie [National Institute of Standards and Technology (NIST), Analytical Chemistry Division, Gaithersburg, MD (United States); GMP/Comparator Labs, Werthenstein Chemie AG, Industrie Nord, Schachen (Switzerland)

    2010-09-15

    SRM 1597 Complex Mixture of Polycyclic Aromatic Hydrocarbons from Coal Tar, originally issued in 1987, was recently reanalyzed and reissued as SRM 1597a with 34 certified, 46 reference, and 12 information concentrations (as mass fractions) for polycyclic aromatic hydrocarbons (PAHs) and polycyclic aromatic sulfur heterocycles (PASHs) including methyl-substituted PAHs and PASHs. The certified and reference concentrations (as mass fractions) were based on results of analyses of the coal tar material using multiple analytical techniques including gas chromatography/mass spectrometry on four different stationary phases and reversed-phase liquid chromatography. SRM 1597a is currently the most extensively characterized SRM for PAHs and PASHs. (orig.)

  7. Establishing the traceability of a uranyl nitrate solution to a standard reference material

    International Nuclear Information System (INIS)

    Jackson, C.H.; Clark, J.P.

    1978-01-01

    A uranyl nitrate solution for use as a Working Calibration and Test Material (WCTM) was characterized, using a statistically designed procedure to document traceability to National Bureau of Standards Reference Material (SPM-960). A Reference Calibration and Test Material (PCTM) was prepared from SRM-960 uranium metal to approximate the acid and uranium concentration of the WCTM. This solution was used in the characterization procedure. Details of preparing, handling, and packaging these solutions are covered. Two outside laboratories, each having measurement expertise using a different analytical method, were selected to measure both solutions according to the procedure for characterizing the WCTM. Two different methods were also used for the in-house characterization work. All analytical results were tested for statistical agreement before the WCTM concentration and limit of error values were calculated. A concentration value was determined with a relative limit of error (RLE) of approximately 0.03% which was better than the target RLE of 0.08%. The use of this working material eliminates the expense of using SRMs to fulfill traceability requirements for uranium measurements on this type material. Several years' supply of uranyl nitrate solution with NBS traceability was produced. The cost of this material was less than 10% of an equal quantity of SRM-960 uranium metal

  8. Grain-size effects on PIXE and INAA analysis of IAEA-336 lichen reference material

    Science.gov (United States)

    Marques, A. P.; Freitas, M. C.; Wolterbeek, H. Th.; Verburg, T. G.; De Goeij, J. J. M.

    2007-02-01

    IAEA-336 lichen certified reference material was used to compare outcomes from INAA and PIXE elemental analyses, in relationship with grain size. The IAEA material (grain size lichen reference material's particle size distribution follows a bimodal distribution, which is turning more and more monomodal after further fine sieving. Replicates of each fraction were analysed by INAA and PIXE. Results for Cl, K, Mn, Fe and Zn by both techniques were compared by application of z-values tested against the criterion ∣ z∣ limited amount of lichen material as "seen" in the PIXE analysis and the grain size distribution in the lichen material were no causes of measurable differences between the results of both techniques. However, fractionation into smaller grain sizes showed to be associated with lower element content, for Na, Cl, K, Mn and Sr even up to a factor of 2. The observed increases of the proportion of algae in the smaller grain-size fractions and the possible accumulation capacity for certain elements in the fungal part of the lichen may explain the observed phenomenon. The sieving process and consequently the discarding of part of the material have lead to a change of the properties of the original sample, namely algae/fungus percentage and elemental contents.

  9. Certification of biological reference materials: participation of the Neutron Activation Laboratory (LAN-IPEN/CNEN-SP)

    International Nuclear Information System (INIS)

    Ticianelli, Regina B.; Figueiredo, Ana Maria G.

    2007-01-01

    Analytical laboratories have as one of their important goals to demonstrate their competence allowing international acceptance and comparison of analytical data. The IPEN Neutron Activation Laboratory (LAN-IPEN) has implemented its Quality Assurance Program which comprises, among other activities, the participation in intercomparison runs. As a part of this Quality Assurance Program, LAN-IPEN has participated in interlaboratorial trials to analyze two biological candidate reference materials: INCT-CF-3 Corn Flour and INCT-SBF-4 Soya Bean Flour from the Institute of Nuclear Chemistry And Technology (Warszawa, Poland). The elements Br, Ca, Co, Cs, Fe, K, Na, Rb and Zn were analyzed in the candidate reference materials by instrumental neutron activation analysis (INAA). The performance of the laboratory was statistically evaluated in relation to the consensus values for these materials using the Z-Score test. This laboratory evaluation method has been accepted as a standard by ISO/IUPAC. In the present study, adequate Z-Score values (|Z|<2) were observed for all of the analyzed elements, confirming the accuracy of the nuclear methodology employed. The contribution of LAN-IPEN in the certification of the reference materials analyzed was very important, since the results provided were used in the statistical evaluation of the certified value. (author)

  10. 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.

  11. Quality control provisions applied in the preparation and characterization of Pu-bearing PERLA standards

    International Nuclear Information System (INIS)

    Guardini, S.; Guzzi, G.; Mousty, F.; Kuhn, E.; Regge, P. de

    1990-01-01

    This report describes the work carried out at the different laboratories where Pu-bearing samples, intended for use as reference materials for NDA measurements, were prepared and characterized. The standard samples were produced from PuO2 and MOX batches of different nature and are at present stored in the PERLA facility at the Institute for Safety Technology of the JRC Ispra and are available for use. Particular attention is paid to the quality control procedures adopted during the sampling, preparation and analysis of the material, to fulfil the requirements established a priori for NDA standards to be used in Safeguards. The results of the different quality control checks are presented and discussed. The drawings of the containers for the PuO2 and MOX powders and of the special fuel rods for MOX pellets are also presented. This report is intended for use in conjunction with the PERLA STANDARD CERTIFICATES which are issued for each type of material considered, and gives to the user the possibility of tracing all analytical data back to primary standards

  12. NBS SRM 1569 Brewer's Yeast: Is it an adequate standard reference material for testing a chromium determination in biological materials tion in biological materials

    International Nuclear Information System (INIS)

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

    1978-01-01

    Some analytical experiences with NBS SRM 1569 Brewer's Yeast are presented. Against this background the adequacy of this standard reference material for the determination of chromium in biological materials is discussed. Authors have three main objections. Due to its high content of insoluble chromium-containing particles, SRM 1569 is not typical for biological materials, possibly not even for Brewer's Yeast. The chromium level of SRM 1569 is not typical for the chromium levels normally encountered in pure biological materials. The major fraction (69 +- 3 percent) of the chromium is present in a form which is insoluble under the conditions used in Author's analysis. (T.I.)

  13. Designing Pu600 for Authentication

    International Nuclear Information System (INIS)

    White, G.

    2008-01-01

    Many recent Non-proliferation and Arms Control software projects include an authentication component. Demonstrating assurance that software and hardware performs as expected without hidden 'back-doors' is crucial to a project's success. In this context, 'authentication' is defined as determining that the system performs only its intended purpose and performs that purpose correctly and reliably over many years. Pu600 is a mature software solution for determining the presence of Pu and the ratio of Pu240 to Pu239 by analyzing the gamma ray spectra in the 600 KeV region. The project's goals are to explore hardware and software technologies which can by applied to Pu600 which ease the authentication of a complete, end-to-end solution. We will discuss alternatives and give the current status of our work

  14. Designing Pu600 for Authentication

    Energy Technology Data Exchange (ETDEWEB)

    White, G

    2008-07-10

    Many recent Non-proliferation and Arms Control software projects include an authentication component. Demonstrating assurance that software and hardware performs as expected without hidden 'back-doors' is crucial to a project's success. In this context, 'authentication' is defined as determining that the system performs only its intended purpose and performs that purpose correctly and reliably over many years. Pu600 is a mature software solution for determining the presence of Pu and the ratio of Pu240 to Pu239 by analyzing the gamma ray spectra in the 600 KeV region. The project's goals are to explore hardware and software technologies which can by applied to Pu600 which ease the authentication of a complete, end-to-end solution. We will discuss alternatives and give the current status of our work.

  15. Thermodynamic assessment of the LiF–ThF4–PuF3–UF4 system

    NARCIS (Netherlands)

    Capelli, E.; Benes, O.; Konings, R.J.M.

    2015-01-01

    The LiF–ThF4–PuF3–UF4 system is the reference salt mixture considered for the Molten Salt Fast Reactor (MSFR) concept started with PuF3. In order to obtain the complete thermodynamic description of this quaternary system, two binary systems (ThF4–PuF3 and UF4–PuF3) and two ternary systems

  16. 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)

  17. Certified reference materials for analytical quality control in neutron activation analysis

    International Nuclear Information System (INIS)

    Wee Boon Siong; Abdul Khalik Wood; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman; Mohd Suhaimi Elias; Nazaratul Ashifa Abdul Salim

    2007-01-01

    Analytical quality control in neutron activation analysis (NAA) requires the use of certified reference materials (CRM) in order to produce reliable analytical results. It is essential to evaluate the performance of NAA method when analyzing various sample matrices. Therefore, the CRM selected for an analysis should be suitable for the type of samples. There are many aspects such as concentration range, matrix match, sample size and uncertainty, which need to be considered when selecting a suitable CRM. Eventually, results of analysis of CRM were plotted into control charts in order to evaluate the qualify of the data. This is to ensure that the results are within the 95 % confidence interval as stipulated in the certificate of CRM. Thus, this article aims to discuss the uses of certified reference materials for quality control purposes in NAA involving various sample matrices. (author)

  18. Comparison of relative INAA and k0-INAA using soil and sediment reference materials

    International Nuclear Information System (INIS)

    Jacimovic, R.

    2014-01-01

    The objective of this work was to compare the results obtained by the relative INAA and k 0 -INAA methods for the same input parameters (sample mass, nuclear data, net peak area for the same gamma line and the same measurement and same cooling and measurement times). In total eight environmental soil and sediment reference materials (RM) or certified reference materials (CRM) from different producers were analysed. In this work only the recommended or certified values were considered, allowing comparison of the two methods for 30 elements. The results point out that k 0 -INAA possesses superior qualities compared to relative INAA, being insensitive to flux gradients, and independent of recommended/certified values in RMs/CRMs, often used as standards in relative INAA. (author)

  19. The preparation and analysis of minerals for use as reference material

    International Nuclear Information System (INIS)

    Stoch, H.

    1976-01-01

    This report covers the progress made in the collection of the material for reference samples, and the five interlaboratory analytical programmes (ferrochromium slags, fluorspar, 'mixed' NIMROC samples, rare earths, and ferromanganese slags). The description of the internal analytical programme has been subdivided into eight main categories, and a comprehensive list of evaluated results covering a wide range of materials is included. Additional results for thorium, rare earths, tin, tantalum, and niobium for the appropriate reference samples are included in updated tables. The main purpose in the preparation of these samples is to provide control samples for analytical work at the National Institute for Metallurgy. Where there is a special need, limited quantities of the samples can be made available to other laboratories

  20. Instrumental neutron activation analysis of proposed marine sediment reference material (IAEA-158)

    International Nuclear Information System (INIS)

    Siddique, N.; Waheed, S.

    2009-01-01

    IAEA-158, sediment prepared by the International Atomic Energy Agency -Marine Environmental Laboratory (IAEA-MEL), Monaco was received under the IAEA Analytical Quality Control Services (AQCS) Intercomparison Programme. Instrumental Neutron Activation Analysis (INAA) was used to determine AI, As, Br, Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Mn, Na, Nd, Rb, Sb, Sc, Se, Sm, Ta, Tb, Th, V, Vb and Zn in this proposed reference material (RM). Four different irradiation protocols were adopted using a miniature neutron source reactor (MNSR) by varying the irradiation, cooling and counting times. IAEA-405 (Estuarine Sediment) and IAEA-SLI (Lake Sediment) were used as compatible matrix reference materials for quality assurance (QA) purposes. Good agreement between our data and lAEA certified values was obtained providing confidence in the reported data. (author)

  1. Reference Materials for Calibration of Analytical Biases in Quantification of DNA Methylation.

    Science.gov (United States)

    Yu, Hannah; Hahn, Yoonsoo; Yang, Inchul

    2015-01-01

    Most contemporary methods for the quantification of DNA methylation employ bisulfite conversion and PCR amplification. However, many reports have indicated that bisulfite-mediated PCR methodologies can result in inaccurate measurements of DNA methylation owing to amplification biases. To calibrate analytical biases in quantification of gene methylation, especially those that arise during PCR, we utilized reference materials that represent exact bisulfite-converted sequences with 0% and 100% methylation status of specific genes. After determining relative quantities using qPCR, pairs of plasmids were gravimetrically mixed to generate working standards with predefined DNA methylation levels at 10% intervals in terms of mole fractions. The working standards were used as controls to optimize the experimental conditions and also as calibration standards in melting-based and sequencing-based analyses of DNA methylation. Use of the reference materials enabled precise characterization and proper calibration of various biases during PCR and subsequent methylation measurement processes, resulting in accurate measurements.

  2. Analysis of soil reference materials for vanadium(+5) species by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Mandiwana, Khakhathi L.; Panichev, Nikolay

    2010-01-01

    Solid Certified Reference Materials (CRMs) with known vanadium(+5) content are currently not commercially available. Because of this, vanadium species have been determined in solid CRMs of soil, viz. CRM023-50, CRM024-50, CRM049-50, SQC001 and SQC0012. These CRMs are certified with only total vanadium content. Vanadium(+5) was extracted from soil reference materials with 0.1 M Na 2 CO 3 . The quantification of V(+5) was carried out by electrothermal atomic absorption spectrometry (ET-AAS). The concentration of V(+5) in the analyzed CRMs was found to be ranging between 3.60 and 86.0 μg g -1 . It was also found that SQC001 contains approximately 88% of vanadium as V(+5) species. Statistical evaluation of the results of the two methods by paired t-test was in good agreement at 95% level of confidence.

  3. Homogeneity study on biological candidate reference materials: the role of neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Daniel P.; Moreira, Edson G., E-mail: dsilva.pereira@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    Instrumental Neutron activation Analysis (INAA) is a mature nuclear analytical technique able to accurately determine chemical elements without the need of sample digestion and, hence, without the associated problems of analyte loss or contamination. This feature, along with its potentiality use as a primary method of analysis, makes it an important tool for the characterization of new references materials and in the assessment of their homogeneity status. In this study, the ability of the comparative method of INAA for the within-bottle homogeneity of K, Mg, Mn and V in a mussel reference material was investigated. Method parameters, such as irradiation time, sample decay time and distance from sample to the detector were varied in order to allow element determination in subsamples of different sample masses in duplicate. Sample masses were in the range of 1 to 250 mg and the limitations of the detection limit for small sample masses and dead time distortions for large sample masses were investigated. (author)

  4. Certification of a niobium metal reference material for neutron dosimetry (EC-NRM 525)

    International Nuclear Information System (INIS)

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

    1990-01-01

    Niobium metal, of 99.98% nominal purity, in the form of 0.02 and 0.1 mm thick foils and of 0.5 mm diameter wire, has been certified for its tantalum mass fraction. The certified value of the tantalum mass fraction is 19.6 ± 1.8 mg.kg -1 and is based on 71 results obtained by six laboratories by neutron activation analysis or inductively coupled plasma source mass spectrometry. The material is intended to be used as a reference material in neutron metrology

  5. Candidate coffee reference material for element content: production and certification schemes adopted at CENA/USP

    Energy Technology Data Exchange (ETDEWEB)

    Tagliaferro, Fabio Sileno; Fernandes, Elisabete A. de Nadai; Bacchi, Marcio Arruda; Franca, Elvis Joacir de [Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil). Lab. de Radioisotopos], e-mail: fabiotag@cena.usp.br, e-mail: lis@cena.usp.br, e-mail: mabacchi@cena.usp.br, e-mail: ejfranca@cena.usp.br; Bode, Peter; Bacchi, Marcio Arruda; Franca, Elvis Joacir de [Delft University of Technology, Delft (Netherlands). Interfaculty Reactor Inst.], e-mail: P.Bode@iri.tudelft.nl

    2003-07-01

    Certified reference materials (CRMs) play a fundamental role in analytical chemistry establishing the traceability of measurement results and assuring accuracy and reliability. In spite of the huge importance of measurements in the food sector, Brazil does not produce CRMs to supply the demand. Consequently the acquisition of CRMs depends on imports at high costs. The coffee sector needs CRMs, however there is no material that represents the coffee composition. Since 1998, the Laboratorio de Radioisotopos (LRi) of CENA/USP has been involved in analysis of coffee. During this period, knowledge has been accumulated about several aspects of coffee, such as system of cultivation, elemental composition, homogeneity of the material, possible contaminants and physical properties of beans. Concomitantly, LRi has concentrated efforts in the field of metrology in chemistry, and now all this expertise is being used as the basis for the production of a coffee certified reference material (CRM) for inorganic element content. The scheme developed for the preparation and certification of coffee RM relies on the ISO Guides 34 and 35. The approaches for selection, collection and preparation of the material, moisture determination method, homogeneity testing, certification and long-term stability testing are discussed and a time frame for the expected accomplishments is provided. (author)

  6. Candidate coffee reference material for element content: production and certification schemes adopted at CENA/USP

    International Nuclear Information System (INIS)

    Tagliaferro, Fabio Sileno; Fernandes, Elisabete A. de Nadai; Bacchi, Marcio Arruda; Franca, Elvis Joacir de; Bode, Peter; Bacchi, Marcio Arruda; Franca, Elvis Joacir de

    2003-01-01

    Certified reference materials (CRMs) play a fundamental role in analytical chemistry establishing the traceability of measurement results and assuring accuracy and reliability. In spite of the huge importance of measurements in the food sector, Brazil does not produce CRMs to supply the demand. Consequently the acquisition of CRMs depends on imports at high costs. The coffee sector needs CRMs, however there is no material that represents the coffee composition. Since 1998, the Laboratorio de Radioisotopos (LRi) of CENA/USP has been involved in analysis of coffee. During this period, knowledge has been accumulated about several aspects of coffee, such as system of cultivation, elemental composition, homogeneity of the material, possible contaminants and physical properties of beans. Concomitantly, LRi has concentrated efforts in the field of metrology in chemistry, and now all this expertise is being used as the basis for the production of a coffee certified reference material (CRM) for inorganic element content. The scheme developed for the preparation and certification of coffee RM relies on the ISO Guides 34 and 35. The approaches for selection, collection and preparation of the material, moisture determination method, homogeneity testing, certification and long-term stability testing are discussed and a time frame for the expected accomplishments is provided. (author)

  7. On the interpretation of micro-PIXE measurements on a prototype microstructured reference material

    International Nuclear Information System (INIS)

    Waetjen, Uwe; Barsony, Istvan; Grime, Geoff W.; Rajta, Istvan

    1999-01-01

    In order to determine the beam spot size and scanning properties of ion microbeam systems, a novel reference material has been developed, consisting of permalloy (81% Ni, 19% Fe) strip patterns on silicon substrate. Due to the choice of substrate and pattern materials, these samples exhibit a high elemental contrast suitable for analysis with X-ray detection and ion scattering techniques. The microlithographic production scheme is briefly described. A prototype chip of this material was investigated with PIXE and RBS analysis in a scanning nuclear microprobe. It proved to be extremely useful in the routine to focus the ion microbeam and to determine its spot size. Due to the microscopic structure of these samples, a geometric dependence of matrix effects in the production of Si X-rays from the substrate material could be shown. Even dead-time effects in the counting electronics, showing up as an apparent thickness gradient, could be observed. Besides its primary role in microbeam diagnostics, this reference material can serve an educational role in developing the analyst's ability to correctly identify and interpret such artefacts

  8. Measurement of polybrominated diphenyl ethers in environmental matrix standard reference materials

    Energy Technology Data Exchange (ETDEWEB)

    Stapleton, H.; Schantz, M.; Wise, S. (National Institute of Standards and Technology)

    2004-09-15

    Polybrominated diphenyl ethers (PBDEs) are a class of emerging contaminants of concern as many studies have now demonstrated that these compounds are bioaccumulative, persistent and increasing in concentration in the environment. PBDEs are being detected in almost every environmental sample examined, and they have even been measured in samples collected in the Arctic, further demonstrating their persistence and potential for long range transport. More and more studies are continuing to examine the fate and transport of these flame retardant compounds in environmental samples and as such, reference materials are needed to provide quality control on these measurements. The National Institute of Standards and Technology (NIST) supports a national Standard Reference Material (SRM) program for measurement of organic contaminants such as PCBs, PAHs and chlorinated pesticides in environmental matrices. This current study was undertaken to provide reference measurements for PBDEs in selected SRMs that are currently used by various laboratories throughout the United States. These SRMs include matrices such as marine mammal blubber, lake trout tissue, mussel tissue, sediment, house dust and human serum. We report here reference values for 22 PBDE congeners that have been quantified in these seven types of SRMs.

  9. Austenitic chromium nickel steel as standard reference material in measurement of thermal and temperature conductivity

    International Nuclear Information System (INIS)

    Binkele, L.

