WorldWideScience

Sample records for certified reference materials

  1. Certified reference materials for organic analysis

    International Nuclear Information System (INIS)

    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

  2. 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.

  3. BCR certified reference materials for reactor neutron dosimetry

    International Nuclear Information System (INIS)

    A series of reference materials intended for use as activation or fission monitors for neutron fluence rate measurements has been prepared by the Joint Research Centre of the European Commission. Certification has been carried out by expert European laboratories and distribution of the certified reference materials (CRMs) is through the BCR programme of the Commission. The list (18 CRMs) includes materials to cover the complete energy spectrum, and suitable for different irradiation times. Fission monitors are 238UO2 or 237NpO2 in the form of microspheres. Activation monitors are high purity metals (Ni, Cu, Al, Fe, Nb, Rh, or Ti), certified for interfering trace impurities, or dilute aluminium-based alloys, where aluminium is chosen as a suitable matrix for reducing the neutron self-shielding effect. Newly certified materials are IRMM-530R Al-0.1%Au, replacing the exhausted IRMM-530 material, used as comparator for k0-standardization, and three new Al-Co alloys (0.01-1%Co). Two others, in the process of certification are Al-0.1%Ag and Al-2%Sc for thermal and epithermal fluence rate measurements. Other candidate reference materials currently being certified are two uranium-doped glass intended for dosimetry by the fission-track technique. (author)

  4. Certified reference materials of trace elements in water

    Indian Academy of Sciences (India)

    A K Agrawal

    2005-07-01

    Measurement of trace elements is playing a vital role in industries and various sectors of science and technology including semiconductors, food, health and environmental sectors. In most of the cases a small error in measurement can vitiate all the measures taken for quality control and management. Many decisions regarding the suitability of material/products are based on the analysis. To reduce or eliminate the rejection rate of the products, accurate and reliable measurements are needed which can be achieved by the use of certified reference materials (CRMs). Their use in calibration of analytical equipments and validation of test methods ensures high quality in measurements and it provides traceability to the measurement data with national/international measurement systems (SI unit) also. In the present scenario of globalization of economy, use of certified reference materials (CRMs) in measurements is essential for global acceptance of products and test reports. Their use fulfil a mandatory requirement of international quality systems (ISO 9000, ISO/IEC standard 17025) including our national accreditation body, National Accreditation Board for Testing and Calibration Laboratories (NABL), World Trade Organization (WTO) etc. International manufacturers of CRMs are meeting most of the requirement of CRMs of the country. To meet the demand of CRMs indigenously, the National Physical Laboratory, India initiated a national programme on preparation and dissemination of certified reference materials.

  5. 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.

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

    International Nuclear Information System (INIS)

    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 235U, indicating the so-called ‘enrichment’, in nuclear material and in environmental samples. In addition to the verification of the major ratios, n(235U)/n(238U) and n(240Pu)/n(239Pu), 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

  7. 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 f...

  8. Assessment of Commutability for Candidate Certified Reference Material ERM-BB130 "Chloramphenicol in Pork"

    OpenAIRE

    Zeleny, Reinhard; EMTEBORG Per; Schimmel, Heinz

    2010-01-01

    Chloramphenicol (CAP), an effective antibiotic against many microorganisms, is meanwhile banned in the EU for treatment of food-producing animals due to adverse health effects. The Institute for Reference Materials and Measurements (IRMM) is currently developing a certified reference material (CRM) for CAP in pork, intended for validation and method performance verifications of analytical methods. The material will be certified using liquid chromatography tandem mass spectrometry (LC-MS/MS) a...

  9. 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

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

    International Nuclear Information System (INIS)

    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

  11. A mussel (Mytilus edulis) tissue certified reference material for the marine biotoxins azaspiracids

    OpenAIRE

    McCarron, Pearse; Giddings, Sabrina D.; Reeves, Kelley L.; Hess, Philipp; Michael A. Quilliam

    2015-01-01

    Azaspiracids (AZAs) are lipophilic biotoxins produced by marine algae that can contaminate shellfish and cause human illness. The European Union (EU) regulates the level of AZAs in shellfish destined for the commercial market, with liquid chromatography-mass spectrometry (LC-MS) being used as the official reference method for regulatory analysis. Certified reference materials (CRMs) are essential tools for the development, validation, and quality control of LC-MS methods. This paper describes...

  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 of...

  13. Development of a mushroom powder Certified Reference Material for calcium, arsenic, cadmium and lead measurements.

    Science.gov (United States)

    Chew, Gina; Sim, Lay Peng; Ng, Sin Yee; Ding, Yi; Shin, Richard Y C; Lee, Tong Kooi

    2016-01-01

    Isotope dilution mass spectrometry and standard addition techniques were developed for the analysis of four elements (Ca, As, Cd and Pb) in a mushroom powder material. Results from the validated methods were compared to those of other national metrology institutes in the CCQM-K89 intercomparisons and the results were in excellent agreement with the reference values. The same methods were then used for the assignment of reference values to a mushroom powder Certified Reference Material (CRM). The certified values obtained for Ca, As, Cd and Pb were 1.444 ± 0.099 mg/g, 5.61 ± 0.59 mg/kg, 1.191 ± 0.079 mg/kg and 5.23 ± 0.94 mg/kg, respectively. The expanded measurement uncertainties were obtained by combining the uncertainty contributions from characterization (uchar) and between-bottle homogeneity (ubb). PMID:26212973

  14. Applicability of microwave digestion for analysis of elements in certified reference material by ICP-MS

    International Nuclear Information System (INIS)

    Quality of an analysis is contingent by several factors such as analysis method, equipment performance, standard preparation, sample preparation, staff competency and environmental condition. One of other major factor that also contributes to the quality of analysis results is the sample pre-treatment. In this study, sample pretreatment is involving digestion process of certified reference material using microwave oven whilst elemental analysis (Ba, Cd, Cu, Mo, Ni, Pb, and Ti) was done by Inductively Couple Plasma - Mass Spectrometer (ICP-MS). The applicability of the analytical method is confirmed by analysis results of the certified reference material (CRM). The results showed that the recovery of the elements of the CRM is 65% to 133% with Z-score value of -1.63 to 1.67. (Author)

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

    International Nuclear Information System (INIS)

    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)

  16. Development and certification of a coal fly ash certified reference material for selected polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Cao, X; Xu, X; Cui, W; Xi, Z

    2001-08-01

    The development and certification of a coal fly ash certified reference material (CRM) for polycyclic aromatic hydrocarbons (PAH) is described; this is the first natural matrix CRM for organic environmental analysis in China. The homogeneity and stability of this material have been tested by HPLC. The concentrations of several PAH were determined by use of two independent, different methods--solvent extraction-HPLC analysis with UV detection coupled with fluorescence detection (FLD) and solvent extraction, isolation with a silica column, and GC analysis with flame ionization detection (FID). Five certified values were determined: phenanthrene 7.1 +/- 2.6 microg g(-1), anthracene 2.0 +/- 0.8 microg g(-1), fluoranthene 7.4 +/- 1.9 microg g(-1), pyrene 7 +/- 2 microg g(-1), and benzo[a]pyrene 1.3 +/- 0.3 microg g(-1). Reference values for several other PAH are also suggested. PMID:11583083

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

    Science.gov (United States)

    Pham, M K; Benmansour, M; Carvalho, F P; Chamizo, E; Degering, D; Engeler, C; Gascó, C; Gwynn, J P; Harms, A V; Hrnecek, E; Ibanez, F L; Ilchmann, C; Ikaheimonen, T; Kanisch, G; Kloster, M; Llaurado, M; Mauring, A; Møller, B; Morimoto, T; Nielsen, S P; Nies, H; Norrlid, L D R; Pettersson, H B L; Povinec, P P; Rieth, U; Samuelsson, C; Schikowski, J; Silobritiene, B V; Smedley, P A; Suplinska, M; Vartti, V-P; Vasileva, E; Wong, J; Zalewska, T; Zhou, W

    2014-05-01

    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 (40)K, (137)Cs, (234)U and (239+240)Pu radionuclides were certified for this material, and information values for 12 other radionuclides ((90)Sr, (99)Tc, (210)Pb ((210)Po), (226)Ra, (228)Ra, (228)Th, (230)Th, (232)Th, (235)U, (238)U, (239)Pu and (240)Pu) 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 of analytical methods, and for training purposes. PMID:24291528