    1990-01-01

    A niobium-stabilized CrNi steel with the NBS designation SRM 735 is introduced as WLF standard reference material in a report by Hust and Giarratano, for the temperature range 300-1200 K and for thermal conductivities around 20 W/mk. However, its specification does not show it to be a direct member of the DIN family of CrNi steels. This report should be regarded as a continuation and supplement to the above-mentioned efforts in America. On the one hand, a solution of a possibly too-narrow specification is aimed at for the reference material, where it is important how sensitive the thermal conductivity is to changes in the chemical composition and changes of the manufacturing parameters and what accuracy can be reached for the reference values with the best measurement techniques. On the other hand, the data base should be expanded and the accuracy of the reference curve should be improved if possible. (orig./MM) [de

  10. Introducing LIR (Lithotheque Ireland, a reference collection of flaked stone tool raw materials from Ireland

    Directory of Open Access Journals (Sweden)

    Killian Driscoll

    2016-09-01

    Full Text Available The LIR (Lithotheque Ireland reference collection of flaked stone tool raw materials from Ireland began in 2013, and is based on the geological prospection from two projects. The first (2013-2015 focused attention primarily on Carboniferous cherts from the northwest of Ireland, collecting 405 samples. The second (2015-2017 is currently collecting samples of the Cretaceous flint primarily from in situ contexts in the northeast of Ireland, but also includes beach surveys of Cretaceous flint from around the island; the first phase of geological prospection in Autumn 2015 collected 239 samples, with the geological prospection continuing in 2016. Therefore, to date the collection contains over 600 hand samples of chert and flint, along with a small number of other materials (siliceous limestone, tuff, mudstone. The physical reference collection is housed at the UCD School of Archaeology, University College Dublin and contains the geological hand samples along with the various thin sections of the samples that are used for petrographic analysis. The physical collection is complemented by an online database that is to be used alongside the physical collection, or can be used as a stand-alone resource. This paper provides an overview of the database’s metadata and the processes of data entry and editing, to serve as a reference point for the database and the fieldwork undertaken to date, and to serve as a template for other researchers undertaking similar work on lithic reference collections.

  11. Initial testing of a neutron activation analysis system by analysing standard reference materials

    International Nuclear Information System (INIS)

    Suhaimi Hamzah; Roslan Idris; Abdul Khalik Haji Wood; Che Seman Mahmood; Abdul Rahim Mohamad Noor.

    1983-01-01

    This paper describes the data acquisition and processing system in our laboratories (ND6600), the methods of activation analysis and the results obtained from our analysis of IAEA standard reference material (SL-l lake sediments and NBS coal ash 1632a). These standards were analysed in order to check the capability of the system, which was designed in such a way as to enable the user to independently collect and process data from multiple radiation detectors. (author)

  12. Stability of aflatoxin B1 in animal feed candidate reference materials

    NARCIS (Netherlands)

    Roos, A.H.; Mazijk, van R.J.; Tuinstra, L.G.M.T.; Huf, F.A.

    1991-01-01

    Two candidate reference materials animal feed were stored at a temperature of -18°C, 4 C, 20°C and 37°C. The stability of aflatoxin B1 was studied duringa period of two years. A significant decrease in the aflatoxin B1 content was measured in the samples stared at 20°C and 37°C. In the samples

  13. The role of adequate reference materials in density measurements in hemodialysis

    Science.gov (United States)

    Furtado, A.; Moutinho, J.; Moura, S.; Oliveira, F.; Filipe, E.

    2015-02-01

    In hemodialysis, oscillation-type density meters are used to measure the density of the acid component of the dialysate solutions used in the treatment of kidney patients. An incorrect density determination of this solution used in hemodialysis treatments can cause several and adverse events to patients. Therefore, despite the Fresenius Medical Care (FME) tight control of the density meters calibration results, this study shows the benefits of mimic the matrix usually measured to produce suitable reference materials for the density meter calibrations.

  14. The role of adequate reference materials in density measurements in hemodialysis

    International Nuclear Information System (INIS)

    Furtado, A; Moura, S; Filipe, E; Moutinho, J; Oliveira, F

    2015-01-01

    In hemodialysis, oscillation-type density meters are used to measure the density of the acid component of the dialysate solutions used in the treatment of kidney patients. An incorrect density determination of this solution used in hemodialysis treatments can cause several and adverse events to patients. Therefore, despite the Fresenius Medical Care (FME) tight control of the density meters calibration results, this study shows the benefits of mimic the matrix usually measured to produce suitable reference materials for the density meter calibrations

  15. Determination of element concentrations in biological reference materials by solid sampling and other analytical methods

    International Nuclear Information System (INIS)

    Schauenburg, H.; Weigert, P.

    1992-01-01

    Using solid sampling with graphite furnace atomic absorption spectrometry (GFAAS), values for cadmium, copper, lead and zinc in six biological reference materials were obtained from up to four laboratories participating in three collaborative studies. These results are compared with those obtained with other methods used in routine analysis from laboratories of official food control. Under certain conditions solid sampling with GFAAS seems to be suitable for routine analysis as well as conventional methods. (orig.)

  16. Neutron activation analysis of reference materials by the k sub 0 standardization and relative methods

    Energy Technology Data Exchange (ETDEWEB)

    Freitas, M C; Martinho, E [LNETI/ICEN, Sacavem (Portugal)

    1989-04-15

    Instrumental neutron activation analysis with the k{sub o}-standardization method was applied to eight geological, environmental and biological reference materials, including leaves, blood, fish, sediments, soils and limestone. To a first approximation, the results were normally distributed around the certified values with a standard deviation of 10%. Results obtained by using the relative method based on well characterized multi-element standards for IAEA CRM Soil-7 are reported.

  17. Production and certification of reference materials; Producao e certificacao de materiais de referencia

    Energy Technology Data Exchange (ETDEWEB)

    Sarkis, Jorge Eduardo de S.; Kakazu, Mauricio H; Hespanhol, Emilio Carlos B; Martins, Elaine Arantes J [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

    1996-07-01

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

  18. Development of benzene, toluene, ethylbenzene and xylenes certified gaseous reference materials

    Science.gov (United States)

    Brum, M. C.; Sobrinho, D. C. G.; Fagundes, F. A.; Oudwater, R. J.; Augusto, C. R.

    2016-07-01

    The work describes the production of certified gaseous reference materials of benzene, toluene, ethylbenzene and xylenes (BTEX) in nitrogen from the gravimetric production up to the long term stability tests followed by the certifying step. The uncertainty in the amount fractions of the compounds in these mixtures was approximately 4% (relative) for the range studied from 2 to 16 µmol/mol. Also the adsorption of the BTEX on the cylinder surface and the tubing were investigated as potential uncertainty source.

  19. Certified reference material IAEA-418: I-129 in Mediterranean sea water

    International Nuclear Information System (INIS)

    2009-01-01

    Our society is attaching increasing importance to the study and assessment of the state and health of the environment. Organizations involved in such activities rely on the quality of the information provided and, ultimately, on the precision and accuracy of the data on which the information is based. Many laboratories are involved in the production of environmental data in many cases leading to wider assessments. These laboratories may develop and validate new analytical methods, study the environmental impact of human activities, provide services to other organizations, etc. In particular, laboratories are providing data on levels of radioactivity in a variety of marine matrixes such as water, suspended matter, sediments and biota. Because of the need to base scientific conclusions on valid and internationally comparable data, the need to provide policy makers with correct information and the need for society to be informed of the state of the environment, it is indispensable to ensure the quality of the data produced by each laboratory. Principles of good laboratory practice require both internal and external procedures to verify the quality of the data produced. Internal quality is verified in a number of ways such as the use of laboratory information systems, keeping full records of equipment performance and standardization of analytical procedures. External quality can also be ascertained in a number of ways, notably accreditation by an external body under a defined quality scheme but also, amongst others, the use of internationally accepted calibration standards that are traceable to the SI international system of units, the participation in interlaboratory comparisons or the regular use of reference materials to test laboratory performance. The Radiometrics Laboratory of the IAEA Marine Environment Laboratories has been providing quality products for the last 40 years which include the organization of interlaboratory comparisons, proficiency tests

  20. 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.)

  1. 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

  2. Evaluation of nuclear data of 244Pu and 237Pu

    International Nuclear Information System (INIS)

    Nakagawa, Tsuneo; Konshin, V.A.

    1995-10-01

    The evaluation of nuclear data for 244 Pu and 237 Pu was made in the neutron energy region from 10 -5 eV to 20 MeV. For the both nuclides, the total, elastic and inelastic scattering, fission, capture, (n,2n) and (n,3n) reaction cross sections were evaluated on the basis of theoretical calculation. The resonance parameters were given for 244 Pu. The angular and energy distributions of secondary neutrons were also estimated for the both nuclides. The results were compiled in the ENDF-5 format and will be adopted in JENDL Actinoid File. (author)

  3. A study on homogeneity of the IAEA candidate reference materials for microanalysis and analytical support in the certification of these materials

    International Nuclear Information System (INIS)

    Dybczynski, R.; Danko, B.; Polkowska-Motrenko, H.

    2002-01-01

    In this paper a study on homogeneity of new IAEA candidate reference materials: IAEA 338 Lichen and IAEA 413 Algae in small (ca.10 mg) samples as well as some data contributing to certification of these materials are presented. (author)

  4. 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

  5. The NISTmAb Reference Material 8671 lifecycle management and quality plan.

    Science.gov (United States)

    Schiel, John E; Turner, Abigail

    2018-03-01

    Comprehensive analysis of monoclonal antibody therapeutics involves an ever expanding cadre of technologies. Lifecycle-appropriate application of current and emerging techniques requires rigorous testing followed by discussion between industry and regulators in a pre-competitive space, an effort that may be facilitated by a widely available test metric. Biopharmaceutical quality materials, however, are often difficult to access and/or are protected by intellectual property rights. The NISTmAb, humanized IgG1κ Reference Material 8671 (RM 8671), has been established with the intent of filling that void. The NISTmAb embodies the quality and characteristics of a typical biopharmaceutical product, is widely available to the biopharmaceutical community, and is an open innovation tool for development and dissemination of results. The NISTmAb lifecyle management plan described herein provides a hierarchical strategy for maintenance of quality over time through rigorous method qualification detailed in additional submissions in the current publication series. The NISTmAb RM 8671 is a representative monoclonal antibody material and provides a means to continually evaluate current best practices, promote innovative approaches, and inform regulatory paradigms as technology advances. Graphical abstract The NISTmAb Reference Material (RM) 8671 is intended to be an industry standard monoclonal antibody for pre-competitive harmonization of best practices and designing next generation characterization technologies for identity, quality, and stability testing.

  6. The use of reference materials in the elemental analysis of biological samples

    International Nuclear Information System (INIS)

    Bowen, H.J.M.

    1975-01-01

    Reference materials (RMs) are useful to compare the accuracy and precision of laboratories and techniques. The desirable properties of biological reference materials are listed, and the problems of production, homogenization and storage described. At present there are only 10 biological RMs available compared with 213 geological and 520 metallurgical RMs. There is a need for more biological RMs including special materials for microprobe analysis and for in vivo activation analysis. A study of 650 mean values for elements in RM Kale, analysed by many laboratories, leads to the following conclusions. 61% of the values lie within +-10% of the best mean, and 80% lie within +-20% of the best mean. Atomic absorption spectrometry gives results that are 5-30% high for seven elements, while intrumental neutron activation analysis gives low and imprecise results for K. Other techniques with poor interlaboratory precision include neutron activation for Mg, polarography for Zn and arc-spectrometry for many elements. More than half the values for elements in Kale were obtained by neutron activation, confirming the importance of this technique and the need for RMs. As a rough estimate, 6 x 10 9 elemental analyses of biological materials are carried out each year, mostly by medical, agricultural and food scientists. It seems likely that a substantial percentage of these are inaccurate, a situation that might be improved by quality control using standard RMs. (author)

  7. 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.

  8. Quality assessment of organic coffee beans for the preparation of a candidate reference material

    International Nuclear Information System (INIS)

    Tagliaferro, F.S.; Nadai Fernandes de, E.A.; Bacchi, M.A.

    2006-01-01

    A random sampling was carried out in the coffee beans collected for the preparation of the organic green coffee reference material in view of assessing the homogeneity and the presence of soil as impurity. Fifteen samples were taken for the between-sample homogeneity evaluation. One of the samples was selected and 10 test portions withdrawn for the within-sample homogeneity evaluation. Br, Ca, Co, Cs, Fe, K, Na, Rb, Sc and Zn were determined by instrumental neutron activation analysis (INAA). The F-test demonstrated that the material is homogeneous for Ca, Co, Cs, K and Sc, but not homogeneous for Br, Fe, Na, Rb and Zn. Results of terrigenous elements suggested negligible soil contamination in the raw material. (author)

  9. Reference Material Kydex(registered trademark)-100 Test Data Message for Flammability Testing

    Science.gov (United States)

    Engel, Carl D.; Richardson, Erin; Davis, Eddie

    2003-01-01

    The Marshall Space Flight Center (MSFC) Materials and Processes Technical Information System (MAPTIS) database contains, as an engineering resource, a large amount of material test data carefully obtained and recorded over a number of years. Flammability test data obtained using Test 1 of NASA-STD-6001 is a significant component of this database. NASA-STD-6001 recommends that Kydex 100 be used as a reference material for testing certification and for comparison between test facilities in the round-robin certification testing that occurs every 2 years. As a result of these regular activities, a large volume of test data is recorded within the MAPTIS database. The activity described in this technical report was undertaken to mine the database, recover flammability (Test 1) Kydex 100 data, and review the lessons learned from analysis of these data.

  10. Testing the homogeneity of candidate reference materials by solid sampling - AAS and INAA

    International Nuclear Information System (INIS)

    Rossbach, M.; Grobecker, K.-H.

    2002-01-01

    The necessity to quantify a natural material's homogeneity with respect to its elemental distribution prior to chemical analysis of a given aliquot is emphasised. Available instruments and methods to obtain the relevant information are described. Additionally the calculation of element specific, relative homogeneity factors, H E , and of a minimum sample mass M 5% to achieve 5% precision on a 95% confidence level is given. Especially, in the production and certification of Certified Reference Materials (CRMs) this characteristic information should be determined in order to provide the user with additional inherent properties of the CRM to enable more economical use of the expensive material and to evaluate further systematic bias of the applied analytical technique. (author)

  11. Performance of NAA methods in an International Interlaboratory Reference Material Characterization Campaign

    International Nuclear Information System (INIS)

    Ihnat, M.

    2000-01-01

    An extensive database of analytical results from a recent biological matrix Reference Material Characterization Campaign permitted an intercomparison of the performances of various methods among each other and with 'true' best estimate concentration values established for these materials. Six different variants of neutron activation analysis (NAA) methods were employed including: instrumental neutron activation analysis, instrumental neutron activation analysis with acid digestion, neutron activation analysis with radiochemical separation, neutron capture prompt gamma activation analysis, epithermal instrumental neutron activation analysis, and neutron activation analysis with preconcentration. The precision and accuracy performance of NAA-based analytical methods are compared with three other major techniques, atomic absorption spectrometry (AAS), atomic emission spectrometry (AES) and mass spectrometry (MS) for 28 elements in 10 natural matrix materials. (author)

  12. Homogeneity and evaluation of the new NIST leaf certified reference materials

    International Nuclear Information System (INIS)

    Becker, D.A.

    1990-01-01

    The NIST has produced and is in the process of certifying two new leaf CRMs, SRM1515 Apple Leaves and SRM 1547 Peach Leaves, as replacements for the no longer available NBS Orchard Leaves and the almost depleted Citrus Leaves. These two new materials have been processed and are being thoroughly evaluated and should provide the most advanced natural matrix botanical trace-element reference materials available. Caution should be used in determining a basis weight (drying) for these CRMs because of their very fine particle size. Homogeneity has been established by instrumental neutron activation analysis on both leaf materials for five elements, to date, to better than 1.5% (1 s) for 100-mg sample sizes

  13. Base case Pu-nitrate to Pu-oxide conversion plant

    International Nuclear Information System (INIS)

    1978-10-01

    This paper explains that the plutonium recovered in the course of reprocessing spent fuel is obtained in the form of plutonium nitrate, whereas PuO 2 is required for the fabrication of fuel rods. The reference conversion plant described in the paper converts plutonium nitrate into plutonium dioxide powder by precipitation with oxalic acid followed by calcination. The paper also describes the main features of the safety, maintenance and safeguards philosophy used in its design

  14. Grain-size effects on PIXE and INAA analysis of IAEA-336 lichen reference material

    International Nuclear Information System (INIS)

    Marques, A.P.; Freitas, M.C.; Wolterbeek, H.Th.; Verburg, T.G.; Goeij, J.J.M. de

    2007-01-01

    IAEA-336 lichen certified reference material was used to compare outcomes from INAA and PIXE elemental analyses, in relationship with grain size. The IAEA material (grain size <125 μm) was ground and sieved through nylon nets with 64 μm, 41 μm and 20 μm pores. Particle sizes were determined by Laser Light Scattering technique: the data indicate that, after sieving, the IAEA-336 lichen reference material's particle size distribution follows a bimodal distribution, which is turning more and more monomodal after further fine sieving. Replicates of each fraction were analysed by INAA and PIXE. Results for Cl, K, Mn, Fe and Zn by both techniques were compared by application of z-values tested against the criterion vertical bar z vertical bar < 3 for approval of results at the 99.7% confidence level. Under the conditions of this study, the limited amount of lichen material as 'seen' in the PIXE analysis and the grain size distribution in the lichen material were no causes of measurable differences between the results of both techniques. However, fractionation into smaller grain sizes showed to be associated with lower element content, for Na, Cl, K, Mn and Sr even up to a factor of 2. The observed increases of the proportion of algae in the smaller grain-size fractions and the possible accumulation capacity for certain elements in the fungal part of the lichen may explain the observed phenomenon. The sieving process and consequently the discarding of part of the material have lead to a change of the properties of the original sample, namely algae/fungus percentage and elemental contents

  15. Catalog of NBS standard reference materials, 1975--76 edition. Special pub

    International Nuclear Information System (INIS)

    Seward, R.W.

    1975-06-01

    This Catalog lists and describes the Standard Reference Materials (SRM's), Research Materials (RM's), and General Materials (GM's) currently distributed by the National Bureau of Standards, as well as many of the materials currently in preparation. SRM's are used to calibrate measurement systems and to provide a central basis for uniformity and accuracy of measurement. The unit and quantity, the type, and the certified characterization are listed for each SRM, as well as directions for ordering. The RM's are not certified, but are issued to meet the needs of scientists engaged in materials research. RM's are issued with a 'Report of Investigation', the sole authority of which is the author of the report. The GM's are standardized by some agency other than NBS. NBS acts only as a distribution point and does not participate in the standardization of these materials. Announcements of new and renewal SRM's, RM's and GM's are made in the semi-annual supplements of this Catalog, SRM Price List, and in scientific and trade journals

  16. Reference Materials for Trace Element Microanalysis of Carbonates by SIMS and other Mass Spectrometric Techniques

    Science.gov (United States)

    Layne, G. D.

    2009-12-01

    Today, many areas of geochemical research utilize microanalytical determinations of trace elements in carbonate minerals. In particular, there has been an explosion in the application of Secondary Ion Mass Spectrometry (SIMS) to studies of marine biomineralization. SIMS provides highly precise determinations of Mg and Sr at the concentration levels normally encountered in corals, mollusks or fish otoliths. It is also a highly effective means for determining a wide range of other trace elements at ppm levels (e.g., Na, Fe, Mn, Ba, REE, Pb, Th, and U) in a variety of naturally occurring calcite and aragonite matrices - and so is potentially valuable in studies of diagenesis, hydrothermal fluids and carbonatitic magmas. For SIMS, modest time per spot (often sputtered ion yields of most elements with the major element composition of the sample matrix, accuracy of SIMS depends intimately on matrix-matched solid reference materials. Despite its rapidly increasing use for trace element analyses of carbonates, there remains a dearth of certified reference materials suitable for calibrating SIMS. The pressed powders used by some analysts to calibrate LA-ICP-MS do not perform well for SIMS - they are not perfectly dense or homogeneous to the desired level at the micron scale of sampling. Further, they often prove incompatible with the sample high vacuum compatibility requirement for stable SIMS analysis (10-8 to 10-9 torr). Some naturally occurring calcite has apparent utility as a reference material. For example, equigranular calcite from some zones of carbonatite intrusions (sovites) and recrystallized calcites from highly metamorphosed metallic ore deposits. Most calcite marbles, though possibly appropriate as Sr standards, show substantial inhomogeneity in Mg, Mn and Ba. Some hydrothermal “Iceland Spar” calcite may prove useful as a reference for extremely low concentrations of Mg, Sr and Ba. The best carbonatitic calcites currently in use appear homogeneous to

  17. NAA study on homogeneity of reference materials and their suitability for microanalytical techniques

    International Nuclear Information System (INIS)

    Dybczynski, R.; Danko, B.; Polkowska-Motrenko, H.

    2000-01-01

    Homogeneity of the existing (Virginia Tobacco Leaves CTA-VTL-2 (ICHTJ), Apatite Concentrate CTA-AC-1 (ICHTJ), Fine Fly Ash CTA-FFA-1 (ICHTJ)) and candidate certified reference materials (CRMs) (IAEA-338 Lichen, IAEA-413 Algae, Spruce Shoots RMF II (Germany)) was studied by neutron activation analysis (NAA). Several samples of small mass (ca. 1 or 10 mg) taken from various containers were analyzed by instrumental NAA and the results for several elements were compared by Fishers's test and t-test with analogous series of results for samples taken from one container. In the second approach, sampling variance was estimated for some elements from overall variance and the components of analytical variance. The results were interpreted with the aid of Ingamells' sampling constant. Particle size distribution of the reference materials was also measured by several techniques. In addition quantitative determinations for some elements were performed and results compared with the certified values. The results of the present study were discussed with reference to suitability of CRMs to microanalytical techniques. It was pointed out that the term 'microanalysis' itself is not always unequivocally understood and used. (author)

  18. The use of reference materials in quality assurance programmes in food microbiology laboratories.

    Science.gov (United States)

    In't Veld, P H

    1998-11-24

    Nine different reference materials (RMs) for use in food and water microbiology have been developed with the support of the European Commission (EC). The production process of RMs is based on spray drying bacteria suspended in milk. The highly contaminated milk powder (HCMP) obtained is mixed with sterile milk powder to achieve the desired level of contamination and is subsequently filled into gelatine capsules. The HCMP may need to be stabilised by storage for more than a year before a stable RM can be prepared. The HCMP are mixed with sterile milk powder using a pestle and mortar in order to produce homogeneous RMs. For routine use of RMs Shewhart control charts can be produced. Based on log10 transformed counts, control limits are calculated. Rules for the interpretation of results facilitate the detection of out of control situations. Besides RMs there are also CRMs (Certified Reference Materials) that are certified by the EC Community Bureau of Reference (BCR) and are intended for occasional use. Based on the BCR certificate, user tables are produced presenting the 95% confidence limits for the number of capsules likely to be examined in practice. Also power analysis is made to indicate the minimum difference between the certified value and the observed geometric mean value in relation to the number of capsules examined.