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

    International Nuclear Information System (INIS)

    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 of radionuclides in water samples, for the development and validation of analytical methods and for training purposes. The material is available in 5 L units from IAEA (http://nucleus.iaea.org/rpst/index.htm). (author)

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

    International Nuclear Information System (INIS)

    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 239+240Pu 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 of analytical methods, and for training purposes

  20. Production of trace elements in coastal sea water certified reference material NMIA MX014.

    Science.gov (United States)

    Merrick, Jeffrey P; Saxby, David L; White, Ian E A W; Antin, Luminita; Murby, E John

    2016-06-01

    A certified reference material (CRM) for trace elements in acidified sea water, NMIA MX014, has been produced by the National Measurement Institute Australia (NMIA). The CRM consists of natural coastal sea water with 12 elements (As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Se and V) fortified to levels relevant to environmental regulatory testing in Australia ranging from 0.4 to 22 μg/kg. Certified values for these 12 elements were assigned using reference methods developed at NMIA, using either isotope dilution or standard addition with ICP-MS measurement. Specialised sample preparation (coprecipitation) and ICP-MS optimisation (online dilution, collision/reaction chemistry, high mass resolution) were used to negate the effect of the high level of dissolved solids. Multiple confirmatory experiments were performed in order to verify that ICP-MS spectral interferences were eliminated and to estimate the measurement uncertainty contribution from method precision and method trueness. Extensive homogeneity and stability testing was performed and the measurement uncertainty of certified values includes contributions from between-bottle homogeneity, short-term stability, medium-term stability and long-term stability. Special attention was paid to the stability of Hg due to well-known preservation problems. Acidified sea water matrix was satisfactory for stabilising Hg at 0.4 μg/kg for at least 4 years. Relative expanded uncertainties (k = 2) for the 12 certified values were between 1 and 11 %. NMIA MX014 is intended for use as a reference material for analytical method validation and quality control for quantification of trace elements in saline water and other similar sample types. PMID:27108283

  1. A new Certified Reference Material for radionuclides in Irish sea sediment (IAEA-385).

    Science.gov (United States)

    Pham, M K; Sanchez-Cabeza, J A; Povinec, P P; Andor, K; Arnold, D; Benmansour, M; Bikit, I; Carvalho, F P; Dimitrova, K; Edrev, Z H; Engeler, C; Fouche, F J; Garcia-Orellana, J; Gascó, C; Gastaud, J; Gudelis, A; Hancock, G; Holm, E; Legarda, F; Ikäheimonen, T K; Ilchmann, C; Jenkinson, A V; Kanisch, G; Kis-Benedek, G; Kleinschmidt, R; Koukouliou, V; Kuhar, B; Larosa, J; Lee, S-H; Lepetit, G; Levy-Palomo, I; Liong Wee Kwong, L; Llauradó, M; Maringer, F J; Meyer, M; Michalik, B; Michel, H; Nies, H; Nour, S; Oh, J-S; Oregioni, B; Palomares, J; Pantelic, G; Pfitzner, J; Pilvio, R; Puskeiler, L; Satake, H; Schikowski, J; Vitorovic, G; Woodhead, D; Wyse, E

    2008-11-01

    A new Certified Reference Material (CRM) for radionuclides in sediment (IAEA-385) is described and the results of the certification process are presented. Eleven radionuclides ((40)K, (137)Cs, (226)Ra, (228)Ra, (230)Th, (232)Th, (234)U, (238)U, (238)Pu, (239+240)Pu and (241)Am) have been certified and information mass activities with 95% confidence intervals are given for seven other radionuclides ((90)Sr, (210)Pb((210)Po), (235)U, (239)Pu, (240)Pu and (241)Pu). Results for less frequently reported radionuclides ((60)Co, (99)Tc, (134)Cs, (155)Eu, (224)Ra and (239)Np) and information on some activity and mass ratios are also reported. The CRM can be used for quality assurance/quality control of the analysis of radionuclides in sediment samples, for the development and validation of analytical methods and for training purposes. PMID:18513984

  2. A new Certified Reference Material for radionuclides in Irish sea sediment (IAEA-385)

    International Nuclear Information System (INIS)

    A new Certified Reference Material (CRM) for radionuclides in sediment (IAEA-385) is described and the results of the certification process are presented. Eleven radionuclides (40K, 137Cs, 226Ra, 228Ra, 230Th, 232Th, 234U, 238U, 238Pu, 239+240Pu and 241Am) have been certified and information mass activities with 95% confidence intervals are given for seven other radionuclides (90Sr, 210Pb(210Po), 235U, 239Pu, 240Pu and 241Pu). Results for less frequently reported radionuclides (60Co, 99Tc, 134Cs, 155Eu, 224Ra and 239Np) and information on some activity and mass ratios are also reported. The CRM can be used for quality assurance/quality control of the analysis of radionuclides in sediment samples, for the development and validation of analytical methods and for training purposes

  3. 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 certifi...

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

    International Nuclear Information System (INIS)

    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)

  5. DNA copy number concentration measured by digital and droplet digital quantitative PCR using certified reference materials

    OpenAIRE

    CORBISIER Philippe; Pinheiro, Leonardo; Mazoua, Stephane; KORTEKAAS Anna Maria; CHUNG PUI YAN JENNY; GERGANOVA TSVETELINA IVANOVA; Roebben, Gert; Emons, Hendrik; Emslie, K

    2015-01-01

    The value assignment for properties of six certified reference materials (ERM-AD623a–f), each containing a plasmid DNA solution ranging from 1 million to 10 copies per μL, by using digital PCR (dPCR) with the BioMark™ HD System (Fluidigm) has been verified by applying droplet digital PCR (ddPCR) using the QX100 system (Bio-Rad). One of the critical factors in the measurement of copy number concentrations by digital PCR is the partition volume. Therefore, we determined the average droplet volu...

  6. Preparation of homogeneous thorium oxide powders for development of certified reference materials

    International Nuclear Information System (INIS)

    In view of the growing importance of Thorium Oxide (ThO2) as a fuel in nuclear power reactors, it is essential to develop Certified Reference Materials (CRMs) for trace level assay of ThO2 in order to validate analytical methods and also to assess the performance of an individual chemical laboratory. The present paper discusses the preparation of four batches of homogeneous Thorium Oxide (ThO2) powders on kilogram levels including a batch of ThO2 and Natural UO2 mixed oxide with varying amounts of impurities and also developing them as CRMs based on round robin tests. (author)

  7. Calibration of HPGe detectors using certified reference materials of natural origin

    International Nuclear Information System (INIS)

    The feasibility of using certified reference materials for the full energy efficiency calibration of p-type coaxial high-purity germanium detectors for the determination of radioactivity in environmental samples is discussed. The main sources of uncertainty are studied and the contributions to the total uncertainty budget for the most intense gamma lines are presented. The correction factors due to self-absorption and true coincidence summing effects are discussed in detail. The calibration procedure is validated for natural and artificial radionuclide determination in different matrices through an internal cross-validation and through the participation in a world-wide open proficiency test. (author)

  8. Certification of the equivalent spherical diameters of silica nanoparticles in aqueous solution - Certified Reference Material ERM®-FD304

    OpenAIRE

    FRANKS Katrin; BRAUN ADELINA; CHAROUD-GOT Jean; COUTEAU Olivier; KESTENS Vikram; LAMBERTY MARIE ANDREE; Linsinger, Thomas; Roebben, Gert

    2011-01-01

    This report describes the certification of several equivalent spherical diameters of silica nanoparticles in aqueous solution, Certified Reference Material (CRM) ERM®-FD304. The CRM has been certified by the European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Geel, BE. ERM-FD304 consists of silica nanoparticles suspended in aqueous solution. The intended use of this CRM is t o check the performance of instruments and methods that determine...