  19. DEVELOPMENT OF THE REFERENCE MATERIALS PRODUCTION BRANCH IN THE JOINT STOCK COMPANY "THE GULIDOV KRASNOYARSK NON-FERROUS METALS PLANT"

    Directory of Open Access Journals (Sweden)

    K. A. Shatnykh

    2015-01-01

    Full Text Available The article deals with the development of the branch for the reference materials production in the Joint Stock Company "The Gulidov Krasnoyarsk Non-Ferrous Metals Plant" (JSC "Krastsvetmet". Here the most important workings for reference materials including the work for the London precious metal exchange, current and future works are stated.

  20. Bias in the absorption coefficient determination of a fluorescent dye, standard reference material 1932 fluorescein solution

    International Nuclear Information System (INIS)

    DeRose, Paul C.; Kramer, Gary W.

    2005-01-01

    The absorption coefficient of standard reference material[registered] (SRM[registered]) 1932, fluorescein in a borate buffer solution (pH=9.5) has been determined at λ=488.0, 490.0, 490.5 and 491.0 nm using the US national reference UV/visible spectrophotometer. The purity of the fluorescein was determined to be 97.6% as part of the certification of SRM 1932. The solution measured was prepared gravimetrically by diluting SRM 1932 with additional borate buffer. The value of the absorption coefficient was corrected for bias due to fluorescence that reaches the detector and for dye purity. Bias due to fluorescence was found to be on the order of -1% for both monochromatic and polychromatic (e.g., diode-array based) spectrophotometers

  1. Standard reference material certification: contribution of NAA with a TRIGA reactor

    International Nuclear Information System (INIS)

    Orvini, E.; Speziali, M.; Salvini, A.; Herborg, C.

    2002-01-01

    Pavia has cooperative links with the major international agencies devoted to the certification of SRMs or CRMs as the Bureau Communautaire de Reference (BCR), the European Institute for Reference Materials and Measurement (IRMM), the USA National Institute of Standards and Technology (NIST) and the International Atomic Energy Agency (IAEA). During these cooperative works, a large amount of analytical data obtained with NAA has been compared, and meaningful methodological information achieved with respect to accuracy and precision in the analysis of several elements at different concentrations in various matrices. Analytical data on As, Cd, Cr, Co, Cu, Cs, Fe, Zn, K, Sc, U, Th, Al, Sb, Mn, V, Hg, Sr, Rb, Se,Pt, all the Rare Earths and halogens Br, Cl, I, have been obtained and contributed for the final certification

  2. 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.

  3. Report of the consultants meeting on proper use of reference and control materials

    International Nuclear Information System (INIS)

    2002-01-01

    Quality control in analytical laboratories as a basis of a complete quality system needs still to be developed in many Member States. To support the dissemination of information in this field a consultants meeting on 'Proper Use of Reference and Quality Control Materials' was held at the IAEA Headquarters, Vienna, from 13 to 17 August 2001. The experts convened with the objective to prepare a TECDOC to advise analytical laboratories in Member States on the correct use of Certified Reference Materials (CRMs) for Quality Control purposes and give practical recommendations to expand this concept to in-house Quality Control Materials (QCMs). In view of the existing literature in this field an urgent need for a practical guidebook for the preparation and application of cost effective and matrix matching QCMs was identified and the experts tried to fill this gap from their relevant experience. One and a half days of lecturing was followed by intensive discussion and brain storming to create a list of key words, which were structured in a logical order to provide a frame for the projected document. Responsibilities were assigned and deadlines fixed for the submission of the full text. (author)

  4. Certified Reference Material IAEA-448: Soil from Oil Field Contaminated with Technically Enhanced Radium-226

    International Nuclear Information System (INIS)

    2013-01-01

    To ensure reliable evaluation of potential radiological hazards and proper decision making related to radiation protection measures, the IAEA, through the IAEA Environment Laboratories, supports Member State laboratories in their efforts to maintain readiness and to improve the quality of analytical results. It does so by producing reference materials, by developing standardized methods for sample collection and analysis, and by conducting interlaboratory comparisons and proficiency tests as tools for external quality control of analytical results. The problem of naturally occurring radioactive material (NORM) contamination is known to be widespread, occurring in oil and gas production facilities throughout the world. It has become a subject of attention in many IAEA Member States. In response to this radiological concern, facilities in many Member States have been characterizing the nature and extent of NORM in oil and gas installations and in the surrounding environment, evaluating the potential for exposure to workers and the public, and developing methods for properly managing these relatively high massic activity residues. Within this context, the IAEA Environment Laboratories, in cooperation with the Atomic Energy Commission of Syria, an IAEA Collaborating Centre, have prepared a new certified reference material of soil contaminated with NORM, identified as IAEA-448, certified for the massic activity of 226Ra. This report presents the methodologies used for the production and certification of IAEA-448

  5. Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies

    Directory of Open Access Journals (Sweden)

    Kirsi Harju

    2015-11-01

    Full Text Available A saxitoxin (STX proficiency test (PT was organized as part of the Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk (EQuATox project. The aim of this PT was to provide an evaluation of existing methods and the European laboratories’ capabilities for the analysis of STX and some of its analogues in real samples. Homogenized mussel material and algal cell materials containing paralytic shellfish poisoning (PSP toxins were produced as reference sample matrices. The reference material was characterized using various analytical methods. Acidified algal extract samples at two concentration levels were prepared from a bulk culture of PSP toxins producing dinoflagellate Alexandrium ostenfeldii. The homogeneity and stability of the prepared PT samples were studied and found to be fit-for-purpose. Thereafter, eight STX PT samples were sent to ten participating laboratories from eight countries. The PT offered the participating laboratories the possibility to assess their performance regarding the qualitative and quantitative detection of PSP toxins. Various techniques such as official Association of Official Analytical Chemists (AOAC methods, immunoassays, and liquid chromatography-mass spectrometry were used for sample analyses.

  6. Challenges in the size analysis of a silica nanoparticle mixture as candidate certified reference material

    International Nuclear Information System (INIS)

    Kestens, Vikram; Roebben, Gert; Herrmann, Jan; Jämting, Åsa; Coleman, Victoria; Minelli, Caterina; Clifford, Charles; Temmerman, Pieter-Jan De; Mast, Jan; Junjie, Liu; Babick, Frank; Cölfen, Helmut; Emons, Hendrik

    2016-01-01

    A new certified reference material for quality control of nanoparticle size analysis methods has been developed and produced by the Institute for Reference Materials and Measurements of the European Commission’s Joint Research Centre. The material, ERM-FD102, consists of an aqueous suspension of a mixture of silica nanoparticle populations of distinct particle size and origin. The characterisation relied on an interlaboratory comparison study in which 30 laboratories of demonstrated competence participated with a variety of techniques for particle size analysis. After scrutinising the received datasets, certified and indicative values for different method-defined equivalent diameters that are specific for dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS), scanning and transmission electron microscopy (SEM and TEM), atomic force microscopy (AFM), particle tracking analysis (PTA) and asymmetrical-flow field-flow fractionation (AF4) were assigned. The value assignment was a particular challenge because metrological concepts were not always interpreted uniformly across all participating laboratories. This paper presents the main elements and results of the ERM-FD102 characterisation study and discusses in particular the key issues of measurand definition and the estimation of measurement uncertainty.

  7. Development of Candidate Reference Materials of Endosulfan Sulfate and Bifenthrin in Black Tea

    Directory of Open Access Journals (Sweden)

    Nurhani Aryana

    2016-03-01

    Full Text Available The candidate reference materials of endosulfan sulfate and bifenthrin in black tea have been developed according to the requirements of ISO Guide 34 and 35. Preparation of candidate material includes grinding and sieving of the black tea leaves, spiking the black tea powder by both analytes, homogenization, and bottling. Homogeneity and short-term stability test were performed using a GC-µECD instrument. Meanwhile, the characterization was carried out by a collaborative study using both of GC-µECD and GC-MS instruments. The uncertainty budget was evaluated from sample inhomogeneity, short-term instability and variability in the characterization procedure. In a dry mass fraction, endosulfan sulfate was assigned to be 491 µg kg-1 with a relative expanded uncertainty of ± 33.2%, and bifenthrin was assigned to be 937 µg kg-1 with a relative expanded uncertainty of ± 18.5%. The candidate reference materials are aimed to support the need of matrix CRM especially for the measurement of pesticide residue for quality assurance work done by laboratories in Indonesia.

  8. Multivariate methods for analysis of environmental reference materials using laser-induced breakdown spectroscopy

    Directory of Open Access Journals (Sweden)

    Shikha Awasthi

    2017-06-01

    Full Text Available Analysis of emission from laser-induced plasma has a unique capability for quantifying the major and minor elements present in any type of samples under optimal analysis conditions. Chemometric techniques are very effective and reliable tools for quantification of multiple components in complex matrices. The feasibility of laser-induced breakdown spectroscopy (LIBS in combination with multivariate analysis was investigated for the analysis of environmental reference materials (RMs. In the present work, different (Certified/Standard Reference Materials of soil and plant origin were analyzed using LIBS and the presence of Al, Ca, Mg, Fe, K, Mn and Si were identified in the LIBS spectra of these materials. Multivariate statistical methods (Partial Least Square Regression and Partial Least Square Discriminant Analysis were employed for quantitative analysis of the constituent elements using the LIBS spectral data. Calibration models were used to predict the concentrations of the different elements of test samples and subsequently, the concentrations were compared with certified concentrations to check the authenticity of models. The non-destructive analytical method namely Instrumental Neutron Activation Analysis (INAA using high flux reactor neutrons and high resolution gamma-ray spectrometry was also used for intercomparison of results of two RMs by LIBS.

  9. Short-term stability test for thorium soil candidate a reference material

    Energy Technology Data Exchange (ETDEWEB)

    Clain, Almir F.; Fonseca, Adelaide M.G.; Dantas, Vanessa V.D.B.; Braganca, Maura J.C.; Souza, Poliana S., E-mail: almir@ird.gov.br, E-mail: adelaide@ird.gov.br, E-mail: vanessa@ird.gov.br, E-mail: maura@ird.gov.br, E-mail: poliana@bolsista.ird.gov.br [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2015-07-01

    This work describes a methodology to determine the soil short-term stability after the steps of production in laboratory. The short-term stability of the soil is an essential property to be determined in order to producing a reference material. The soil is a candidate of reference material for chemical analysis of thorium with metrological traceability to be used in environmental analysis, equipment calibration, validation methods, and quality control. A material is considered stable in a certain temperature if the property of interest does not change with time, considering the analytical random fluctuations. Due to this, the angular coefficient from the graphic of Th concentration versus elapsed time must be near to zero. The analytical determinations of thorium concentration were performed by Instrumental Neutron activation Analysis. The slopes and their uncertainties were obtained from the regression lines at temperatures of 20 deg C and 60 deg C, with control temperature of -20 deg C. From the obtained data a t-test was applied. In both temperatures the calculated t-value was lower than the critical value, so we can conclude with 95% confidence level that no significant changes happened during the period studied concerning thorium concentration in soil at temperatures of 20 deg C and 60 deg C, showing stability at these temperatures. (author)

  10. Evaluation of a fungal collection as certified reference material producer and as a biological resource center

    Directory of Open Access Journals (Sweden)

    Tatiana Forti

    2016-06-01

    Full Text Available Abstract Considering the absence of standards for culture collections and more specifically for biological resource centers in the world, in addition to the absence of certified biological material in Brazil, this study aimed to evaluate a Fungal Collection from Fiocruz, as a producer of certified reference material and as Biological Resource Center (BRC. For this evaluation, a checklist based on the requirements of ABNT ISO GUIA34:2012 correlated with the ABNT NBR ISO/IEC17025:2005, was designed and applied. Complementing the implementation of the checklist, an internal audit was performed. An evaluation of this Collection as a BRC was also conducted following the requirements of the NIT-DICLA-061, the Brazilian internal standard from Inmetro, based on ABNT NBR ISO/IEC 17025:2005, ABNT ISO GUIA 34:2012 and OECD Best Practice Guidelines for BRCs. This was the first time that the NIT DICLA-061 was applied in a culture collection during an internal audit. The assessments enabled the proposal for the adequacy of this Collection to assure the implementation of the management system for their future accreditation by Inmetro as a certified reference material producer as well as its future accreditation as a Biological Resource Center according to the NIT-DICLA-061.

  11. Evaluation of a fungal collection as certified reference material producer and as a biological resource center.

    Science.gov (United States)

    Forti, Tatiana; Souto, Aline da S S; do Nascimento, Carlos Roberto S; Nishikawa, Marilia M; Hubner, Marise T W; Sabagh, Fernanda P; Temporal, Rosane Maria; Rodrigues, Janaína M; da Silva, Manuela

    2016-01-01

    Considering the absence of standards for culture collections and more specifically for biological resource centers in the world, in addition to the absence of certified biological material in Brazil, this study aimed to evaluate a Fungal Collection from Fiocruz, as a producer of certified reference material and as Biological Resource Center (BRC). For this evaluation, a checklist based on the requirements of ABNT ISO GUIA34:2012 correlated with the ABNT NBR ISO/IEC17025:2005, was designed and applied. Complementing the implementation of the checklist, an internal audit was performed. An evaluation of this Collection as a BRC was also conducted following the requirements of the NIT-DICLA-061, the Brazilian internal standard from Inmetro, based on ABNT NBR ISO/IEC 17025:2005, ABNT ISO GUIA 34:2012 and OECD Best Practice Guidelines for BRCs. This was the first time that the NIT DICLA-061 was applied in a culture collection during an internal audit. The assessments enabled the proposal for the adequacy of this Collection to assure the implementation of the management system for their future accreditation by Inmetro as a certified reference material producer as well as its future accreditation as a Biological Resource Center according to the NIT-DICLA-061. Copyright © 2016 Sociedade Brasileira de Microbiologia. Published by Elsevier Editora Ltda. All rights reserved.

  12. Challenges in the size analysis of a silica nanoparticle mixture as candidate certified reference material

    Energy Technology Data Exchange (ETDEWEB)

    Kestens, Vikram, E-mail: vikram.kestens@ec.europa.eu; Roebben, Gert [Joint Research Centre (JRC), European Commission, Institute for Reference Materials and Measurements (IRMM) (Belgium); Herrmann, Jan; Jämting, Åsa; Coleman, Victoria [National Measurement Institute Australia, Nanometrology Section (Australia); Minelli, Caterina; Clifford, Charles [National Physical Laboratory, Analytical Science Division (United Kingdom); Temmerman, Pieter-Jan De; Mast, Jan [Service Electron Microscopy, Veterinary and Agrochemical Research Centre (CODA-CERVA) (Belgium); Junjie, Liu [National Institute of Metrology, Division of Nanoscale Measurement and Advanced Materials (China); Babick, Frank [Technische Universität Dresden, Institut für Verfahrens- und Umwelttechnik (Germany); Cölfen, Helmut [University of Konstanz, Physical Chemistry, Department of Chemistry (Germany); Emons, Hendrik [Joint Research Centre (JRC), European Commission, Institute for Reference Materials and Measurements (IRMM) (Belgium)

    2016-06-15

    A new certified reference material for quality control of nanoparticle size analysis methods has been developed and produced by the Institute for Reference Materials and Measurements of the European Commission’s Joint Research Centre. The material, ERM-FD102, consists of an aqueous suspension of a mixture of silica nanoparticle populations of distinct particle size and origin. The characterisation relied on an interlaboratory comparison study in which 30 laboratories of demonstrated competence participated with a variety of techniques for particle size analysis. After scrutinising the received datasets, certified and indicative values for different method-defined equivalent diameters that are specific for dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS), scanning and transmission electron microscopy (SEM and TEM), atomic force microscopy (AFM), particle tracking analysis (PTA) and asymmetrical-flow field-flow fractionation (AF4) were assigned. The value assignment was a particular challenge because metrological concepts were not always interpreted uniformly across all participating laboratories. This paper presents the main elements and results of the ERM-FD102 characterisation study and discusses in particular the key issues of measurand definition and the estimation of measurement uncertainty.

  13. Report of the consultants meeting on proper use of reference and control materials

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2002-07-01

    Quality control in analytical laboratories as a basis of a complete quality system needs still to be developed in many Member States. To support the dissemination of information in this field a consultants meeting on 'Proper Use of Reference and Quality Control Materials' was held at the IAEA Headquarters, Vienna, from 13 to 17 August 2001. The experts convened with the objective to prepare a TECDOC to advise analytical laboratories in Member States on the correct use of Certified Reference Materials (CRMs) for Quality Control purposes and give practical recommendations to expand this concept to in-house Quality Control Materials (QCMs). In view of the existing literature in this field an urgent need for a practical guidebook for the preparation and application of cost effective and matrix matching QCMs was identified and the experts tried to fill this gap from their relevant experience. One and a half days of lecturing was followed by intensive discussion and brain storming to create a list of key words, which were structured in a logical order to provide a frame for the projected document. Responsibilities were assigned and deadlines fixed for the submission of the full text. (author)

  14. Short-term stability test for thorium soil candidate a reference material

    International Nuclear Information System (INIS)

    Clain, Almir F.; Fonseca, Adelaide M.G.; Dantas, Vanessa V.D.B.; Braganca, Maura J.C.; Souza, Poliana S.

    2015-01-01

    This work describes a methodology to determine the soil short-term stability after the steps of production in laboratory. The short-term stability of the soil is an essential property to be determined in order to producing a reference material. The soil is a candidate of reference material for chemical analysis of thorium with metrological traceability to be used in environmental analysis, equipment calibration, validation methods, and quality control. A material is considered stable in a certain temperature if the property of interest does not change with time, considering the analytical random fluctuations. Due to this, the angular coefficient from the graphic of Th concentration versus elapsed time must be near to zero. The analytical determinations of thorium concentration were performed by Instrumental Neutron activation Analysis. The slopes and their uncertainties were obtained from the regression lines at temperatures of 20 deg C and 60 deg C, with control temperature of -20 deg C. From the obtained data a t-test was applied. In both temperatures the calculated t-value was lower than the critical value, so we can conclude with 95% confidence level that no significant changes happened during the period studied concerning thorium concentration in soil at temperatures of 20 deg C and 60 deg C, showing stability at these temperatures. (author)

  15. Nanomaterials for environmental studies: Classification, reference material issues, and strategies for physico-chemical characterisation

    Energy Technology Data Exchange (ETDEWEB)

    Stone, Vicki, E-mail: v.stone@napier.ac.uk [School of Life Sciences, Edinburgh Napier University, 10 Colinton Road, Edinburgh EH10 5DT (United Kingdom); Nowack, Bernd [Materials, Products and the Environment Group, Empa - Swiss Federal Laboratories for Materials Testing and Research, Lerchenfeldstrasse 5 CH - 9014 St. Gallen (Switzerland); Baun, Anders [Department of Environmental Engineering, Technical University of Denmark, NanoDTU, Building 113, 2800 Kgs. Lyngby (Denmark); Brink, Nico van den [Alterra, P.O. Box 47, 6700 AA Wageningen (Netherlands); Kammer, Frank von der [Department of Environmental Geosciences, Vienna University, Althanstrasse 14, Wien 1090 (Austria); Dusinska, Maria [Health Effects Laboratory, Centre for Ecological Economics, Norwegian Institute for Air Research (NILU), Instituttveien, 18, 2027 Kjeller (Norway); Handy, Richard [University of Plymouth, Davy Building, Drake Circus, Plymouth PL4 8AA (United Kingdom); Hankin, Steven [Institute of Occupational Medicine, Research Avenue North, Riccarton, Edinburgh EH14 4AP (United Kingdom); Hasselloev, Martin [Department of Chemistry, Environmental Nanoparticle Research Group, Goeteborg University, SE-412 96 Goeteborg (Sweden); Joner, Erik [Bioforsk Soil and Environment, Fredrik A Dahls vei 20, N-1432 Aas (Norway); Fernandes, Teresa F. [School of Life Sciences, Edinburgh Napier University, 10 Colinton Road, Edinburgh EH10 5DT (United Kingdom)

    2010-03-01

    NanoImpactNet is a European Commission Framework Programme 7 (FP7) funded project that provides a forum for the discussion of current opinions on nanomaterials in relation to human and environmental issues. In September 2008, in Zurich, a NanoImpactNet environmental workshop focused on three key questions: 1.What properties should be characterised for nanomaterials used in environmental and ecotoxicology studies? 2.What reference materials should be developed for use in environmental and ecotoxicological studies? 3.Is it possible to group different nanomaterials into categories for consideration in environmental studies? Such questions have been, at least partially, addressed by other projects/workshops especially in relation to human health effects. Such projects provide a useful basis on which this workshop was based, but in this particular case these questions were reformulated in order to focus specifically on environmental studies. The workshop participants, through a series of discussion and reflection sessions, generated the conclusions listed below. The physicochemical characterisation information identified as important for environmental studies included measures of aggregation/agglomeration/dispersability, size, dissolution (solubility), surface area, surface charge, surface chemistry/composition, with the assumption that chemical composition would already be known. There is a need to have test materials for ecotoxicology, and several substances are potentially useful, including TiO{sub 2} nanoparticles, polystyrene beads labelled with fluorescent dyes, and silver nanoparticles. Some of these test materials could then be developed into certified reference materials over time. No clear consensus was reached regarding the classification of nanomaterials into categories to aid environmental studies, except that a chemistry-based classification system was a reasonable starting point, with some modifications. It was suggested, that additional work may be

  16. Nanomaterials for environmental studies: Classification, reference material issues, and strategies for physico-chemical characterisation

    International Nuclear Information System (INIS)

    Stone, Vicki; Nowack, Bernd; Baun, Anders; Brink, Nico van den; Kammer, Frank von der; Dusinska, Maria; Handy, Richard; Hankin, Steven; Hasselloev, Martin; Joner, Erik; Fernandes, Teresa F.