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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

  11. A mussel (Mytilus edulis) tissue certified reference material for the marine biotoxins azaspiracids.

    Science.gov (United States)

    McCarron, Pearse; Giddings, Sabrina D; Reeves, Kelley L; Hess, Philipp; Quilliam, Michael A

    2015-04-01

    Azaspiracids (AZAs) are lipophilic biotoxins produced by marine algae that can contaminate shellfish and cause human illness. The European Union (EU) regulates the level of AZAs in shellfish destined for the commercial market, with liquid chromatography-mass spectrometry (LC-MS) being used as the official reference method for regulatory analysis. Certified reference materials (CRMs) are essential tools for the development, validation, and quality control of LC-MS methods. This paper describes the work that went into the planning, preparation, characterization, and certification of CRM-AZA-Mus, a tissue matrix CRM, which was prepared as a wet homogenate from mussels (Mytilus edulis) naturally contaminated with AZAs. The homogeneity and stability of CRM-AZA-Mus were evaluated, and the CRM was found to be fit for purpose. Extraction and LC-MS/MS methods were developed to accurately certify the concentrations of AZA1 (1.16 mg/kg), AZA2 (0.27 mg/kg), and AZA3 (0.21 mg/kg) in the CRM. Quantitation methods based on standard addition and matrix-matched calibration were used to compensate for the matrix effects in LC-MS/MS. Other toxins present in this CRM at lower levels were also measured with information values reported for okadaic acid, dinophysistoxin-2, yessotoxin, and several spirolides. PMID:25335820

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

    Science.gov (United States)

    da Conceição, F. C.; Borges, P. P.; Gomes, J. F. S.

    2016-07-01

    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 (K2Cr2O7), 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.

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

    International Nuclear Information System (INIS)

    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.

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

    International Nuclear Information System (INIS)

    , production of reference materials and certified reference materials, and training. More than 40 reference materials have been produced, which include a wide range of marine sample matrices and radionuclide concentrations. As part of these activities, a new interlaboratory comparison was organized to provide the participating laboratories with the possibility to test the performance of their analytical methods for 129I on a Mediterranean sea water sample. The material was designed for the analysis of low level 129I in sea water. The sample, after successful certification, has been issued as a certified reference material for 129I in sea water. Laboratories were informed that, after the completion of the exercise, an IAEA report describing the results of the interlaboratory comparison would be issued, including their identities, but that the results would remain anonymous

  15. Assessment of commutability for candidate certified reference material ERM-BB130 "chloramphenicol in pork".

    Science.gov (United States)

    Zeleny, Reinhard; Emteborg, Håkan; Schimmel, Heinz

    2010-10-01

    Chloramphenicol (CAP), an effective antibiotic against many microorganisms, is meanwhile banned in the EU for treatment of food-producing animals due to adverse health effects. The Institute for Reference Materials and Measurements (IRMM) is currently developing a certified reference material (CRM) for CAP in pork, intended for validation and method performance verifications of analytical methods. The material will be certified using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) methods and has a target CAP level around the minimum required performance limit (MRPL) of 0.3 microg/kg. To prove that the material can be applied as a quality control tool for screening methods, a commutability study was conducted, involving five commercially available enzyme-linked immunosorbent assay kits and one biosensor assay (BiaCore kit). Meat homogenates (cryo-milled wet tissue) with CAP concentrations around the MRPL and the candidate CRM (lyophilised powder) were measured by LC-MS/MS and GC-MS as well as the six screening methods. Pairwise method comparisons of results obtained for the two sample types showed that the CRM can successfully be applied as quality control (QC) sample to all six screening methods. The study suggests that ERM-BB130 is sufficiently commutable with the investigated assays and that laboratories applying one of the investigated kits therefore benefit from using ERM-BB130 to demonstrate the correctness of their results. However, differences among the assays were observed, either in the abundance of bias between screening and confirmatory LC and GC methods, the repeatability of test results, or goodness of fit between the methods. PMID:20665007

  16. k0-NAA quality assessment by analysis of different certified reference materials using the KAYZERO/SOLCOI software

    International Nuclear Information System (INIS)

    A suite of natural matrix reference materials (RMs) were used to assess the quality of analytical results obtained by k0-instrumental neutron activation analysis (k0-INAA) at the Jozef Stefan Institute (IJS). Five certified reference materials (CRMs) from the Institute for Reference Materials and Measurements (IRMM), two standard reference materials (SRMs) from the National Institute of Standards and Technology (NIST), three RMs from the International Atomic Energy Agency (IAEA) and one RM from IJS were analyzed. Altogether, results for twenty-four elements in inorganic matrices and twenty-nine elements in organic matrices, obtained by k0-INAA, were compared to certified values. Results obtained show good agreement with certified or assigned values except for Fe, La, Nd, Sm and U in inorganic matrices, and Ag, Al and Cr in organic matrices. (author)

  17. Development of Certified Reference Materials for Diarrhetic Shellfish Poisoning Toxins, Part 1: Calibration Solutions.