    2010-01-01

    NanoImpactNet is a European Commission Framework Programme 7 (FP7) funded project that provides a forum for the discussion of current opinions on nanomaterials in relation to human and environmental issues. In September 2008, in Zurich, a NanoImpactNet environmental workshop focused on three key questions: 1.What properties should be characterised for nanomaterials used in environmental and ecotoxicology studies? 2.What reference materials should be developed for use in environmental and ecotoxicological studies? 3.Is it possible to group different nanomaterials into categories for consideration in environmental studies? Such questions have been, at least partially, addressed by other projects/workshops especially in relation to human health effects. Such projects provide a useful basis on which this workshop was based, but in this particular case these questions were reformulated in order to focus specifically on environmental studies. The workshop participants, through a series of discussion and reflection sessions, generated the conclusions listed below. The physicochemical characterisation information identified as important for environmental studies included measures of aggregation/agglomeration/dispersability, size, dissolution (solubility), surface area, surface charge, surface chemistry/composition, with the assumption that chemical composition would already be known. There is a need to have test materials for ecotoxicology, and several substances are potentially useful, including TiO 2 nanoparticles, polystyrene beads labelled with fluorescent dyes, and silver nanoparticles. Some of these test materials could then be developed into certified reference materials over time. No clear consensus was reached regarding the classification of nanomaterials into categories to aid environmental studies, except that a chemistry-based classification system was a reasonable starting point, with some modifications. It was suggested, that additional work may be required

  17. Historical changes in 239Pu and 240Pu sources in sedimentary records in the East China Sea: Implications for provenance and transportation

    DEFF Research Database (Denmark)

    Wang, Jinlong; Baskaran, Mark; Hou, Xiaolin

    2017-01-01

    from 0.158 to 0.297 and were mostly higher than the mean global fallout value of 0.18. The 239,240Pu inventories in the ECS varied widely, from 2 to 807 Bqm−2, with the highest values commonly found in the coastal areas. In the Yangtze Estuary, the mean 239+240Pu activity concentration is close...... to the estimated value of the suspended material from the Yangtze River catchment (0.18 Bqkg−1), and the 240Pu/239Pu atom ratio was found to be ∼0.18, which indicates that the Yangtze River input is the dominant source of Pu for this area. The total annual Yangtze River input of 239+240Pu was estimated to be 2...

  18. Development of saw palmetto (Serenoa repens) fruit and extract standard reference materials.

    Science.gov (United States)

    Schantz, Michele M; Bedner, Mary; Long, Stephen E; Molloy, John L; Murphy, Karen E; Porter, Barbara J; Putzbach, Karsten; Rimmer, Catherine A; Sander, Lane C; Sharpless, Katherine E; Thomas, Jeanice B; Wise, Stephen A; Wood, Laura J; Yen, James H; Yarita, Takashi; NguyenPho, Agnes; Sorenson, Wendy R; Betz, Joseph M

    2008-10-01

    As part of a collaboration with the National Institutes of Health's Office of Dietary Supplements and the Food and Drug Administration's Center for Drug Evaluation and Research, the National Institute of Standards and Technology has developed two standard reference materials (SRMs) representing different forms of saw palmetto (Serenoa repens), SRM 3250 Serenoa repens fruit and SRM 3251 Serenoa repens extract. Both of these SRMs have been characterized for their fatty acid and phytosterol content. The fatty acid concentration values are based on results from gas chromatography with flame ionization detection (GC-FID) and mass spectrometry (GC/MS) analysis while the sterol concentration values are based on results from GC-FID and liquid chromatography with mass spectrometry analysis. In addition, SRM 3250 has been characterized for lead content, and SRM 3251 has been characterized for the content of beta-carotene and tocopherols. SRM 3250 (fruit) has certified concentration values for three phytosterols, 14 fatty acids as triglycerides, and lead along with reference concentration values for four fatty acids as triglycerides and 16 free fatty acids. SRM 3251 (extract) has certified concentration values for three phytosterols, 17 fatty acids as triglycerides, beta-carotene, and gamma-tocopherol along with reference concentration values for three fatty acids as triglycerides, 17 fatty acids as free fatty acids, beta-carotene isomers, and delta-tocopherol and information values for two phytosterols. These SRMs will complement other reference materials currently available with concentrations for similar analytes and are part of a series of SRMs being developed for dietary supplements.

  19. Status of 239Pu evaluations

    International Nuclear Information System (INIS)

    Kawano, Toshihiko; Talou, Patrick; Chadwick, Mark B.

    2014-01-01

    This paper summarises the current status of nuclear data evaluations for n+ 239 Pu. The nuclear data we address include fission, capture, scattering cross-sections, as well as the prompt fission neutron energy spectrum, which has large sensitivities to the criticality benchmark testing. The evaluated nuclear data files currently available for 239 Pu are compared, and the source of differences in the cross-sections are discussed. Some open questions on the statistical model calculations for deformed systems are also given. (authors)

  20. Determination of Natural Levels of Radionuclides in Proposed Mushroom Reference Material (A Proficiency Test Exercise)

    International Nuclear Information System (INIS)

    Waheed, S.; Rahman, A.; Siddique, N.; Ahmad, S.; Zaidi, J.H.

    2006-08-01

    A proficiency test (PT) was organized within the framework of international Atomic Energy Agency (IAEA) project INT/1/054, entitled 'Preparation' of Reference Materials and Organization of Proficiency Test Rounds'. This exercise served to estimate the proficiency of the analytical laboratories from participating countries. This report presents the results of the proficiency test exercise on the proposed Mushroom Reference Material for the determination of natural levels of radionuclides. Laboratories from 6 different countries submitted data on the following three radionuclides: /sup 134/Cs, /sup 137/Cs, /sup 40/K. Results for /sup 134/Cs, 137/sup 137/Cs, and /sup 40/K in the mushroom reference material were reported by three or more participating laboratories and could be subjected to statistical evaluation. The original data of these raionuclides was subjected to a computer program 'Histo Vession 2.1' provided by IAEA. The four outlier tests i.e. Dixon, Grubbs, Skewness and Kurtosis were applied to the data sets. All values for these three radionuclides were accepted by the software. Consensus (overall) mean value, absolute standard deviation, relative standard deviation, standard error, median and range of values for these three radionuclides have been are obtained (at significance level 0.05). the consensus mean values and confidence intervals are given./sup 134/Cs: 4.4 Bq/kg (3.4-5.3 Bq/kg) /sup 137/Cs: 2899 Bq/kg (2740-3058 Bq/kg) /sup 40/K: 1136 Bq/kg (1046-1226 Bq/kg). (author)

  1. Value determination of ZrO2 in-house reference material (RM) candidate

    International Nuclear Information System (INIS)

    Susanna Tuning Sunanti; Samin; Supriyanto C

    2013-01-01

    The value determination of zirconium oxide in-house reference materials (RM) candidate has been done by referring to ISO:35-2006 standard. The raw material of RM was 4 kg of ZrO 2 , Merck, that was dried at 90°C for 2×6 hours in a closed room. The samples were crushed with stainless steel (SS) pestle to pass ≤ 200 mesh sieve, homogenized in a homogenizer for 3×6 hours to obtain the powdered, dried and homogenous samples. The gravimetric method was performed to test the moisture content, while XRF and AAS methods were used to test the homogeneity and stability of samples candidates. Reference material (RM) candidates of ZrO 2 powder were put into polyethylene bottles, each weighing 100 g. Samples were distributed to 10 testing laboratories that have been accredited for testing the composition of the oxide contents and loss of ignition (LOI) using variety of analytical methods that have been validated such as AAS, XRF, NAA, and UV-Vis. The testing results of oxide content and loss of ignition parameters from various laboratories were analyzed using statistical methods. The testing data of oxide concentration in zirconium oxide RM candidates obtained from various laboratories were ZrO 2 : 97.7334 ± 0.0016%, HfO 2 : 1.7329 ± 0.0024%, SiO 2 : 30.1224 ± 0.0053%, Al 2 O 3 : 0.0245 ± 0.0015%, TiO 2 : 0.0153 ± 0.0006%, Fe 2 O 3 : 0.0068 ± 0.0005%, CdO: 3.1798 ± 0.00006 ppm, and the LOI results was = 0.0217 ± 0.00022%. (author)

  2. 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.

  3. Spiked environmental matrix for use as a reference material for gamma-ray spectrometry: Production and homogeneity test

    International Nuclear Information System (INIS)

    Sobiech-Matura, K.; Máté, B.; Altzitzoglou, T.

    2016-01-01

    The application of a spiking method for reference material production and its utilisation for a food matrix is presented. The raw rice powder was tested by means of γ-ray spectrometry and spiked with a "1"3"7Cs solution. The spiked material was mixed and tested for homogeneity. The future use of the rice powder reference material after the entire characterisation cycle will be for γ-ray spectrometry method validation. - Highlights: • Spiking blank substance with a traceable radioactive solution • Spiked reference material for γ-ray emitting radionuclides in food matrix • Results of the homogeneity tests are presented

  4. Characterisation of candidate reference materials by PIXE analysis and nuclear microprobe PIXE imaging

    International Nuclear Information System (INIS)

    Jaksic, M.; Pastuovic, Z.; Bogdanovic, I.; Tadic, T.

    2002-01-01

    In order to test whether some candidate reference materials show homogeneity that can satisfy quality control of the PIXE technique, six bottles of each of the two Candidate RM's - Lichen (IAEA 338) and Algae (IAEA 413) were tested. Four different tests were performed. First, two pellets from each bottle were prepared and analysed using broad beam (φ = 5 mm) PIXE. Second and third was analysis of homogeneity using scanning focussed beam at the nuclear microprobe. Scans of 50x50 μm 2 and 240x260 μm 2 were performed. Finally, individual grains with composition differing from the rest of the sample, were analysed using PIXE and RBS. (author)

  5. 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.)

  6. Certified reference materials of agricultural products and foods bearing radioactivity from the Fukushima nuclear accident

    International Nuclear Information System (INIS)

    Minai, Y.; Miura, T.; Yonezawa, C.; Iwamoto, H.; Shibukawa, M.; Takagai, Y.; Furukawa, M.; Arakawa, F.; Okada, Y.; Kakita, K.

    2016-01-01

    Certified reference materials (CRMs) for food analysis were developed in an inter-laboratory experiment for validation of measurement of radiocesium in foodstuffs. Since 2012, five series of CRMs were developed, including for brown rice grain, soybean powder, beef flake, shiitake mushroom powder and marine fish (meat and bone parts). This paper discusses the strategy of development, including choice of CRMs developed and the preparation and certification procedures applied for CRM development. In particular, some detailed data are presented for the most popular CRMs developed: brown rice grain, soybean powder and beef flake. (author)

  7. 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...

  8. Determination of silicon in biological and botanical reference materials by epithermal INAA and Compton suppression

    International Nuclear Information System (INIS)

    Landsberger, S.; Peshev, S.; Becker, D.A.

    1994-01-01

    Silicon determination in sixteen botanical and biological standard reference materials is described using the 29 Si(n, p) 29 Al reaction through instrumental epithermal neutron activation analysis and Compton suppression gamma-ray spectroscopy. By simultaneous utilization of both cadmium and boron epithermal filters along with anticoincidence gamma-counting, detection limits as low as 12 ppm were obtained for certain matrices, much lower than previously reported values for this type of analysis. The method is applicable to many botanical and biological matrices and is attractive with its interference free, purely instrumental nature, compared with methods using the 28 Si(n, p) 28 Al reaction or chemical separation techniques. ((orig.))

  9. Fundamental studies to develop certified reference material to calibrate spectrophotometer in the ultraviolet region

    International Nuclear Information System (INIS)

    Da Conceição, F C; Borges, P P; Gomes, J F S

    2016-01-01

    Spectrophotometry is the technique used in a great number of laboratories around the world. Quantitative determination of a high number of inorganic, organic and biological species can be made by spectrophotometry using calibrated spectrophotometers. International standards require the use of optical filters to perform the calibration of spectrophotometers. One of the recommended materials is the crystalline potassium dichromate (K_2Cr_2O_7), which is used to prepare solutions in specific concentrations for calibration or verification of spectrophotometers in the ultraviolet (UV) spectral regions. This paper presents the results concerning the fundamental studies for developing a certified reference material (CRM) of crystalline potassium dichromate to be used as standard of spectrophotometers in order to contribute to reliable quantitative analyses. (paper)

  10. Development of a certified reference material for specific surface area of quartz sand

    Directory of Open Access Journals (Sweden)

    Egor P Sobina

    2017-01-01

    Full Text Available The paper presents results of conducting research on the development of a certified reference material (CRM for specific surface area of quartz sand, which is practically non-porous and therefore has low specific surface area value ~ 0.8 m2/g. The standard uncertainty due to RM inhomogeneity, the standard uncertainty due to RM instability, as well as the standard uncertainty due to characterization were estimated using the State Primary Standard GET 210‑2014 for Units of Specific Absorption of Gases, Specific Surface Area, Specific Volume, and Pore Size of Solid Substances and Materials. The metrological characteristics of the CRM were determined using a low-temperature gas adsorption method. Krypton was used as an adsorbate to increase measurement accuracy.

  11. Utilizing a reference material for assessing absolute tumor mechanical properties in modality independent elastography

    Science.gov (United States)

    Kim, Dong Kyu; Weis, Jared A.; Yankeelov, Thomas E.; Miga, Michael I.

    2014-03-01

    There is currently no reliable method for early characterization of breast cancer response to neoadjuvant chemotherapy (NAC) [1,2]. Given that disruption of normal structural architecture occurs in cancer-bearing tissue, we hypothesize that further structural changes occur in response to NAC. Consequently, we are investigating the use of modalityindependent elastography (MIE) [3-8] as a method for monitoring mechanical integrity to predict long term outcomes in NAC. Recently, we have utilized a Demons non-rigid image registration method that allows 3D elasticity reconstruction in abnormal tissue geometries, making it particularly amenable to the evaluation of breast cancer mechanical properties. While past work has reflected relative elasticity contrast ratios [3], this study improves upon that work by utilizing a known stiffness reference material within the reconstruction framework such that a stiffness map becomes an absolute measure. To test, a polyvinyl alcohol (PVA) cryogel phantom and a silicone rubber mock mouse tumor phantom were constructed with varying mechanical stiffness. Results showed that an absolute measure of stiffness could be obtained based on a reference value. This reference technique demonstrates the ability to generate accurate measurements of absolute stiffness to characterize response to NAC. These results support that `referenced MIE' has the potential to reliably differentiate absolute tumor stiffness with significant contrast from that of surrounding tissue. The use of referenced MIE to obtain absolute quantification of biomarkers is also translatable across length scales such that the characterization method is mechanics-consistent at the small animal and human application.

  12. Development and application of a general plasmid reference material for GMO screening.

    Science.gov (United States)

    Wu, Yuhua; Li, Jun; Wang, Yulei; Li, Xiaofei; Li, Yunjing; Zhu, Li; Li, Jun; Wu, Gang

    The use of analytical controls is essential when performing GMO detection through screening tests. Additionally, the presence of taxon-specific sequences is analyzed mostly for quality control during GMO detection. In this study, 11 commonly used genetic elements involving three promoters (P-35S, P-FMV35S and P-NOS), four marker genes (Bar, NPTII, HPT and Pmi), and four terminators (T-NOS, T-35S, T-g7 and T-e9), together with the reference gene fragments from six major crops of maize, soybean, rapeseed, rice, cotton and wheat, were co-integrated into the same single plasmid to construct a general reference plasmid pBI121-Screening. The suitability test of pBI121-Screening plasmid as reference material indicated that the non-target sequence on the pBI121-Screening plasmid did not affect the PCR amplification efficiencies of screening methods and taxon-specific methods. The sensitivity of screening and taxon-specific assays ranged from 5 to 10 copies of pBI121-Screening plasmid, meeting the sensitivity requirement of GMO detection. The construction of pBI121-Screening solves the lack of a general positive control for screening tests, thereby reducing the workload and cost of preparing a plurality of the positive control. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Multielement analysis of rice flour-unpolished reference material by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Suzuki, Shogo; Hirai, Shoji

    1990-01-01

    Trace elements in NIES certified reference material No. 10-a∼10-c Rice Flour-Unpolished, prepared by the National Institute for Environmental Studies of Japan (NIES), were determined by instrumental neutron activation analysis (INAA). A set of three samples with different Cd concentration levels was subjected to analyses. Portions of each sample (ca. 200∼1000 mg) were irradiated, either with thermal neutrons without cadmium filter or with epithermal neutrons with cadmium filter, in the Musashi Institute of Technology Research Reactor (MITRR). The activated samples were analyzed by the three methods; conventional γ-ray spectrometry using a coaxial Ge detector, anticoincidence counting spectrometry, and coincidence counting spectrometry using a coaxial Ge detector and a well type NaI(Tl) detector. Concentrations of 26∼28 elements were determined by these methods. The values obtained for many elements, except for Mg and K, were in good agreement with those of the NIES certified and reference. Concentrations of 10 elements (S, Sc, V, Ag, Sb, Cs, Ba, La, Sm, Th), whose certified or reference values are not available from NIES, were also determined in this work. (author)

  14. 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)

  15. Final certification of two new reference materials for inorganic trace analysis

    International Nuclear Information System (INIS)

    Dybczynski, R.; Danko, B.; Kulisa, K.; Chajduk-Maleszewska, E.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z.

    2004-01-01

    Two new biological reference materials for inorganic trace analysis: Tea Leaves (INCT-TL-1) and Mixed Polish Herbs (INCT-MPH-2) were prepared and certified at the Institute of Nuclear Chemistry and Technology (INCT), Warsaw, employing the general strategy of the preparation and certification of CRMs developed in INCT. For both materials ca 40 kg of ground, sieved and carefully homogenized fraction of nominal particle size ≤ 67 mm was obtained. Homogeneity of the materials studied by INAA was shown to be good for samples of masses: m ≥ 100 mg but further investigations indicate that for most of elements these materials can be considered homogeneous down to masses of ca 5 mg or perhaps even lower. The certification was based on results of a worldwide interlaboratory comparison, in which 109 laboratories from 19 countries participated. The results of the analysis of a CRM, which was sent and analyzed along with intercomparison samples and the identity of which was known only to the organizers, were utilized in the process of certification. In addition selected elements were analyzed also by definitive methods based on RNAA. The content of more than 30 elements could be certified in each of the new CRMs. Analytical uncertainties and stability uncertainties were quantified to arrive at combined uncertainties of the certified values. In addition information values were provided for some other elements. (author)

  16. Prepare of microanalysis reference material for nuclear analysis of Chinese ancient ceramic

    International Nuclear Information System (INIS)

    Feng Songlin; Xu Qing; Feng Xiangqian; Fan Dongyu; Lei Yong; Cheng Lin

    2005-01-01

    Some analytic technique can play important role for identifying the provenance and age of ceramic ware. However, it is usually not allowed to destructive analyze for a valuable intact porcelain ware. These analysis methods such as X-ray Fluorescence (XRF), Proton Induced X-ray Emission (PIXE), and Synchrotron Radiation X-ray Fluorescence (SRXRF) are suitable for nondestructive analysis of ancient ceramic wares. In order to compare the analytic data obtained by different measuring method and identify the provenance and age accurately, the effective way is to calibrate elemental concentration in body and glaze of ceramic ware. Microanalysis reference material (MRM) of ancient ceramic has to be prepared for achieving quantitative analysis. A solid powder 99% in size of 500 mesh for microanalysis reference material (MRM) has being prepared in institute of high energy physics. The minimum analytic masses of 1 mg were determined by Neutron Activation Analysis (NAA) for these elements (Sc, Cr, Co, Rb: Cs, La, Ce, Nd, Sm, Tb, Yb, Lu; Hf, Ta, Th, U), and by SRXRF for elements (K, Ca, Ti, Mn, Fe, Zn; Rb, Sr).

  17. Neutron activation analysis of trace elements in a marine sediment reference material

    International Nuclear Information System (INIS)

    Esquivel, D.; Eguren, L.; Montoya, E.

    1993-01-01

    As part of the second intercomparison run of ARCAL-IV, it was analyzed the marine sediment, reference materials PACS-NR CC1 by INAA, in the RP-10 Reactor with a thermal flux of 7,8 x 10 13 n/cm 2 s. The results obtained (± 1σ,n=4) were: Co: 17,2±0,8 ppm; Cr:97,8±0,6 ppm; Fe: 46,0± 0,7 ppm; Na: 31,0±1,09/kg; Sb: 175±5 ppm; in good agreement with the certified values. The results in ppm (±18,n=4), for non certified elements were:Ba: 730±58; Ce: 25±3; Cs: 3,8±0,8; Eu: 1,00±0,03; Hf: 3,30±0,07; Lu:0,25±0,04; Rb: 44,0±0,9; Sc: 14,40±0,04; Sm: 3,4±0,5; Ta: 0,60±0,03; Tb: 0,5±0,05; Th: 3,80±0,02; U: 2,6±0,4; which are in good agreement with other three Latin American and one European INAA Laboratories. It was used the comparative method with AGV-1, GSP-1 and G-2 , USGS reference materials, as standards. (authors). 7 refs., 4 tabs

  18. Preparation and certification of arsenate [As(V)] reference material, NMIJ CRM 7912-a.

    Science.gov (United States)

    Narukawa, Tomohiro; Kuroiwa, Takayoshi; Narushima, Izumi; Jimbo, Yasujiro; Suzuki, Toshihiro; Chiba, Koichi

    2010-05-01

    Arsenate [As(V)] solution reference material, National Metrology Institute of Japan (NMIJ) certified reference material (CRM) 7912-a, for speciation of arsenic species was developed and certified by NMIJ, the National Institute of Advanced Industrial Science and Technology. High-purity As(2)O(3) reagent powder was dissolved in 0.8 M HNO(3) solution and As(III) was oxidized to As(V) with HNO(3) to prepare 100 mg kg(-1) of As(V) candidate CRM solution. The solution was bottled in 400 bottles (50 mL each). The concentration of As(V) was determined by four independent analytical techniques-inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectrometry, graphite furnace atomic absorption spectrometry, and liquid chromatography inductively coupled plasma mass spectrometry-according to As(V) calibration solutions, which were prepared from the arsenic standard of the Japan Calibration Service system and whose species was guaranteed to be As(V) by NMIJ. The uncertainties of all the measurements and preparation procedures were evaluated. The certified value of As(V) in the CRM is (99.53 +/- 1.67) mg kg(-1) (k = 2).

  19. Palm-Based Standard Reference Materials for Iodine Value and Slip Melting Point

    Directory of Open Access Journals (Sweden)

    Azmil Haizam Ahmad Tarmizi

    2008-01-01

    Full Text Available This work described study protocols on the production of Palm-Based Standard Reference Materials for iodine value and slip melting point. Thirty-three laboratories collaborated in the inter-laboratory proficiency tests for characterization of iodine value, while thirty-two laboratories for characterization of slip melting point. The iodine value and slip melting point of palm oil, palm olein and palm stearin were determined in accordance to MPOB Test Methods p3.2:2004 and p4.2:2004, respectively. The consensus values and their uncertainties were based on the acceptability of statistical agreement of results obtained from collaborating laboratories. The consensus values and uncertainties for iodine values were 52.63 ± 0.14 Wijs in palm oil, 56.77 ± 0.12 Wijs in palm olein and 33.76 ± 0.18 Wijs in palm stearin. For the slip melting points, the consensus values and uncertainties were 35.6 ± 0.3 ° C in palm oil, 22.7 ± 0.4 ° C in palm olein and 53.4 ± 0.2 ° C in palm stearin. Repeatability and reproducibility relative standard deviations were found to be good and acceptable, with values much lower than that of 10%. Stability of Palm-Based Standard Reference Materials remained stable at temperatures of -20 ° C, 0 ° C, 6 ° C and 24 ° C upon storage for one year.

  20. Periodic reference tracking control approach for smart material actuators with complex hysteretic characteristics

    Science.gov (United States)

    Sun, Zhiyong; Hao, Lina; Song, Bo; Yang, Ruiguo; Cao, Ruimin; Cheng, Yu

    2016-10-01

    Micro/nano positioning technologies have been attractive for decades for their various applications in both industrial and scientific fields. The actuators employed in these technologies are typically smart material actuators, which possess inherent hysteresis that may cause systems behave unexpectedly. Periodic reference tracking capability is fundamental for apparatuses such as scanning probe microscope, which employs smart material actuators to generate periodic scanning motion. However, traditional controller such as PID method cannot guarantee accurate fast periodic scanning motion. To tackle this problem and to conduct practical implementation in digital devices, this paper proposes a novel control method named discrete extended unparallel Prandtl-Ishlinskii model based internal model (d-EUPI-IM) control approach. To tackle modeling uncertainties, the robust d-EUPI-IM control approach is investigated, and the associated sufficient stabilizing conditions are derived. The advantages of the proposed controller are: it is designed and represented in discrete form, thus practical for digital devices implementation; the extended unparallel Prandtl-Ishlinskii model can precisely represent forward/inverse complex hysteretic characteristics, thus can reduce modeling uncertainties and benefits controllers design; in addition, the internal model principle based control module can be utilized as a natural oscillator for tackling periodic references tracking problem. The proposed controller was verified through comparative experiments on a piezoelectric actuator platform, and convincing results have been achieved.

  1. Application of reference materials for quality assessment in neutron activation analysis

    International Nuclear Information System (INIS)

    Obrusnik, I.; Eckschlager, K.

    1993-01-01

    It is generally accepted that an analytical procedure can be regarded as an information production system yielding information on the composition of the analyzed sample. Thus, information theory can be useful and the quantities characterizing the information properties of an analytical method may be applied not only as evaluation criteria but also as objective functions in the optimization. The usability of information theory is demonstrated on the example of neutron activation analysis. Both precision and bias of NAA results are taken into account together with the possible use of reference materials for quality assessment. The influence of the above-mentioned parameters on information properties such as information gain and profitability of NAA results is discussed in detail. It has been proved that information theory is especially useful in choosing suitable reference materials for the quality assessment of routine analytical procedures not only with respect to matrix and analyte concentration in the sample but also to concentrations and uncertainties of certified values in the CRM used. In the extreme trace analysis, CRMs with relatively large uncertainties and very low certified concentrations can still yield rather high information gain of results. (author) 14 refs.; 9 figs

  2. Certified Reference Materials for Radioactivity Measurements in Environmental Samples of Soil and Water: IAEA-444 and IAEA-445

    International Nuclear Information System (INIS)

    2011-01-01

    Reference Materials are an important 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 1960's 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. Within the frame of IAEA activities in production and certification of reference materials, this report describes the certification of the IAEA-444 and IAEA-445: soil and water spiked with gamma emitting radionuclides respectively. Details are given on methodologies and data evaluation

  3. 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

  4. Nanoscale reference materials for environmental, health and safety measurements: needs, gaps and opportunities.

    Science.gov (United States)

    Stefaniak, Aleksandr B; Hackley, Vincent A; Roebben, Gert; Ehara, Kensei; Hankin, Steve; Postek, Michael T; Lynch, Iseult; Fu, Wei-En; Linsinger, Thomas P J; Thünemann, Andreas F

    2013-12-01

    The authors critically reviewed published lists of nano-objects and their physico-chemical properties deemed important for risk assessment and discussed metrological challenges associated with the development of nanoscale reference materials (RMs). Five lists were identified that contained 25 (classes of) nano-objects; only four (gold, silicon dioxide, silver, titanium dioxide) appeared on all lists. Twenty-three properties were identified for characterisation; only (specific) surface area appeared on all lists. The key themes that emerged from this review were: 1) various groups have prioritised nano-objects for development as "candidate RMs" with limited consensus; 2) a lack of harmonised terminology hinders accurate description of many nano-object properties; 3) many properties identified for characterisation are ill-defined or qualitative and hence are not metrologically traceable; 4) standardised protocols are critically needed for characterisation of nano-objects as delivered in relevant media and as administered to toxicological models; 5) the measurement processes being used to characterise a nano-object must be understood because instruments may measure a given sample in a different way; 6) appropriate RMs should be used for both accurate instrument calibration and for more general testing purposes (e.g., protocol validation); 7) there is a need to clarify that where RMs are not available, if "(representative) test materials" that lack reference or certified values may be useful for toxicology testing and 8) there is a need for consensus building within the nanotechnology and environmental, health and safety communities to prioritise RM needs and better define the required properties and (physical or chemical) forms of the candidate materials.

  5. High frequency dielectric reference materials BCR projekt 43. Final report of phase 1

    International Nuclear Information System (INIS)

    Chantry, G.

    1980-01-01

    The Group of High Frequency Specialists from Belgium, France, Germany, The Netherlands and the UK, was awarded contracts in 1975 to carry out a programme of measurements on the high frequency dielectric properties of materials. The object of this first phase of a projected three phase programme was to establish the reliability of existing methods of measurement and to examine the possibilities of specifying and producing some standard reference materials, both liquid and solid, which could be used for calibrating and checking the performance of industrial measurement equipment. The liquids chosen for the first phase were cyclohexane, cis and trans decalin, chlorobenzene and 0.1, 1, and 10% solutions of chlorobenzene in cyclohexane. Each group had a limited frequency range over which it could make meaningful measurements but there was sufficient overlap to ensure that all random and systematic errors could be quantitatively assayed. The real (epsilon') and imaginary (epsilon'') components of the complex permittivity for all the liquids were measured over the frequency range 10 - 3,000 GHz and for the two most lossy liquids (chlorobenzene and 10% chlorobenzene in cyclohexane) this range was extended downwards to one GHz. The programme established for the first time the possible experimental imprecisions to be expected in high frequency dielecric measurements and showed that the chosen liquids could be useful standard reference materials if sufficiently pure specimens could be obtained commercially at a reasonable price. The programme did however reveal an unexpected snag in that the liquids, especially cyclohexane, were found to be rather more liable to contamination than expected. Since cyclohexane is a very low-loss liquid, only a small amount of a lossy contaminant need be absorbed to make the observed loss increase dramatically. This report contains all the measured results in both tabular and graphical form and in addition full technical details are given of the

  6. 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.

  7. 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.

  8. The determination, by instrumental neutron-activation analysis, of some elements in the NIMROC standard reference materials

    International Nuclear Information System (INIS)

    Eddy, B.T.; Pearton, D.C.G.; Bibby, D.M.

    1975-01-01

    Instrumental neutron-activation analysis was used for the determination of sixteen trace and minor elements in the six NIMROC reference materials. Six reference rock materials prepared by the U.S. Geological Survey were also analysed, and the results were compared with the recommended, average, or magnitude values given for these rocks by Flanagan. The agreement between the two sets of results was found to be generally good, indicating that INAA is an acceptable technique for the determination of most of these elements. The values found for the NIMROC samples represent a significant contribution to the evaluation of the trace elements in these reference materials [af

  9. Evaluation of the neutron cross sections for Pu-240

    International Nuclear Information System (INIS)

    Weston, L.W.; Arthur, E.D.

    1987-04-01

    The present evaluation is proposed to supersede the ENDF/B-V, Revision 2 file for 240 Pu. In this work, resonance parameters, cross sections, energy distributions, and angular distributions have been modified. These changes are outlined in detail and appropriate references included. 37 refs., 21 figs., 2 tabs

  10. The use of high accuracy NAA for the certification of NIST Standard Reference Materials

    International Nuclear Information System (INIS)

    Becker, D.A.; Greenberg, R.R.; Stone, S.

    1991-01-01

    Neutron activation analysis (NAA) is only one of many analytical techniques used at the National Institute of Standards and Technology (NIST) for the certification of NIST Standard Reference Materials (SRMs). We compete daily against all of the other available analytical techniques in terms of accuracy, precision, and the cost required to obtain that requisite accuracy and precision. Over the years, the authors have found that NAA can and does compete favorably with these other techniques because of its' unique capabilities for redundancy and quality assurance. Good examples are the two new NIST leaf SRMs, Apple Leaves (SRM 1515) and Peach Leaves (SRM 1547). INAA was used to measure the homogeneity of 12 elements in 15 samples of each material at the 100 mg sample size. In addition, instrumental and radiochemical NAA combined for 27 elemental determinations, out of a total of 54 elemental determinations made on each material with all NIST techniques combined. This paper describes the NIST NAA procedures used in these analyses, the quality assurance techniques employed, and the analytical results for the 24 elements determined by NAA in these new botanical SRMs. The NAA results are also compared to the final certified values for these SRMs

  11. Development of reference material for proficiency tests: arsenic in fish tissue

    International Nuclear Information System (INIS)

    Santana, Luciana Vieira de; Sarkis, Jorge E.S.; Ulrich, Joao C.; Hortellani, Marcos Antonio

    2013-01-01

    Proficiency tests (PT) are extensively used to evaluate the analytical competence of laboratories, and are also used as a part of accreditation processes. For this reason are important tool for quality control of laboratories including laboratories that act directly with food exporting companies. In Brazil there are no providers of proficiency testing for toxic metals, such as arsenic in fish tissue. This study presents a protocol to produce reference material to be used in proficiency test for arsenic in fish tissue following the recommendations of the ISO Guide 35. The preparation scheme consisted of: selecting of individuals, cleaning of scale and skin, trituration, homogenization, and spiking with arsenic at two levels of concentration. The mixture was then irradiated in a cyclotron Cyclone 30 Applications ion beam with cobalt 60 at 10.00 ± 1.05 KGy, before being packed into sachets. To verify the efficacy of the irradiation procedure, 26 (randomly selected) irradiated sachets and 26 non-irradiated sachets were assessed for homogeneity and stability. The results indicate that irradiation with cobalt 60 is crucial for ensuring the preservation of the integrity of the material, providing stable material at room temperature for 2 months. The samples can therefore be transported at room temperature. (author)

  12. Development of reference material for proficiency tests: arsenic in fish tissue

    Energy Technology Data Exchange (ETDEWEB)

    Santana, Luciana Vieira de; Sarkis, Jorge E.S.; Ulrich, Joao C.; Hortellani, Marcos Antonio, E-mail: santana-luciana@ig.com.br, E-mail: jesarkis@ipen.br, E-mail: jculrich@ipen.br, E-mail: mahortel@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    Proficiency tests (PT) are extensively used to evaluate the analytical competence of laboratories, and are also used as a part of accreditation processes. For this reason are important tool for quality control of laboratories including laboratories that act directly with food exporting companies. In Brazil there are no providers of proficiency testing for toxic metals, such as arsenic in fish tissue. This study presents a protocol to produce reference material to be used in proficiency test for arsenic in fish tissue following the recommendations of the ISO Guide 35. The preparation scheme consisted of: selecting of individuals, cleaning of scale and skin, trituration, homogenization, and spiking with arsenic at two levels of concentration. The mixture was then irradiated in a cyclotron Cyclone 30 Applications ion beam with cobalt 60 at 10.00 ± 1.05 KGy, before being packed into sachets. To verify the efficacy of the irradiation procedure, 26 (randomly selected) irradiated sachets and 26 non-irradiated sachets were assessed for homogeneity and stability. The results indicate that irradiation with cobalt 60 is crucial for ensuring the preservation of the integrity of the material, providing stable material at room temperature for 2 months. The samples can therefore be transported at room temperature. (author)

  13. Contribution to the study of U-Ti and U-Pu-Ti carbides

    International Nuclear Information System (INIS)

    Milet, C.A.

    1968-01-01

    After having discussed the reasons to use (U,Pu) carbides as fast reactor fuel, we examine the influence of the addition of titanium to these carbides. A preliminary study has been done on the system of U-C-Ti and some properties have been measured such as: density, thermal expansion, electrical resistivity, atmospheric corrosion and compatibility with stainless steel. The systems U-Pu-C-Ti (Pu/U + Pu equal to 15 per cent) and U-C-Ti have been found to be very similar. There exists a two phases region (U,Pu)C + TiC, an eutectic between (U,Pu)C and TiC for approximately 15 at %. The solubilities of U + Pu in TiC and of Ti in (U,Pu)C is less than 1 % at. The addition of titanium does not markedly change thermal expansion coefficients of (U,Pu)C. However the resistance to atmospheric corrosion and compatibility with stainless steel is improved. Thermal conductivity, calculated from electrical resistivity, has increased. On the other side, the density of fissile material is lowered. The combination of (U,Pu)C + TiC seems to be the most promising alloy for application as nuclear fuel. (author) [fr

  14. PU-ICE Summary Information.

    Energy Technology Data Exchange (ETDEWEB)

    Moore, Michael [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-05-01

    The Generator Knowledge Report for the Plutonium Isentropic Compression Experiment Containment Systems (GK Report) provides information for the Plutonium Isentropic Compression Experiment (Pu- ICE) program to support waste management and characterization efforts. Attachment 3-18 presents generator knowledge (GK) information specific to the eighteenth Pu-ICE conducted in August 2015, also known as ‘Shot 18 (Aug 2015) and Pu-ICE Z-2841 (1).’ Shot 18 (Aug 2015) was generated on August 28, 2015 (1). Calculations based on the isotopic content of Shot 18 (Aug 2015) and the measured mass of the containment system demonstrate the post-shot containment system is low-level waste (LLW). Therefore, this containment system will be managed at Sandia National Laboratory/New Mexico (SNL/NM) as LLW. Attachment 3-18 provides documentation of the TRU concentration and documents the concentration of any hazardous constituents.

  15. 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)

  16. 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

  17. 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

  18. Certified reference, intercomparison, performance evaluation and emergency preparedness exercise materials for radionuclides in food

    International Nuclear Information System (INIS)

    Jerome, S.M.; Inn, K.G.W.; Uwe Waetjen; Zhichao Lin

    2015-01-01

    The threat to global security from terrorist attack does not solely arise from illicit use of firearms, explosives or weapons of mass destruction. Terrorist threats will inevitably become more subtle as information and expertise is acquired by terrorist groups, and one vulnerable area is food and the food supply chain. Many laboratories, especially in countries with nuclear programmes, are involved in the routine monitoring of foodstuffs, and will be required to respond with increased food monitoring necessary for ensuring food safety and protecting public health after real (or perceived) contamination of food by either accidental or illicit means. This paper examines the needs for reference and performance testing materials that were identified at an international workshop to discuss this matter held at NIST in 2008, and further refined at a follow-up workshop in 2009. (author)

  19. Instrumental neutron activation analysis of rib bone samples and of bone reference materials

    International Nuclear Information System (INIS)

    Saiki, M.; Takata, M.K.; Kramarski, S.; Borelli, A.

    2000-01-01

    The instrumental neutron activation analysis method was used for the determination of trace elements in rib bone samples taken from autopsies of accident victims. The elements Br, Ca, Cl, Cr, Fe, Mg, Mn, Na, P, Sr, Rb and Zn were determined in cortical tissues by using short and long irradiations with thermal neutron flux of the IEA-R1m nuclear reactor. The reference materials NIST SRM 1400 Bone Ash and NIST SRM 1486 Bone Meal were also analyzed in order to evaluate the precision and the accuracy of the results. It was verified that lyophilization is the most convenient process for drying bone samples since it does not cause any element losses. Comparisons were made between the results obtained for rib samples and the literature values as well as between the results obtained for different ribs from a single individual and for bones from different individuals. (author)

  20. k0IAEA software validation at CDTN/CNEN, Brazil, using certified reference materials

    International Nuclear Information System (INIS)

    Menezes, M.A.B.C.; Jacimovic, R.

    2007-01-01

    The IAEA distributed the k 0I AEA software package program to several laboratories. The Laboratory for Neutron Activation Analysis, at CDTN/CNEN (Centro de Desenvolvimento da Tecnologia Nuclear/Comissao Nacional de Energia Nuclear), Belo Horizonte, Brazil, acquired the k 0I AEA software package during the Workshop on Nuclear Data for Activation Analysis, 2005, held at the Abdus Salam International Centre for Theoretical Physics, Trieste, Italy. This paper is about the validation procedure carried out at the local laboratory aiming at the validation of the k 0I AEA software package. After the software was set up according to the guidelines, the procedure followed at CDTN/CNEN to validate the k 0I AEA software was to analyse several reference materials. The overall results pointed out that the k 0I AEA software is working properly. (author)

  1. Determination of rare earth elements in the biological reference materials Pine Needles and Spruce Needles by neutron activation analysis

    International Nuclear Information System (INIS)

    Machado, C.N.; Maria, S.P.; Saiki, M.; Figueiredo, A.M.G.

    1998-01-01

    Instrumental neutron activation analysis was applied to determine La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and Sc in two biological reference materials: NIST 1575 Pine Needles and BCR-CRM 101 Spruce Needles. The purpose was to contribute to the reference data for these two reference materials. The results were obtained with a good precision (relative standard deviations less than 15%). For the Pine Needles reference material there are already some proposed values and our results showed, in general, a good agreement with the data published. The contribution of uranium fission products to La, Ce, Nd and Sm was evaluated and considered in the determination of these elements. Interferences in the determination of rare earth elements in biological materials are also discussed. (author)

  2. Advancements in Particle Analysis Procedures and their Application to the Characterization of Reference Materials for Safeguards

    International Nuclear Information System (INIS)

    Admon, U.; Chinea-Cano, E.; Dzigal, N.; Vogt, K.S.; Halevy, I.; Boblil, E.; Elkayam, T.; Weiss, A.