    Science.gov (United States)

    Beach, Daniel G; Crain, Sheila; Lewis, Nancy; LeBlanc, Patricia; Hardstaff, William R; Perez, Ruth A; Giddings, Sabrina D; Martinez-Farina, Camilo F; Stefanova, Roumiana; Burton, Ian W; Kilcoyne, Jane; Melanson, Jeremy E; Quilliam, Michael A; McCarron, Pearse

    2016-09-01

    Okadaic acid (OA) and its analogs dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic polyethers produced by marine dinoflagellates. These toxins accumulate in shellfish and cause diarrhetic shellfish poisoning (DSP) in humans. Regulatory testing of shellfish is essential to safeguard public health and for international trade. Certified reference materials (CRMs) play a key role in analytical monitoring programs. This paper presents an overview of the interdisciplinary work that went into the planning, production, and certification of calibration-solution CRMs for OA, DTX1, and DTX2. OA and DTX1 were isolated from large-scale algal cultures and DTX2 from naturally contaminated mussels. Toxins were isolated by a combination of extraction and chromatographic steps with processes adapted to suit the source and concentration of each toxin. New 19-epi-DSP toxin analogs were identified as minor impurities. Once OA, DTX1, and DTX2 were established to be of suitable purity, solutions were prepared and dispensed into flame-sealed glass ampoules. Certification measurements were carried out using quantitative NMR spectroscopy and LC-tandem MS. Traceability of measurements was established through certified external standards of established purity. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization, with components from the measurement, stability, and homogeneity studies being propagated into final combined uncertainties. PMID:27524810

  18. A new Certified Reference Material for radionuclides in Irish sea sediment (IAEA-385)

    Energy Technology Data Exchange (ETDEWEB)

    Pham, M.K. [Marine Environment Laboratories, International Atomic Energy Agency, MC 98000 Principality of Monaco (Monaco)], E-mail: m.pham@iaea.org; Sanchez-Cabeza, J.A.; Povinec, P.P. [Marine Environment Laboratories, International Atomic Energy Agency, MC 98000 Principality of Monaco (Monaco); Andor, K. [Frederic Joliot-Curie National Research Inst. for Radiobiology and Radiohygiene, Anna u. 5, 1221 Budapest (Hungary); Arnold, D. [Physikalisch-Technische Bundesanstalt, Bundesallee 100, 38116 Braunschweig (Germany); Benmansour, M. [Centre National de l' Energies des Sciences et des Techniques Nucleaires, 1382 Agdal, Rabat 10001 (Morocco); Bikit, I. [Dept. of Physics, Faculty of Science and Mathematics, University of Novi Sad, Trg Dositeja Obradovica 4, 21000 Novi Sad, Serbia (Serbia ); Carvalho, F.P. [Instituto Tecnologico e Nuclear, E.N. 10, P-2686-953 Sacavem (Portugal); Dimitrova, K. [Executive Environment Agency of Bulgaria, Regional Laboratory Varna, 4 Jan Palah Str., Varna 9000 (Bulgaria); Edrev, Z.H. [Regional Inspectorate of Environment and Waters, 2 Stara Planina str., 6000 Stara Zagora (Bulgaria); Engeler, C. [Radiochemistry Dept., Institute for Inland Water Management and Waste Water Treatment, P.O. Box 17, 8200 AA Lelystad (Netherlands); Fouche, F.J. [South African Nuclear Energy Corporation NECSA Ltd., P.O. Box 582, Pretoria 0001 (South Africa); Garcia-Orellana, J. [Dept. de Fisica, Universitat Automona de Barcelona, 08193-Cerdanyola del Valles (Spain); Gasco, C. [Instituto de Medio Ambiente, Radioecologia del Medio Acuatico, Av. de la Complutense 22, 28040 Madrid (Spain); Gastaud, J. [Marine Environment Labs., International Atomic Energy Agency, MC 98000 Principality of Monaco (Monaco); Gudelis, A. [Institute of Physics, Nuclear and Environmental Radioactivity Research Lab., Savanoriu Ave 231, 2053 Vilnius (Lithuania); Hancock, G. [CSIRO Land and Water, Clunies Ross St., GPO Box 1666, Canberra, ACT 2601 (Australia)] (and others)