    2015-01-01

    Two approaches may be employed in the preparation of Reference Materials (RMs) for use in micro analytical techniques: placement of characterized micro artefacts in bulk materials and characterization of certain classes of individual particles in existing materials. In November 2013, a collaborative project was launched with the aim of adding information about such individual particles in existing RMs. The motivation behind this project was to investigate and characterize micro-artefacts present in certain commercially available RM, making them available and fit for use in safeguards and several other nuclear applications. The implementation and development of new techniques for particle characterization in bulk materials are also part of this project. The strategy for that approach includes the following steps: 1. Sample preparation: Dispersion of particles on stubs and planchets by an in-house shock-wave device. 2. Particle-of-Interest identification and characterization: (a) Fission Track (FT) route: Mosaic imaging of detectors containing FT stars; Applying automatic pattern recognition and localization of FT stars in detectors; Using Laser Micro-Dissection (LMD) for retrieval of individual particles; Preparation of sampled particles for SEM observation and other analytical techniques. (b) Alpha Track (αT) route: Direct particle identification and localization using position sensitive detectors (instrumental auto-radiography). (c) The advanced SEM route: Integration of analytical SEM techniques for characterization of individual particles of interest: EDS, mass spectrometry, FIB, micro-Raman. Preliminary results of the ongoing efforts will be reported. Utilization of these hyphenated techniques and instruments represents an innovative approach to particle characterization for Safeguards applications. (author)

  3. Feasibility study on production of a matrix reference material for cyanobacterial toxins.

    Science.gov (United States)

    Hollingdale, Christie; Thomas, Krista; Lewis, Nancy; Békri, Khalida; McCarron, Pearse; Quilliam, Michael A

    2015-07-01

    The worldwide increase in cyanobacterial contamination of freshwater lakes and rivers is of great concern as many cyanobacteria produce potent hepatotoxins and neurotoxins (cyanotoxins). Such toxins pose a threat to aquatic ecosystems, livestock, and drinking water supplies. In addition, dietary supplements prepared from cyanobacteria can pose a risk to consumers if they contain toxins. Analytical monitoring for toxins in the environment and in consumer products is essential for the protection of public health. Reference materials (RMs) are an essential tool for the development and validation of analytical methods and are necessary for ongoing quality control of monitoring operations. Since the availability of appropriate RMs for cyanotoxins has been very limited, the present study was undertaken to examine the feasibility of producing a cyanobacterial matrix RM containing various cyanotoxins. The first step was large-scale culturing of various cyanobacterial cultures that produce anatoxins, microcystins, and cylindrospermopsins. After harvesting, the biomass was lyophilized, blended, homogenized, milled, and bottled. The moisture content and physical characteristics were assessed in order to evaluate the effectiveness of the production process. Toxin levels were measured by liquid chromatography with tandem mass spectrometry and ultraviolet detection. The reference material was found to be homogeneous for toxin content. Stability studies showed no significant degradation of target toxins over a period of 310 days at temperatures up to +40 °C except for the anatoxin-a, which showed some degradation at +40 °C. These results show that a fit-for-purpose matrix RM for cyanotoxins can be prepared using the processes and techniques applied in this work.

  4. Remarks on some reference materials for applications in elastic peak electron spectroscopy

    International Nuclear Information System (INIS)

    Jablonski, A.; Zemek, J.

    2010-01-01

    The quantification of results of electron spectroscopies, AES and XPS, requires knowledge of the inelastic mean free path (IMFP) of signal electrons in solids. This parameter determines the surface sensitivity of both techniques. There are two methods of determining the IMFPs that provide these parameters in agreement with the definition: (1) calculations based on the experimental optical data, and (2) calculations based on measurements of the electron elastic backscattering intensity. The latter method requires the use of some reference material for which the IMFP is known. In 1999, an extensive analysis of the published IMFPs has been performed; the results indicated that there is a very good agreement between the calculated and measured IMFPs for four elemental solids: Ni, Cu, Ag and Au. The averaged IMFPs for these elements are known under the name of the recommended IMFPs. However, no preference among these four elements has been established. In the present work, an attempt is made to select an element for which the recommended IMFPs result in the best agreement between the calculated and measured intensities of elastic electron backscattering. For this purpose, the elastic backscattering intensity has been measured at eight electron energies varying from 200 to 1500 eV. At each energy, the intensity was measured over a wide range of emission angles from 35deg to 74deg. The experiments were accompanied with Monte Carlo calculations of the elastic backscattering probability for the same energies and experimental configurations. It has been found, from comparison, that the best agreement is observed for Au, and this element is thus recommended as the reference material. It has been shown that the shape of the emission angle dependence of the elastic backscattering intensity is noticeably influenced by the surface energy losses. (author)

  5. Palm-Based Standard Reference Materials for Iodine Value and Slip Melting Point

    Directory of Open Access Journals (Sweden)

    Azmil Haizam Ahmad Tarmizi

    2008-01-01

    Full Text Available This work described study protocols on the production of Palm-Based Standard Reference Materials for iodine value and slip melting point. Thirty-three laboratories collaborated in the inter-laboratory proficiency tests for characterization of iodine value, while thirty-two laboratories for characterization of slip melting point. The iodine value and slip melting point of palm oil, palm olein and palm stearin were determined in accordance to MPOB Test Methods p3.2:2004 and p4.2:2004, respectively. The consensus values and their uncertainties were based on the acceptability of statistical agreement of results obtained from collaborating laboratories. The consensus values and uncertainties for iodine values were 52.63 ± 0.14 Wijs in palm oil, 56.77 ± 0.12 Wijs in palm olein and 33.76 ± 0.18 Wijs in palm stearin. For the slip melting points, the consensus values and uncertainties were 35.6 ± 0.3 °C in palm oil, 22.7 ± 0.4 °C in palm olein and 53.4 ± 0.2 °C in palm stearin. Repeatability and reproducibility relative standard deviations were found to be good and acceptable, with values much lower than that of 10%. Stability of Palm-Based Standard Reference Materials remained stable at temperatures of –20 °C, 0 °C, 6 °C and 24 °C upon storage for one year.

  6. New radiochemical methods for determination of 237Np a 241Pu using extraction chromatography (Presentation)

    International Nuclear Information System (INIS)

    Strisovska, J.

    2013-01-01

    Thesis was focused on the development of a new methodology for the separation of anthropogenic transuranium radionuclides 237 Np a 241 Pu from different kinds of matrices. The analytical methods used in this study were based on extraction chromatography and were optimized according to the sample type. The proposed radiochemical procedure is a combination of two algorithms, which represent the separation of radionuclides by using extraction chromatographic sorbents TEVA resin and TRU resin supplied by Eichrom Technologies LLC. 239 Np a 237 Np were selectively captured on sorbent TEVA resin in oxidation state 4+. TRU resin was used for purification of plutonium fraction from interfering americium radionuclide. 242 Pu and 239 Np radionuclides as tracers have been used to monitor the radiochemical yields of separation. Before every radiochemical separation tracer radionuclide 239 Np was obtained by separation from the parent radionuclide 2 43 Am, which is in radioactive equilibrium to 239 Np. The average yield of chemical separation was 69,3% for 239 Np at 277 keV energy line and 65,9% at 228 keV energy line. The NPL AH-B08069 (2008) samples which consist of the mixture of alpha-radionuclides were used for the modification and optimization of separation method used for separation of Np and Pu in model samples. This method provided high radiochemical yields of 239,240 Pu (95,0 ± 3,5)% and 237 Np (87,9 ± 3,0)%.. Reliability of the method was verified by applying our modified separation procedures on reference materials IAEA-375 and IAEA-414 supplied by International Atomic Energy Agency. A good agreement between the results is obtained by this procedure and the certified values were found. Samples of contaminated soils from the area of Nuclear power plant A-1 Jaslovske Bohunice which is stored temporarily before disposal were analyzed using developed separation procedure. Specific activity of investigated radionuclides was determined in these samples. (author)

  7. Recent advances in ratio primary reference measurement procedures (definitive methods) and their use in certification of reference materials and controlling assigned values in proficiency testing

    International Nuclear Information System (INIS)

    Dybczynski, R.S.; Polkowska-Motrenko, H.; Chajduk, E.; Danko, B.; Pyszynska, M.

    2014-01-01

    Three very accurate (definitive) methods by RNAA for the determination of Se, As and Fe respectively, which were recently elaborated in our laboratory, are reviewed and their use in certification of reference materials and in checking the assigned values in proficiency tests is demonstrated on several examples. According to VIM 3 nomenclature these methods may be called: ratio primary reference measurement procedures (RPRMPs). RPRMPs with their expanded uncertainties of 2.7-3.6 % are comparable to ID-MS methods and are the only methods of such high metrological quality which can be used for the determination of trace amounts of monoisotopic elements. (author)

  8. Certification for copper concentration in reference material for fuel anhydro ethylic alcohol; Certificacao da concentracao de cobre em material de referencia para alcool etilico anidro combustivel (AEC)

    Energy Technology Data Exchange (ETDEWEB)

    Reis, Lindomar Augusto dos; Rocha, Marcia Silva da; Mesko, Marcia Foster; Silva, Fagner Francisco da; Quaresma, Maria Cristina Baptista; Araujo, Thiago Oliveira [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (DIMCI/INMETRO), Duque de Caxias, RJ (Brazil). Diretoria de Metrologia Cientifica e Industrial], E-mail: lareis@inmetro.gov.br

    2009-07-01

    This work aiming to obtain the first certified reference material for fuel anhydro ethylic alcohol relative to the copper concentration, which has his maximum limit determined by the in force legislation providing traceability and reliability for the measurement results.

  9. Certification of B-group vitamins (b1, b2, b6, and b12) in four food reference materials

    NARCIS (Netherlands)

    Ollilainen, V.; Finglas, P.M.; Berg, H. van den; Froidmont-Görtz, I. de

    2001-01-01

    In 1989, the Community Bureau of Reference started a research program to improve the quality of vitamin analysis in food. To achieve this task, vitamin methodology was evaluated and tested by interlaboratory studies and the preparation of certified reference materials, which will be used for quality

  10. Effect of reference parameters and properties of materials for WWER-type fuel elements on their reliability

    Energy Technology Data Exchange (ETDEWEB)

    Bibilashvili, Yu K; Malachenko, L L; Medvedev, A V; Solyany, V I; Sukhanov, G I; Tonkov, V Yu

    1987-05-01

    Present approach to requirements for reference parameters and properties of materials for WWER-1000 fuel elements is presented as well as evaluation of their effects on fuel reliability. Some results of investigations with the aim of improving fuel element reliability in operational NPP conditions are discussed. 4 references, 7 figures, 3 tables.

  11. Estimation of uncertainty of a reference material for proficiency testing for the determination of total mercury in fish in nature

    International Nuclear Information System (INIS)

    Santana, L V; Sarkis, J E S; Ulrich, J C; Hortellani, M A

    2015-01-01

    We provide an uncertainty estimates for homogeneity and stability studies of reference material used in proficiency test for determination of total mercury in fish fresh muscle tissue. Stability was estimated by linear regression and homogeneity by ANOVA. The results indicate that the reference material is both homogeneous and chemically stable over the short term. Total mercury concentration of the muscle tissue, with expanded uncertainty, was 0.294 ± 0.089 μg g −1

  12. 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)

  13. Physics of the fuel cycle. Evaluation of methods, uncertainties and estimation of the material balance for fuels UO{sub 2} and UO{sub 2}-PuO{sub 2}; Physique du cycle du combustible evaluation des methodes, incertitudes et estimation du bilan matiere pour les combustibles UO{sub 2} et UO{sub 2}-PuO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Monier, C

    1997-09-01

    The research works of this thesis are aimed to evaluate the methods and the associated uncertainties for the material balances estimation of the burn-up UO{sub 2} and MOX fuels which intervene in the fuel cycle physics. The studies carried out are used to qualify the cycle `package` DARWIN for the PWRs material balances estimation. The elaboration and optimisation of the calculation routes are carried out following a very specific methodology, aimed at estimating the bias introduced by the modelizations simplification by a comparison with almost exact reference modelizations. Depending on the precision goals and the informations, the permissible approximation will be determined. Two calculation routes have been developed and the qualified by applying them to the used fuels isotopic analysis interpretation: one `industry-oriented` calculation route which can calculate full UO{sub 2} assemblies material balances with a 2 % precision on the main actinides, respecting the industrial specifications. This route must run with a reasonable calculation time and stay user-friendly; one reference calculation route for the precise interpretation of fuel samples made of pieces of burn-up MOX rods. Aiming to provide material balances with the best possible precision, this route does not have the same specifications concerning its use and its calculation time performance. (author)

  14. 11-year field study of Pu migration from Pu III, IV, and VI sources

    International Nuclear Information System (INIS)

    Kaplan, D.I.; Serkiz, S.M.; Demirkanli, D.I.; Gumapas, L.; Fjeld, R.A.; Molz, F.J.; Powell, B.A.

    2005-01-01

    Full text of publication follows: Understanding the processes controlling Pu mobility in the subsurface environment is important for estimating the amount of Pu waste that can be safely disposed in vadose zone burial sites. To study long-term Pu mobility, four 52-L lysimeters filled with sediment collected from the Savannah River Site near Aiken South Carolina were amended with well characterized solid Pu sources (Pu III Cl 3 , Pu IV (NO 3 ) 4 , Pu IV (C 2 O 4 ) 2 , and Pu VI O 2 (NO 3 ) 2 ) and left exposed to natural precipitation for 2 to 11 years. Pu oxidation state distribution in the Pu(III) and Pu(IV) lysimeters sediments (a red clayey sediment, pH = 6.3) were similar, consisting of 0% Pu(III), >92% Pu(IV), 1% Pu(V), 1% Pu(VI), and the remainder was a Pu polymer. These three lysimeters also had near identical sediment Pu concentration profiles, where >95% of the Pu remained within 1.25 cm of the source after 11 years; moving at an overall rate of 0.9 cm yr -1 . As expected, Pu moved more rapidly through the Pu(VI) lysimeter, at an overall rate of 12.5 cm yr -1 . Solute transport modeling of the sediment Pu concentration profile data in the Pu(VI) lysimeter indicated that some transformation of Pu into a much less mobile form, presumably Pu(IV), had occurred during the course of the two year study. This modeling also supported previous laboratory measurements showing that Pu(V) or Pu(VI) reduction was five orders of magnitude faster than corresponding Pu(III) or Pu(IV) oxidation. The slow oxidation rate (1 x 10-8 hr -1 ; t 1/2 = 8,000 yr) was not discernable from the Pu(VI) lysimeter data that reflected only two years of transport but was readily discernable from the Pu(III) and Pu(IV) lysimeter data that reflected 11 yr of transport. (authors)

  15. Polish reference material: corn flour (INCT-CF-3)for inorganic trace analysis - preparation and certification

    International Nuclear Information System (INIS)

    Polkowska-Motrenko, H.; Dybczynski, R.; Chajduk, E.; Danko, B.; Kulisa, K.; Samczynski, Z.; Sypula, M.; Szopa, Z.

    2006-01-01

    Preparation, examination and certification of the new matrix reference material of biological origin: Corn Flour (INCT-CF-3) is described. The material was prepared from corn grown in Poland according to Polish standard PN-A-74205:1997. The material was sieved through the 250 mm nylon sieves and stored in a polyethylene (PE) bag. Approximately 50 kg of sieved corn flour was collected. Examination by optical microscopy revealed that Martin's diameter of over 98% of particles was below 25 mm. The whole lot of corn flour was then homogenized by mixing for 20 hours in a 110 dm 3 PE drum rotated in three directions. Preliminary homogeneity testing by X-ray fluorescence (XRF) method and final checking of homogeneity by neutron activation analysis (NAA) after distribution of the material into containers revealed, that it is sufficiently homogeneous at least for a sample size ≥ 100 mg. In order to assure the long-term stability, all containers with INCT-CF-3 were sterilized by electron beam radiation. Long-term stability was checked by analyzing concentrations of selected elements in the material stored in the air-conditioned room at 20 o C. Short-term stability was examined by the determination of concentrations of the selected elements in the bottle stored in the CO 2 incubator at 37 o C. The material was certified on the basis of a worldwide interlaboratory comparison, in which 92 laboratories from 19 countries participated providing 962 laboratory averages (4228 individual determinations) for 57 elements. A method of data evaluation leading to assignment of certified values was the same as that used previously in the Laboratory of the Department of Analytical Chemistry, Institute of Nuclear Chemistry and Technology. The result for Mo was obtained by definitive methods developed in the Laboratory and used to support the certification process. Analytical uncertainties and stability uncertainties were quantified to arrive at combined uncertainties of the certified

  16. Quantitative micro x-ray fluorescence analyses without reference standard material; Referenzprobenfreie quantitative Mikro-Roentgenfluoreszenzanalyse

    Energy Technology Data Exchange (ETDEWEB)

    Wolff, Timo

    2009-07-15

    X-ray fluorescence analysis (XRF) is a standard method for non-destructive investigations. Due to the development of polycapillary optics and SDDdetectors requiring no cooling with liquid nitrogen, XRF becomes a suitable method for a large number of applications, e. g. for the analysis of objects in arts and archaeology. Spectrometers developed for those purposes allow investigations outside of laboratories und provide excitation areas with diameters of 10-70 {mu}m. In most applications, quantification of XRF data is realized by the usage of standard reference materials. Due to absorption processes in the samples the accuracy of the results depends strongly on the similarity of the sample and the reference standard. In cases where no suitable references are available, quantification can be done based on the ''fundamental parameter (fp) method''. This quantification procedure is based on a set of equations describing the fluorescence production and detection mathematical. The cross sections for the interaction of x-rays with matter can be taken from different databases. During an iteration process the element concentrations can be determined. Quantitative XRF based on fundamental parameters requires an accurate knowledge of the excitation spectrum. In case of a conventional setup this spectrum is given by the X-ray tube spectrum and can be calculated. The use of polycapillary optics in micro-XRF spectrometers changes the spectral distribution of the excitation radiation. For this reason it is necessary to access the transmission function of the used optic. The aim of this work is to find a procedure to describe this function for routine quantification based on fundamental parameters. Most of the measurements have been carried out using a commercial spectrometer developed for applications in arts and archaeology. On the one hand the parameters of the lens, used in the spectrometer, have been investigated by different experimental characterization

  17. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements

    DEFF Research Database (Denmark)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin

    2014-01-01

    counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5×105 for 20 g soil compared to the level reported in the literature......, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference......Pu. However, it is impossible to measure 238Pu using ICP-MS in environmental samples even a decontamination factor as high as 106 for uranium was obtained by chemical separation....

  18. Milk and serum standard reference materials for monitoring organic contaminants in human samples.

    Science.gov (United States)

    Schantz, Michele M; Eppe, Gauthier; Focant, Jean-François; Hamilton, Coreen; Heckert, N Alan; Heltsley, Rebecca M; Hoover, Dale; Keller, Jennifer M; Leigh, Stefan D; Patterson, Donald G; Pintar, Adam L; Sharpless, Katherine E; Sjödin, Andreas; Turner, Wayman E; Vander Pol, Stacy S; Wise, Stephen A

    2013-02-01

    Four new Standard Reference Materials (SRMs) have been developed to assist in the quality assurance of chemical contaminant measurements required for human biomonitoring studies, SRM 1953 Organic Contaminants in Non-Fortified Human Milk, SRM 1954 Organic Contaminants in Fortified Human Milk, SRM 1957 Organic Contaminants in Non-Fortified Human Serum, and SRM 1958 Organic Contaminants in Fortified Human Serum. These materials were developed as part of a collaboration between the National Institute of Standards and Technology (NIST) and the Centers for Disease Control and Prevention (CDC) with both agencies contributing data used in the certification of mass fraction values for a wide range of organic contaminants including polychlorinated biphenyl (PCB) congeners, chlorinated pesticides, polybrominated diphenyl ether (PBDE) congeners, and polychlorinated dibenzo-p-dioxin (PCDD) and dibenzofuran (PCDF) congeners. The certified mass fractions of the organic contaminants in unfortified samples, SRM 1953 and SRM 1957, ranged from 12 ng/kg to 2200 ng/kg with the exception of 4,4'-DDE in SRM 1953 at 7400 ng/kg with expanded uncertainties generally <14 %. This agreement suggests that there were no significant biases existing among the multiple methods used for analysis.

  19. Meta-Cresol Purple Reference Material® (RM) for Seawater pH Measurements

    Science.gov (United States)

    Easley, R. A.; Waters, J. F.; Place, B. J.; Pratt, K. W.

    2016-02-01

    The pH of seawater is a fundamental quantity that governs the carbon dioxide - carbonate system in the world's oceans. High quality pH measurements for long-term monitoring, shipboard studies, and shorter-term biological studies (mesocosm and field experiments) can be ensured through a reference material (RM) that is compatible with existing procedures and which is traceable to primary pH measurement metrology. High-precision spectrophotometric measurements of seawater pH using an indicator dye such as meta-cresol purple (mCP) are well established. However, traceability of these measurements to the International System of Units (SI) additionally requires characterizing the spectrophotometric pH response of the dye in multiple artificial seawater buffers that themselves are benchmarked via primary pH (Harned cell) measurements at a range of pH, salinity, and temperature. NIST is currently developing such a mCP pH RM using this approach. This material will also incorporate new procedures developed at NIST for assessing the purity and homogeneity of the mCP reagent itself. The resulting mCP will provide long-term (years) stability and ease of shipment compared to artificial seawater pH buffers. These efforts will provide the oceanographic user community with a NIST issued mCP (RM), characterized as to its molar absorptivity values and acid dissociation constants (pKa), with uncertainties that comply with the Guide to the Expression of Uncertainty in Measurement (GUM).

  20. Early retention of 237Pu + 239Pu in mature beagles

    International Nuclear Information System (INIS)

    Lloyd, R.D.; McFarland, S.S.; Atherton, D.R.; Bruenger, F.W.; Taylor, G.N.; Mays, C.W.

    1978-01-01

    Five mature beagles, ranging in age from 57 to 84 months, were injected intravenously with about 0.05-0.1 μCi/kg of 239 Pu(IV) citrate to which tracer amounts of the photon-emitter 237 Pu had been added. Plutonium retention in liver and in non-liver tissue (mainly skeleton) was measured periodically in the living dogs for nearly 4 months after injection by a combination of total-body and partial-body counting. All excreta were collected during the first 21 days and analysed for their Pu content. One dog was sacrificed at 14 days and another at 118 days for distribution studies. About 17% (14-20%) of the injected Pu was excreted in the urine and feces in the first 3 weeks, about the same as that excreted in a corresponding time by beagles injected as young adults (14%), but substantially more than beagles injected as juveniles (11%). In contrasts to juvenile beagles injected at 3 months of age, in which early retention was about 12% in liver and 68% in the skeleton, mature beagles retained about 30% in liver and 50% in the skeleton. Retention in young adult beagles injected at 17 months of age was similar to that of mature dogs. Relative distribution of skeletal plutonium among various bones was similar in the mature animals to that seen previously in young adults, but quite different from that of juveniles. A notable exception was the humerus for which there was no significant difference (P>0.2) in the % of retained skeletal Pu represented by the humerus among the juvenile, young adult and mature dogs. (author)

  1. Direct spectrophotometric analysis of low level Pu (III) in Pu(IV) nitrate solution

    International Nuclear Information System (INIS)

    Mageswaran, P.; Suresh Kumar, K.; Kumar, T.; Gayen, J.K.; Shreekumar, B.; Dey, P.K.

    2010-01-01

    Among the various methods demonstrated for the conversion of plutonium nitrate to its oxide, the oxalate precipitation process either as Pu (III) or Pu (IV) oxalate gained wide acceptance. Since uranous nitrate is the most successful partitioning agent used in the PUREX process for the separation of Pu from the bulk amount of U, the Pu (III) oxalate precipitation of the purified nitrate solution will not give required decontamination from U. Hence Pu IV oxalate precipitation process is a better option to achieve the end user's specified PuO 2 product. Prior to the precipitation process, ensuring of the Pu (IV) oxidation state is essential. Hence monitoring of the level of Pu oxidation state either Pu (III) or Pu (IV) in the feed solution plays a significant role to establish complete conversion of Pu (III). The method in vogue to estimate Pu(lV) content is extractive radiometry using Theonyl Trifluoro Acetone (TTA). As the the method warrants a sample preparation with respect to acidity, a precise measurement of Pu (IV) without affecting the Pu(III) level in the feed sample is difficult. Present study is focused on the exploration of direct spectrophotometry using an optic fiber probe of path length of 40mm to monitor the low level of Pu(III) after removing the bulk Pu(lV) which interfere in the Pu(III) absorption spectrum, using TTA-TBP synergistic mixture without changing the sample acidity

  2. Determination of tin in biological reference materials by atomic absorption spectrophotometry and neutron activation analysis

    International Nuclear Information System (INIS)

    Chiba, M.; Iyengar, V.; Gills, T.

    1991-01-01

    Because of a lack of reliable analytical techniques for the determination of tin in biological materials, there have been no reference materials certified for this element. However, the authors' experience has shown that it is feasible to use both atomic absorption and nuclear activation techniques at least for selected matrices. Therefore, an investigation was undertaken to determine tin in several biological materials such as non-fat milk powder (NBS-SRM-1549), citrus leaves (NBS-SRM-1572), total diet (NIST-SRM-1548), mixed diet (NBS-RM-8431), and USDIET-I by atomic absorption spectrophotometry (AAS) and neutron activation analysis (NAA). AAS-ashed samples were extracted with MIBK and assayed using a Perkin Elmer model 5000 apparatus. NAA was carried out by irradiating the samples at the NIST reactor in the RT-4 facility and counting with the help of a Ge(Li) detector connected to a multichannel analyzer. The concentration of tin measured by both AAS and NAA agree well for USDIET-I, total diet, citrus leaves and non-fat milk powder (the concentration ranges for tin in these matrices were from 0.0025 to 3.8 micro g/g). However, in the case of mixed diet (RM-8431), the mean values found were 47 ± 5.6 (n = 19) by AAS and 55.5 ± 2.5 (n = 6) by INAA. Since RM-8431 is not certified it is difficult to draw conclusions. For apple and peach leaves, a distillation step was required. The results were apple leaves 0.085 ± 0.015 (n = 10) by AAS and < 0.2 (n = 3) by RNAA; for peach leaves 0.077 ± 0.02 (n = 9) by AAS and < 0.1 (n = 3) by RNAA. All concentrations are expressed in micro g/g dry weight

  3. 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)

  4. 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)

  5. Study of phase equilibria in function of temperature in UO2-PuO2-Pu2O3 system for nuclear ceramics with high plutonium contents

    International Nuclear Information System (INIS)

    Truphemus, Thibaut

    2013-01-01

    In the UO 2 -PuO 2 -Pu 2 O 3 section, a monophasic (U 1-y ,Pu y )O 2-x domain is stable for y≤0,20 at 25 C and up to solid-liquid equilibrium. At higher Pu content, phase equilibria are more unclear with a phase separation process. The main objective of this work consisted in upgrading the representation of this system for 0,15≤y≤0,65 and 25≤T(C)≤1500. At 25 C, a miscibility gap composed by two different (U 1-y ,Pu y )O 2-x phases has been observed for y≤0,45, with one very closed to stoichiometric state (Oxygen/Metal=2) and one other very reduced. For the first time, a triphasic domain has been characterized at higher Pu contents, with two (U 1-y ,Pu y )O 2-x phases near y=0,45 and one (U 1-y ,Pu y ) 2 O 3 phase with a low U content inside. Concerning the study in function of temperature, we have demonstrated that phase separation temperature increase when Pu content grows. Several representations have been established. At 200 C, the representation is closed to that at 25 C. At 400 C, the phase separation have been specified at a lower Pu content than that of literature: y=0,35. At 600 C, our results have clarified the section, until then very unclear, with a phase separation appearing at y=0,60.The microstructural analysis has clearly demonstrated the significant impact of the phase separation on the material. Indeed many cracks have been observed in our samples, and quantity of these defects increases when Pu content grows. (author) [fr

  6. Methodology and levels of {sup 137} Cs, {sup 90} Sr and {sup 239} {sup +} {sup 240} Pu in marine sediments from the Brazilian Southern Coast

    Energy Technology Data Exchange (ETDEWEB)

    Figueira, R.C.L. [Universidade Cruzeiro do Sul - CETEC/UNICSUL - Sao Paulo/SP (Brazil); Tessler, M.G.; Mahiques, M.M. de [Instituto Oceanografico da Univesidade de Sao Paulo - IOUSP - Sao Paulo/SP (Brazil); Cunha, I.I.L. [Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP -Sao Paulo/SP (Brazil)]. e-mail: figueira@curiango.ipen.br

    2004-07-01

    Methodologies for analysis of {sup 137} Cs, {sup 90} Sr and {sup 239} {sup +} {sup 240} Pu were developed and applied to sediment samples collected along the Brazilian coast. This paper presents the instrumental steps for {sup 137} Cs analysis and the radiochemical steps necessary to analyse {sup 90} Sr and {sup 239} {sup +} {sup 240} Pu. The analytical quality control for radionuclide analysis was verified by participation in international intercomparison exercise running by IAEA as well as in reference material analysis. Further, methodologies were applied in sediments collected from 1976 to 1986 at the Brazilian southern coastal region. {sup 137}Cs levels ranged from 0.37 to 2.03 Bq kg{sup -1}, for {sup 90} Sr from MDC to 8.2 Bq kg{sup -1} and for {sup 239} {sup +} {sup 240} Pu from MDC to 227 m Bq kg{sup -1}. The minimum detectable concentration values (MDC) for {sup 90} Sr and {sup 239} {sup +} {sup 240} Pu were of 0.3 Bq kg{sup -1} and 4.2 mBq kg{sup -1}, respectively. The artificial radioactivity levels in Brazilian sediments are typical values due to fallout deposition and represent reference values for our country. (Author)

  7. Use of 236Pu and 242Pu as a radiochemical tracer for estimation of Pu in bioassay samples by fission track analysis

    International Nuclear Information System (INIS)

    Sawant, Pramilla D.; Prabhu, Supreetha P.; Kalsi, P.C.

    2008-01-01

    236 Pu and 242 Pu are routinely used as radiochemical yield monitors in India for bioassay monitoring of occupational workers by alpha spectrometry. Fission Track Analysis (FTA) is also being standardized for trace level determination of Pu in bioassay samples. The present study, reports the utility of 236 Pu and 242 Pu as radiochemical tracers in estimation of Pu in bioassay samples by FTA technique. The advantages of using 236 Pu tracer in FTA over 242 Pu as well as the interference caused due to presence of 241 Pu in the bioassay samples of occupational workers handling power reactor grade Pu is discussed. (author)

  8. 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

  9. 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.

  10. Report of the 2nd research co-ordination meeting on reference materials for microanalytical nuclear techniques

    International Nuclear Information System (INIS)

    2002-01-01

    Many microanalytical procedure require specific natural-matrix reference materials containing very low levels of trace elements and having a high degree of homogeneity. This proposed CRP will specifically address the question of quality control materials for these techniques. The participants of the meeting discussed the requirements for certified reference materials to by used in microanalysis with particular emphasis on the homogeneity issues. This publication contains summary of the discussions along with conclusions and recommendations made by the participants. The publication also contains ten individual presentations delivered by the participants. Each of the individual papers has been provided with an abstract and indexed separately

  11. Development of a new certified reference material of diosgenin using mass balance approach and Coulometric titration method.

    Science.gov (United States)

    Gong, Ningbo; Zhang, Baoxi; Hu, Fan; Du, Hui; Du, Guanhua; Gao, Zhaolin; Lu, Yang

    2014-12-01

    Certified reference materials (CRMs) can be used as a valuable tool to validate the trueness of measurement methods and to establish metrological traceability of analytical results. Diosgenin has been selected as a candidate reference material. Characterization of the material relied on two different methods, mass balance method and Coulometric titration method (CT). The certified value of diosgenin CRM is 99.80% with an expanded uncertainty of 0.37% (k=2). The new CRM of diosgenin can be used to validate analytical methods, improve the accuracy of measurement data and control the quality of diosgenin in relevant pharmaceutical formulations. Copyright © 2014 Elsevier Inc. All rights reserved.

  12. An attempt to prepare and characterize a soil reference material for Cr(VI) and Cr(III)

    International Nuclear Information System (INIS)

    Solano, G.; Katz, S.A.; Holzbecher, J.; Chatt, A.

    1994-01-01

    Reference materials for the speciation and quantification of chromium in contaminated soils were prepared by impregnating diatomaceous earth with BaCrO 4 and Cr 2 O 3 . The chromium concentrations of these materials were confirmed to be 200 mg/kg both by atomic absorption spectrometry and by instrumental neutron activation analysis, but monthly assays over two calendar quarters of the reference material impregnated with BaCrO 4 revealed the hexavalent chromium was not stable in this matrix. (author) 6 refs,; 2 tabs

  13. In vivo canine studies of a Sinkhole valve and vascular graft coated with biocompatible PU-PEO-SO3.

    Science.gov (United States)

    Han, D K; Lee, K B; Park, K D; Kim, C S; Jeong, S Y; Kim, Y H; Kim, H M; Min, B G

    1993-01-01

    PU-PEO-SO3 was applied as a coating material over a newly designed Sinkhole bileaflet PU heart valve and a porous PU vascular graft. Performance and biocompatibility were evaluated using an in vivo canine shunt system between the right ventricle and pulmonary artery. The survival periods in three implantations were 14, 24, and 39 days, during which no mechanical failure occurred in any Sinkhole valve or vascular graft. Scanning electron microscopy (SEM) studies demonstrated much less platelet adhesion and thrombus formation on PU-PEO-SO3 grafts than on PU vascular grafts. Cracks in the valve leaflet were occasionally observed on PU surfaces, but not on PU-PEO-SO3. After a 39 day implantation, calcium deposition on vascular grafts was decreased as compared with valve leaflets, and calcification on PU-PEO-SO3 was much lower than on PU. These results suggest that Sinkhole valves and vascular grafts are promising, and PU-PEO-SO3 as a coating material is more blood compatible, biostable, and calcification resistant in vivo than in untreated PU.

  14. Preliminary homogeneity study of in-house reference material using neutron activation analysis and X-ray fluorescence

    International Nuclear Information System (INIS)

    Gras, N.; Munoz, L.; Cassorla, V.; Castillo, P.

    1993-01-01

    Although many biological reference materials for quality control of trace element analysis are commercially available, there is still a need for additional local materials for special matrices. In the Latin American region a preliminary study has been commenced involving analytical strategies for the characterization of in-house reference material. A biological sample, prepared in Brazil, constitutes the first regional attempt to prepare reference material. It was analyzed by neutron activation analysis (NAA) and X-ray fluorescence (XRF) to verify its homogeneity. The determination of the trace elements and certain major elements was carried out by instrumental NAA. Trace elements such as Cd, Mn, Mo and Cu were determined using NAA with radiochemical separations to improve the sensitivity and precision. XRF was applied only to major constituents and some trace elements with concentration of more than 10 μg/g. From a total of 18 elements analyzed, only Fe, Cr and Sc were not homogeneously distributed. (orig.)

  15. 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.

  16. Electrochemical investigations of Pu(IV)/Pu(III) redox reaction using graphene modified glassy carbon electrodes and a comparison to the performance of SWCNTs modified glassy carbon electrodes

    International Nuclear Information System (INIS)

    Gupta, Ruma; Gamare, Jayashree; Sharma, Manoj K.; Kamat, J.V.

    2016-01-01

    Highlights: • First report of aqueous electrochemistry of Plutonium on graphene modified electrode. • Graphene is best electrocatalytic material for Pu(IV)/Pu(III) redox couple among the reported modifiers viz. reduced graphene oxide (rGO) and SWCNT’s. • The electrochemical reversibility of Pu(IV)/Pu(III) redox couple improves significantly on graphene modified electrode compared to previously reported rGO & SWCNTs modified electrodes • Donnan interaction between plutonium species and graphene surface offers a possibility for designing a highly sensitive sensor for plutonium • Graphene modified electrode shows higher sensitivity for the determination of plutonium compared to glassy carbon and single walled carbon nanotube modified electrode - Abstract: The work reported in this paper demonstrates for the first time that graphene modified glassy carbon electrode (Gr/GC) show remarkable electrocatalysis towards Pu(IV)/Pu(III) redox reaction and the results were compared with that of single-walled carbon nanotubes modified GC (SWCNTs/GC) and glassy carbon (GC) electrodes. Graphene catalyzes the exchange of current of the Pu(IV)/Pu(III) couple by reducing both the anodic and cathodic overpotentials. The Gr/GC electrode shows higher peak currents (i p ) and smaller peak potential separation (ΔE p ) values than the SWCNTs/GC and GC electrodes. The heterogeneous electron transfer rate constants (k s ), charge transfer coefficients (α) and the diffusion coefficients (D) involved in the electrocatalytic redox reaction were determined. Our observations show that graphene is best electrocatalytic material among both the SWCNTs and GC to study Pu(IV)/Pu(III) redox reaction.

  17. LEAD SLOWING DOWN SPECTROSCOPY FOR DIRECT Pu MASS MEASUREMENTS

    International Nuclear Information System (INIS)

    Ressler, Jennifer J.; Smith, Leon E.; Anderson, Kevin K.

    2008-01-01

    The direct measurement of Pu in previously irradiated fuel assemblies is a recognized need in the international safeguards community. A suitable technology could support more timely and independent material control and accounting (MC and A) measurements at nuclear fuel storage areas, the head-end of reprocessing facilities, and at the product-end of recycled fuel fabrication. Lead slowing down spectroscopy (LSDS) may be a viable solution for directly measuring not only the mass of 239Pu in fuel assemblies, but also the masses of other fissile isotopes such as 235U and 241Pu. To assess the potential viability of LSDS, an LSDS spectrometer was modeled in MCNP5 and 'virtual assays' of nominal PWR assemblies ranging from 0 to 60 GWd/MTU burnup were completed. Signal extraction methods, including the incorporation of nonlinear fitting to account for self-shielding effects in strong resonance regions, are described. Quantitative estimates of Pu uncertainty are given for simplistic and more realistic fuel isotopic inventories calculated using ORIGEN. A discussion of additional signal-perturbing effects that will be addressed in future work, and potential signal extraction approaches that could improve Pu mass uncertainties, are also discussed

  18. Analysis of cement solidified product and ash samples and preparation of a reference material

    International Nuclear Information System (INIS)

    Ishimori, Ken-ichiro; Haraga, Tomoko; Shimada, Asako; Kameo, Yutaka; Takahashi, Kuniaki

    2010-08-01

    Simple and rapid analytical methods for radionuclides in low-level radioactive waste have been developed by the present authors. The methods were applied to simulated solidified products and actual metal wastes to confirm their usefulness. The results were summarized as analytical guide lines. In the present work, cement solidified product and ash waste were analyzed followed by the analytical guide lines and subjects were picked up and solved for the application of the analytical guide lines to these wastes. Pulverization and homogenization method for ash waste was improved to prevent a contamination since the radioactivity concentrations of the ash samples were relatively high. Pre-treatment method was altered for the cement solidified product and ash samples taking account for their high concentration of Ca. Newly, an analytical method was also developed to measure 129 I with a dynamic reaction cell inductively coupled plasma mass spectrometer. In the analytical test based on the improved guide lines, gamma-ray emitting nuclides, 60 Co and 137 Cs, were measured to estimate the radioactivity of the other alpha and beta-ray emitting nuclides. The radionuclides assumed detectable, 3 H, 14 C, 36 Cl, 63 Ni, 90 Sr, and alpha-ray emitting nuclides, were analyzed with the improved analytical guide lines and their applicability for cement solidified product and ash samples were confirmed. Additionally a cement solidified product sample was evaluated in terms of the homogeneity and the radioactivity concentrations in order to prepare a reference material for radiochemical analysis. (author)

  19. Determination of non-ortho polychlorinated biphenyls in environmental Standard Reference Materials.

    Science.gov (United States)

    Brubaker, W W; Schantz, M M; Wise, S A

    2000-07-01

    The concentrations of three non-ortho ("coplanar") polychlorinated biphenyls, 3,3',4,4'-tetrachlorobiphenyl (IUPAC PCB 77), 3,3',4,4',5-pentachlorobiphenyl (IUPAC PCB 126), and 3,3',4,4',5,5'-hexachlorobiphenyl (IUPAC PCB 169), were determined in five NIST Standard Reference Materials (SRMs) of environmental and biological interest. The measured levels were approximately between (0.2 to 1.3) ng/g in SRM 1588a (Organics in Cod Liver Oil), (0.3 to 9) ng/g in SRM 1944 (New York/New Jersey Waterway Sediment), (0.2 to 0.4) ng/g in SRM 1945 (Organics in Whale Blubber), (1 to 18) ng/g in SRM 2974 (Organics in Freeze-dried Mussel Tissue [Mytilus edulis]), and (0.1 to 0.4) ng/g in candidate SRM 1946 (Lake Superior Fish Tissue). PCB 169 was present at < 0.1 ng/g in SRMs 1944 and 2974.

  20. Multielemental analysis in small amounts of environmental reference materials with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Dombovári, J; Becker, J S; Dietze, H J

    2000-07-01

    The lowest possible sample weight for performing multielemental trace element analysis on environmental and biological samples by ICP-MS has been investigated. The certified reference materials Bovine Liver NIST SRM 1577b, Human Hair NCS DC 73347 and Oriental Tobacco Leaves CTA-OTL-1 were applied at sample weights (1, 5, 20 and 50 mg aliquots, n = 10) which were significantly lower than those recommended with most recoveries in the range of 95-110%. Samples were digested in a mixture of nitric acid, hydrogen peroxide and hydrogen fluoride by closed-vessel microwave digestion. Multielemental analysis was performed with an optimized ICP-QMS method. Aqueous standard solutions were applied for external calibration with rhodium as the internal standard element. The detection limits varied between 0.02-0.38 microg/g for Li, Na, Cr, Mn, Ni, Cu, Zn, Sr, Cd, Ba and Pb, and up to 1.92 microg/g for Mg, Al, Ca, Fe and Ni. Digested human plasma samples were spiked with multielemental solution (0.5-10 microg/L) to test the analytical method and the recoveries were 95-105% for most analytes. Our results show that in the case of homogeneous SRMs it is possible to use them in very low amounts (1-5 mg) for method development and quality control.

  1. Trace elements determination in silicon and ferrosilicon reference materials by instrumental neutron activation analysis method

    International Nuclear Information System (INIS)

    Moreira, Edson Goncalves; Vasconcellos, Marina Beatriz Agostini; Saiki, Mitiko; Iamashita, Celia Omine

    2002-01-01

    The use of certified reference materials, CRM, is of uppermost importance in the rastreability realization of the measurement process. At times, CRM use is restricted by the non existence of a suitable CRM with similarity to the sample in respect to matrix composition or with element levels in different orders of magnitude. IPT Chemical Division launched a project to prepare a metallic silicon CRM, due to the requirements of the industries in this field. To characterize this new CRM, IPEN Nuclear Reactor Center is able to perform instrumental neutron activation analysis, INAA, a very suitable method for silicon matrix samples because they produce basically the short lived radionuclide 3 1 Si under thermal neutrons flux, which after radioactive decay, does not interfere in the determination of other elements. In this paper, it is presented the determination of As, Br, Co, Cr, K, Eu, Fe, La, Mn, Na Nb, Sb, Sm, Sc, Th, Tb, U, V, W and Yb in silicon CRM NBS SRM 57; ferrosilicon CRM IPT 56; IPT 70; NBS SRM 58a; NBS SRM 59a and silicon RM under preparation IPT 132. From the results, the accuracy and the precision of the process were assessed. (author)

  2. Development of a Certified Reference Material (NMIJ CRM 7203-a) for Elemental Analysis of Tap Water.

    Science.gov (United States)

    Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Miyashita, Shin-Ichi; Kuroiwa, Takayoshi; Ariga, Tomoko; Kudo, Izumi; Koguchi, Masae; Heo, Sung Woo; Suh, Jung Ki; Lee, Kyoung-Seok; Yim, Yong-Hyeon; Lim, Youngran

    2017-01-01

    A certified reference material (CRM), NMIJ CRM 7203-a, was developed for the elemental analysis of tap water. At least two independent analytical methods were applied to characterize the certified value of each element. The elements certified in the present CRM were as follows: Al, As, B, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Ni, Pb, Rb, Sb, Se, Sr, and Zn. The certified value for each element was given as the (property value ± expanded uncertainty), with a coverage factor of 2 for the expanded uncertainty. The expanded uncertainties were estimated while considering the contribution of the analytical methods, the method-to-method variance, the sample homogeneity, the long-term stability, and the concentrations of the standard solutions for calibration. The concentration of Hg (0.39 μg kg -1 ) was given as the information value, since loss of Hg was observed when the sample was stored at room temperature and exposed to light. The certified values of selected elements were confirmed by a co-analysis carried out independently by the NMIJ (Japan) and the KRISS (Korea).