    2008-11-15

    A new Certified Reference Material (CRM) for radionuclides in sediment (IAEA-385) is described and the results of the certification process are presented. Eleven radionuclides ({sup 40}K, {sup 137}Cs, {sup 226}Ra, {sup 228}Ra, {sup 230}Th, {sup 232}Th, {sup 234}U, {sup 238}U, {sup 238}Pu, {sup 239+240}Pu and {sup 241}Am) have been certified and information mass activities with 95% confidence intervals are given for seven other radionuclides ({sup 90}Sr, {sup 210}Pb({sup 210}Po), {sup 235}U, {sup 239}Pu, {sup 240}Pu and {sup 241}Pu). Results for less frequently reported radionuclides ({sup 60}Co, {sup 99}Tc, {sup 134}Cs, {sup 155}Eu, {sup 224}Ra and {sup 239}Np) and information on some activity and mass ratios are also reported. The CRM can be used for quality assurance/quality control of the analysis of radionuclides in sediment samples, for the development and validation of analytical methods and for training purposes.

  19. Characterization of certified reference material for the quantification of water in bioethanol.

    Science.gov (United States)

    Inagaki, Shinsuke; Numata, Masahiko; Hanari, Nobuyasu; Iwasawa, Ryoko; Matsuo, Mayumi; Kato, Kenji

    2012-01-01

    The National Metrology Institute of Japan has issued a certified reference material of bioethanol (NMIJ CRM 8301-a) for the quantification of water, methanol, sulfur, and copper. This paper presents technical details for the characterization of the water in NMIJ CRM 8301-a. The characterization was performed using coulometric and volumetric Karl-Fischer (KF) titrations. To reduce moisture absorption, sample handling and KF titration were performed in a glove box under a dried nitrogen atmosphere. In addition, a rubber cap with a three-way valve was attached to the ampoule immediately after opening so as to minimize the influence of moisture. Sample aliquots were obtained using a gas-tight microsyringe through the valve, and injected into the KF cell as soon as possible. The certified value of water obtained from coulometric and volumetric KF titrations was 1.688 mg g(-1), and the expanded uncertainty (coverage factor, k = 2) was 0.028 mg g(-1). This CRM would be suitable for the monitoring of water in bioethanol and similar matrices. PMID:23149610

  20. Development of a certified reference material for genetically modified potato with altered starch composition.

    Science.gov (United States)

    Broothaerts, Wim; Corbisier, Philippe; Emons, Hendrik; Emteborg, Håkan; Linsinger, Thomas P J; Trapmann, Stefanie

    2007-06-13

    The presence of genetically modified organisms (GMOs) in food and feed products is subject to regulation in the European Union (EU) and elsewhere. As part of the EU authorization procedure for GMOs intended for food and feed use, reference materials must be produced for the quality control of measurements to quantify the GMOs. Certified reference materials (CRMs) are available for a range of herbicide- and insect-resistant genetically modified crops such as corn, soybean, and cotton. Here the development of the first CRM for a GMO that differs from its non-GMO counterpart in a major compositional constituent, that is, starch, is described. It is shown that the modification of the starch composition of potato (Solanum tuberosum L.) tubers, together with other characteristics of the delivered materials, have important consequences for the certification strategy. Moreover, the processing and characterization of the EH92-527-1 potato material required both new and modified procedures, different from those used routinely for CRMs produced from genetically modified seeds. PMID:17508757

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

    International Nuclear Information System (INIS)

    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 233U, 236gNp, 244Pu, and 243Am, 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)

  2. Toward the Development of Certified Reference Materials for Effective Biodiesel Testing - Part 1: Processing, Homogeneity, and Stability