  3. Report on the characterization of the naturally grown algae Reference Material IAEA-392

    International Nuclear Information System (INIS)

    Zeiller, E.; Shakhashiro, A.

    2005-12-01

    This report describes the characterization of IAEA 392, naturally grown algae Reference Material, for mass fractions (of concentration) of several major, minor and trace elements. Details are given on the homogeneity studies, the long term stability, the analytical work performed and the evaluation of the data. Recommended values for the elemental content could be established for: Ca (2680±67.4mg/kg), Cu (23.2±1.7 mg/kg), Fe (497±13.6 mg/kg), Mg (2376±78.8 mg/kg), Mn (67.5±1.54 mg/kg), Na (680±23.0 mg/kg), Ni (0.571±0.028 mg/kg), Pb (0.574 ±0.028 mg/kg) and Zn (128±2.0 mg/kg) For As (0.175±0.016 mg/kg), Cd (0.0173±0.0014 mg/kg), Co (3.33±0.12 mg/kg), Cr (4.57±0.18 mg/kg), and K (8383±252 mg/kg), information values are reported. (author)

  4. Inter-laboratory analysis of selected genetically modified plant reference materials with digital PCR.

    Science.gov (United States)

    Dobnik, David; Demšar, Tina; Huber, Ingrid; Gerdes, Lars; Broeders, Sylvia; Roosens, Nancy; Debode, Frederic; Berben, Gilbert; Žel, Jana

    2018-01-01

    Digital PCR (dPCR), as a new technology in the field of genetically modified (GM) organism (GMO) testing, enables determination of absolute target copy numbers. The purpose of our study was to test the transferability of methods designed for quantitative PCR (qPCR) to dPCR and to carry out an inter-laboratory comparison of the performance of two different dPCR platforms when determining the absolute GM copy numbers and GM copy number ratio in reference materials certified for GM content in mass fraction. Overall results in terms of measured GM% were within acceptable variation limits for both tested dPCR systems. However, the determined absolute copy numbers for individual genes or events showed higher variability between laboratories in one third of the cases, most possibly due to variability in the technical work, droplet size variability, and analysis of the raw data. GMO quantification with dPCR and qPCR was comparable. As methods originally designed for qPCR performed well in dPCR systems, already validated qPCR assays can most generally be used for dPCR technology with the purpose of GMO detection. Graphical abstract The output of three different PCR-based platforms was assessed in an inter-laboratory comparison.

  5. Determination of 25 elements in biological standard reference materials by neutron activation analysis

    International Nuclear Information System (INIS)

    Guzzi, G.; Pietra, R.; Sabbioni, E.

    1974-12-01

    Standard and Certified Reference Materials programme of the JRC includes the determination of trace elements in complex biological samples delivered by the U.S. National Bureau of Standards: Bovine liver (NBS SRM 1577), Orchard Leaves (NBS SRM 1571) and Tomato Leaves. The study has been performed by the use of neutron activation analysis. Due to the very low concentration of some elements, radiochemical groups or elemental separation procedures were necessary. The paper describes the techniques used to analyse 25 elements. Computer assisted instrumental neutron activation analysis with high resolution Ge(Li) spectrometry was considerably advantageous in the determination of Na, K, Cl, Mn, Fe, Rb and Co and in some cases of Ca, Zn, Cs, Sc, and Cr. For low contents of Ca, Mg, Ni and Si special chemical separation schemes, followed by Cerenkov counting have been developped. Two other separation procedures allowing the determination of As, Cd, Ga, Hg, Mo, Cu, Sr Se, Ba and P have been set up. The first, the simplified one involves the use of high resolution Ge(Li) detectors, the second, the more complete one involves a larger number of shorter measurements performed by simpler and more sensitive techniques, such as NaI(Tl) scintillation spectrometry and Cerenkov counting. The results obtained are presented and discussed

  6. Development of bone-lead reference materials for validating in vivo XRF measurements

    International Nuclear Information System (INIS)

    Parsons, P.J.; Zong, Y.Y.; Matthews, M. R.

    1995-01-01

    A number of biological reference materials (RM) have been prepared in our laboratory specifically for validating analytical methods for the determination of Pb in biological matrices (e.g. blood, urine, liver, and bone). The RM's were developed using animal (goats and cows) that are routinely dosed with lead acetate to produce proficiency test samples for blood lead (and erythrocyte protoporphyrin). In cases where an animal becomes injured or infirm, the veterinarian in charge may recommend that the animal be euthanized. In such cases, samples of bone, brain, liver, and other tissues containing lead are removed at autopsy. Currently, we have collected bone samples from nine goats and one cow that were dosed with lead over periods ranging from 1 to 10 years. During the autopsy, the epiphyses (bone joints) are separated from each long bone. Skin, muscle, and other adhering tissues are dissected or scraped from each bone. Bone marrow is also removed. All bare bones are currently stored at -70 degrees C until analyses for Pb are conducted

  7. Application of INAA complementary gamma ray photopeaks to homogeneity study of candidate reference materials

    International Nuclear Information System (INIS)

    Moreira, Edson G.; Vasconcellos, Marina B.A.; Lima, Ana P.S.; Catharino, Marilia G.M.; Maihara, Vera A.; Saiki, Mitiko

    2009-01-01

    Characterization and certification of reference materials, RMs, is a complex task involving many steps. One of them is the homogeneity testing to assure that key property values will not present variation among RM bottles. Good precision is the most important figure of merit of an analytical technique to allow it to be used in the homogeneity testing of candidate RMs. Due to its inherent characteristics, Instrumental Neutron Activation Analysis, INAA, is an analytical technique of choice for homogeneity testing. Problems with sample digestion and contamination from reagents are not an issue in INAA, as solid samples are analyzed directly. For element determination via INAA, the activity of a suitable gamma ray decay photopeak for an element is chosen and it is compared to the activity of a standard of the element. An interesting possibility is the use of complementary gamma ray photopeaks (for the elements that present them) to confirm the homogeneity test results for an element. In this study, an investigation of the use of the complementary gamma ray photopeaks of 110 mAg, 82 Br, 60 Co, 134 Cs, 152 Eu, 59 Fe, 140 La, 233 Pa (for Th determination), 46 Sc and 75 Se radionuclides was undertaken in the between bottle homogeneity study of a mussel candidate RM under preparation at IPEN - CNEN/SP. Although some photopeaks led to biased element content results, the use of complementary gamma ray photopeaks proved to be helpful in supporting homogeneity study conclusions of new RMs. (author)

  8. Determination of Al, Si and P in certified reference materials by Instrumental Neutron Activation Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Noyori, Amanda; Saiki, Mitiko, E-mail: anoyori@gmail.com, E-mail: mitiko@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2017-11-01

    Neutron analysis activation is not commonly used for aluminum, phosphorus and silicon determination, due to the difficulty to obtain reliable results. In this study, Al was determined by measuring {sup 28}Al and the contribution of P and Si due to {sup 28}Al formed in {sup 31}P(n,α){sup 28}Al and {sup 28}Si(n,p){sup 28}Al reactions were corrected using correction factors determined experimentally. Phosphorus was determined by measuring {sup 32}P (pure beta emitter) formed in reaction {sup 31}P(n,γ){sup 32}P. Silicon was determined by epithermal neutron analysis activation (ENAA) and measuring {sup 29}Al radionuclide formed in {sup 29}Si(n,p){sup 29}Al reaction. Aliquots of certified reference materials (CRMs) and synthetic standards of the elements were irradiated together, using the pneumatic transfer station of IEA-R1 nuclear research reactor. Results obtained for biological and geological CRMs showed good precision and accuracy with |Z-score| < 2 for Al, P and Si determinations. The detection limits for Al, P and Si determinations CRMs were also evaluated. Results obtained in this study demonstrated the viability of applying INAA procedures in the determination of Al, P and Si. (author)

  9. ICP-MS determination of boron: method optimization during preparation of graphite reference material for boron

    International Nuclear Information System (INIS)

    Granthali, S.K.; Shailaja, P.P.; Mainsha, V.; Venkatesh, K.; Kallola, K.S.; Sanjukta, A.K.

    2017-01-01

    Graphite finds widespread use in nuclear reactors as moderator, reflector, and fuel fabricating components because of its thermal stability and integrity. The manufacturing process consists of various mixing, moulding and baking operations followed by heat-treatment between 2500 °C and 3000 °C. The high temperature treatment is required to drive the amorphous carbon-to-graphite phase transformation. Since synthetic graphite is processed at high temperature, impurity concentrations in the precursor carbon get significantly reduced due to volatilization. However boron may might partly gets converted into boron carbide at high temperatures in the carbon environment of graphite and remains stable (B_4C: boiling point 3500 °C) in the matrix. Literature survey reveals the use of various methods for determination of boron. Previously we have developed a method for determination of boron in graphite electrodes using inductively coupled plasma mass spectrometry (ICP-MS). The method involves removal of graphite matrix by ignition of the sample at 800°C in presence of saturated barium hydroxide solution to prevent the loss of boron. Here we are reporting a modification in the method by using calcium carbonate in place of barium hydroxide and using beryllium (Be) as an internal standard, which resulted in a better precession. The method was validated by spike recovery experiments as well as using another technique viz. Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The modified method was applied in evaluation of boron concentration in the graphite reference material prepared

  10. Determination of Al, Si and P in certified reference materials by Instrumental Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Noyori, Amanda; Saiki, Mitiko

    2017-01-01

    Neutron analysis activation is not commonly used for aluminum, phosphorus and silicon determination, due to the difficulty to obtain reliable results. In this study, Al was determined by measuring "2"8Al and the contribution of P and Si due to "2"8Al formed in "3"1P(n,α)"2"8Al and "2"8Si(n,p)"2"8Al reactions were corrected using correction factors determined experimentally. Phosphorus was determined by measuring "3"2P (pure beta emitter) formed in reaction "3"1P(n,γ)"3"2P. Silicon was determined by epithermal neutron analysis activation (ENAA) and measuring "2"9Al radionuclide formed in "2"9Si(n,p)"2"9Al reaction. Aliquots of certified reference materials (CRMs) and synthetic standards of the elements were irradiated together, using the pneumatic transfer station of IEA-R1 nuclear research reactor. Results obtained for biological and geological CRMs showed good precision and accuracy with |Z-score| < 2 for Al, P and Si determinations. The detection limits for Al, P and Si determinations CRMs were also evaluated. Results obtained in this study demonstrated the viability of applying INAA procedures in the determination of Al, P and Si. (author)

  11. Calculation and analysis of a HTR-pebble-bed reference core in the low enriched (U, Pu)- and (U, Th)-cycle with the new modular programme system DRACULA-II

    International Nuclear Information System (INIS)

    Hoffmann, K.

    1975-12-01

    A short description of the programme system is given. Investigations are undertaken on the burn-up and temperature dependence of the resonance adsorption and the flux lowering in a fuel ball as well as the influence of the heterogeneous fuel distribution in a ball-shaped fuel element on the neutron spectrum. The feedback of these effects on the burn-up behaviour is analysed in the subsequent calculations of the above-mentioned reference cores. Beyond this a comparison of the DRAKULA II results with the VSOP calculations for these reference cores is performed and discussed. Especially the new graphical plotting possibility has to be mentioned for the burn-up and load condition of individual fuel element balls during their flow through the core in addition with the netto balance of the isotope vector at their removal from the reactor. (orig.) [de

  12. The effects of preparation, shipment and ageing on the Pu elemental assay results of milligram-sized samples

    International Nuclear Information System (INIS)

    Berger, J.; Doubek, N.; Jammet, G.; Aigner, H.; Bagliano, G.; Donohue, D.; Kuhn, E.

    1994-02-01

    Specialized procedures have been implemented for the sampling of Pu-containing materials such as Pu nitrate, oxide or mixed oxide in States which have not yet approved type B(U) shipment containers for the air-shipment of gram-sized quantities of Pu. In such cases, it it necessary to prepare samples for shipment which contain only milligram quantities of Pu dried from solution in penicillin vials. Potential problems due to flaking-off during shipment could affect the recovery of Pu at the analytical laboratory. Therefore, a series of tests was performed with synthetic Pu nitrated, and mixed U, Pu nitrated samples to test the effectiveness of the evaporation and recovery procedures. Results of these tests as well as experience with actual inspection samples are presented, showing conclusively that the existing procedures are satisfactory. (author). 11 refs, 6 figs, 8 tabs

  13. Development of Lentivirus-Based Reference Materials for Ebola Virus Nucleic Acid Amplification Technology-Based Assays.

    Science.gov (United States)

    Mattiuzzo, Giada; Ashall, James; Doris, Kathryn S; MacLellan-Gibson, Kirsty; Nicolson, Carolyn; Wilkinson, Dianna E; Harvey, Ruth; Almond, Neil; Anderson, Robert; Efstathiou, Stacey; Minor, Philip D; Page, Mark

    2015-01-01

    The 2013-present Ebola virus outbreak in Western Africa has prompted the production of many diagnostic assays, mostly based on nucleic acid amplification technologies (NAT). The calibration and performance assessment of established assays and those under evaluation requires reference materials that can be used in parallel with the clinical sample to standardise or control for every step of the procedure, from extraction to the final qualitative/quantitative result. We have developed safe and stable Ebola virus RNA reference materials by encapsidating anti sense viral RNA into HIV-1-like particles. The lentiviral particles are replication-deficient and non-infectious due to the lack of HIV-1 genes and Envelope protein. Ebola virus genes were subcloned for encapsidation into two lentiviral preparations, one containing NP-VP35-GP and the other VP40 and L RNA. Each reference material was formulated as a high-titre standard for use as a calibrator for secondary or internal standards, and a 10,000-fold lower titre preparation to serve as an in-run control. The preparations have been freeze-dried to maximise stability. These HIV-Ebola virus RNA reference materials were suitable for use with in-house and commercial quantitative RT-PCR assays and with digital RT-PCR. The HIV-Ebola virus RNA reference materials are stable at up to 37°C for two weeks, allowing the shipment of the material worldwide at ambient temperature. These results support further evaluation of the HIV-Ebola virus RNA reference materials as part of an International collaborative study for the establishment of the 1st International Standard for Ebola virus RNA.

  14. Development of Lentivirus-Based Reference Materials for Ebola Virus Nucleic Acid Amplification Technology-Based Assays.

    Directory of Open Access Journals (Sweden)

    Giada Mattiuzzo

    Full Text Available The 2013-present Ebola virus outbreak in Western Africa has prompted the production of many diagnostic assays, mostly based on nucleic acid amplification technologies (NAT. The calibration and performance assessment of established assays and those under evaluation requires reference materials that can be used in parallel with the clinical sample to standardise or control for every step of the procedure, from extraction to the final qualitative/quantitative result. We have developed safe and stable Ebola virus RNA reference materials by encapsidating anti sense viral RNA into HIV-1-like particles. The lentiviral particles are replication-deficient and non-infectious due to the lack of HIV-1 genes and Envelope protein. Ebola virus genes were subcloned for encapsidation into two lentiviral preparations, one containing NP-VP35-GP and the other VP40 and L RNA. Each reference material was formulated as a high-titre standard for use as a calibrator for secondary or internal standards, and a 10,000-fold lower titre preparation to serve as an in-run control. The preparations have been freeze-dried to maximise stability. These HIV-Ebola virus RNA reference materials were suitable for use with in-house and commercial quantitative RT-PCR assays and with digital RT-PCR. The HIV-Ebola virus RNA reference materials are stable at up to 37°C for two weeks, allowing the shipment of the material worldwide at ambient temperature. These results support further evaluation of the HIV-Ebola virus RNA reference materials as part of an International collaborative study for the establishment of the 1st International Standard for Ebola virus RNA.

  15. Determination of polychlorinated dibenzo-p-dioxin and dibenzofuran congeners in air particulate and marine sediment standard reference materials (SRMs).

    Science.gov (United States)

    Chiu, C H; Turle, R; Poole, G; Thibert, B; Brubaker, W W; Schantz, M M; Wise, S A

    2001-02-01

    Due to the limited number of environmental matrix certified reference materials (CRMs) with assigned values for natural levels of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), an interlaboratory study was undertaken by the National Institute of Standards and Technology (NIST) and Environment Canada to establish reference concentration values for selected PCDD/Fs in two well-characterized NIST Standard Reference Materials (SRMs): SRM 1649a (Urban Dust) and SRM 1944 (New York/New Jersey Waterway Sediment). Results from 14 laboratories were used to provide reference values for the seventeen 2, 3, 7, 8-substituted PCDD/F congeners, the totals for individual tetra- through hepta-substituted PCDD/F homologues, and the total amount of tetra- through hepta-substituted PCDD/Fs. The mass fractions for the individual 2, 3, 7, 8-substituted congeners range from approximately 0.01 microg/kg to 7 microg/kg dry mass.

  16. U.S. N.R.C. special safeguards study on nuclear material control and accounting

    International Nuclear Information System (INIS)

    Smith, G.D.

    1976-01-01

    In Feb. 1975, NRC directed that an effort be made to determine a safeguards program for Pu recycle. This paper summarizes results of individual contractor evaluations of upgrading material control and accounting concepts as applied to strategically important special nuclear material and describes staff interpretations of these results as applied to future high-throughput fuel-cycle facilities. Real-time material control, design for physical inventory, Pu isotopics control and calorimetry, and material control and accounting for highly enriched uranium fuel materials were the concepts studied. 1 table, 15 references

  17. Preparation and characterization of 238Pu-ceramics for radiation damage experiments

    International Nuclear Information System (INIS)

    DM Strachan; RD Scheele; WC Buchmiller; JD Vienna; RL Sell; RJ Elovich

    2000-01-01

    As a result of treaty agreements between Russia and the US, portions of their respective plutonium and nuclear weapons stockpiles have been declared excess. In support of the US Department of Energy's 1998 decision to pursue immobilization of a portion of the remaining Pu in a titanate-based ceramic, the authors prepared nearly 200 radiation-damage test specimens of five Pu- and 238 Pu-ceramics containing 10 mass% Pu to determine the effects of irradiation from the contained Pu and U on the ceramic. The five Pu-ceramics were (1) phase-pure pyrochlore [ideally, Ca(U, Pu)Ti 2 O 7 ], (2) pyrochlore-rich baseline, (3) pyrochlore-rich baseline with impurities, (4) phase-pure zirconolite [ideally Ca(U, Pu)Ti 2 O 7 ], and (5) a zirconolite-rich baseline. These ceramics were prepared with either normal weapons-grade Pu, which is predominantly 239 Pu, or 238 Pu. The 238 Pu accelerates the radiation damage relative to the 239 Pu because of its much higher specific activity. The authors were unsuccessful in preparing phase-pure (Pu, U) brannerite, which is the third crystalline phase present in the baseline immobilization form. Since these materials will contain ∼10 mass% Pu and about 20 mass% U, radiation damage to the crystalline structure of these materials will occur overtime. As the material becomes damaged from the decay of the Pu and U, it is possible for the material to swell as both the alpha particles and recoiling atoms rupture chemical bonds within the solid. As the material changes density, cracking, perhaps in the form of microcracks, may occur. If cracking occurs in ceramic that has been placed in a repository, the calculated rate of radionuclide release if the can has corroded would increase proportionately to the increase in surface area. To investigate the effects of radiation damage on the five ceramics prepared, the authors are storing the specimens at 20, 125, and 250 C until the 238 Pu specimens become metamict and the damage saturates. They will

  18. Multi-isotopic determination of plutonium (239Pu, 240Pu, 241Pu and 242Pu) in marine sediments using sector-field inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Donard, O F X; Bruneau, F; Moldovan, M; Garraud, H; Epov, V N; Boust, D

    2007-03-28

    Among the transuranic elements present in the environment, plutonium isotopes are mainly attached to particles, and therefore they present a great interest for the study and modelling of particle transport in the marine environment. Except in the close vicinity of industrial sources, plutonium concentration in marine sediments is very low (from 10(-4) ng kg(-1) for (241)Pu to 10 ng kg(-1) for (239)Pu), and therefore the measurement of (238)Pu, (239)Pu, (240)Pu, (241)Pu and (242)Pu in sediments at such concentration level requires the use of very sensitive techniques. Moreover, sediment matrix contains huge amounts of mineral species, uranium and organic substances that must be removed before the determination of plutonium isotopes. Hence, an efficient sample preparation step is necessary prior to analysis. Within this work, a chemical procedure for the extraction, purification and pre-concentration of plutonium from marine sediments prior to sector-field inductively coupled plasma mass spectrometry (SF-ICP-MS) analysis has been optimized. The analytical method developed yields a pre-concentrated solution of plutonium from which (238)U and (241)Am have been removed, and which is suitable for the direct and simultaneous measurement of (239)Pu, (240)Pu, (241)Pu and (242)Pu by SF-ICP-MS.

  19. 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)

  20. The radiolysis of solutions containing Pu(6)

    International Nuclear Information System (INIS)

    Rance, P.J.W.; Zilberman, B.Y.

    2000-01-01

    The reduction of Pu(VI) in nitric acid solutions containing uranium and various fission product elements as a result of both its inherent alpha radiation and also external gamma irradiation at dose rates similar to those experienced by dissolved fuel solutions has been investigated. The presence of the additional metals has been shown to eliminate the induction periods required prior to the reduction of Pu(VI) in nitric acid. G values for the auto-radiolytic reduction of Pu(VI) have been found to be between 0.6 and 1.1 for 3 g/1 Pu solutions containing between 0.12 and 9.2 % 238 Pu (balance 239 Pu). Uranium and palladium have been found to accelerate the reduction of Pu(VI) during gamma irradiation at dose rates of between 0.41 and 1.64 kGy/hour. (authors)