    OpenAIRE

    ULBERTH-BUCHGRABER MANUELA; POTALIVO MONICA; EMTEBORG Per; HELD Andrea

    2011-01-01

    To address the current lack of certified reference materials (CRMs) for biodiesel analysis, the Institute for Reference Materials and Measurements (IRMM), Joint Research Centre (JRC), European Commission (EC), launched a comprehensive feasibility study on the production of biodiesel CRMs for relevant specification parameters as provided in EN 14214,1 the basis for defining product specifications and measurement methods for biodiesel in the European Union (EU). Laboratories need to be able to ...

  3. Development of certified matrix reference materials for quality assurance of screening 134Cs and 137Cs in food

    International Nuclear Information System (INIS)

    A certified reference material using activated alumina powder certified for activity of 134Cs and 137Cs was developed. The results of the verification and the certification are described. The certified reference material can be used for quality assurance of screening activity measurements of 134Cs and 137Cs in food/foodstuffs. Commercially available equipments were experimentally tested using the CRM and another CRM including 40K. The results of these tests are also shown. - Highlights: • CRM of 134Cs and 137Cs using activated alumina was developed. • CRM including 134Cs, 137Cs and 40K was also developed. • Results of experimental performance test of commercial inspection equipments using CRMs were shown

  4. Development of a new sodium diclofenac certified reference material using the mass balance approach and ¹H qNMR to determine the certified property value.

    Science.gov (United States)

    Nogueira, Raquel; Garrido, Bruno C; Borges, Ricardo M; Silva, Gisele E B; Queiroz, Suzane M; Cunha, Valnei S

    2013-02-14

    Certified reference materials (CRMs) are essential tools to guarantee the metrological traceability of measurement results to the International System of Units (SI), which means the accuracy and comparability of results over time and space. In the pharmaceutical area, only a few CRMs are available and the use of (non-certified) reference materials is a much more common practice. In this paper, the studies on a new candidate CRM of sodium diclofenac based on the ISO Guides 34:2009 and 35:2005 are described. The project steps included characterization, homogeneity test, stability studies, and uncertainties estimation. In the characterization, the mass fractions of organic, inorganic, and volatile impurities were determined, and the results were cross-checked by independent reference methods or interlaboratorial study. The API mass fraction was calculated by mass balance and cross-checked by quantitative proton nuclear magnetic resonance (¹H qNMR). The paper also presents a Monte Carlo simulation to estimate the measurement uncertainty as an approach to validate the GUM results in ¹H qNMR. The homogeneity between batch units was verified, and the candidate CRM stability under transport and storage conditions was evaluated in short- and long-term stability studies. The CRM certified property value and corresponding expanded uncertainty, obtained from the combined standard uncertainty multiplied by the coverage factor (k=2), for a confidence level of 95%, was (999.76+0.10) mg g⁻¹. PMID:23220339

  5. Determination of multielements in a typical Japanese diet certified reference material by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Multielements in a typical Japanese diet certified reference material prepared at the National Institute for Environmental Studies (NIES) of Japan, in collaboration with the National Institute of Radiological Sciences (NIRS) of Japan were determined by instrumental neutron activation analysis (INAA). Five samples (ca. 510 - 1000 mg) and comparative standards were irradiated for a short time (10 s) at a thermal neutron flux of 1.5 x 1012 n cm-2 s-1 (pneumatic transfer) and for a long time (6 h) at a thermal neutron flux of 3.7 x 1012 n cm-2 s-1 (central thimble) in the Rikkyo University Research Reactor (TRIGA Mark-II, 100 kW). The irradiated samples were measured by conventional γ-ray spectrometry using a coaxial Ge detector, and by anti-coincidence and coincidence γ-ray spectrometry with a coaxial Ge detector and a well-type NaI (Tl) detector. The concentrations of 38 elements were determined by these methods. (author)

  6. Determination of multielements in a typical Japanese diet certified reference material by instrumental neutron activation analysis.

    Science.gov (United States)

    Suzuki, Shogo; Okada, Yukiko; Hirai, Shoji

    2003-08-01

    Multielements in a typical Japanese diet certified reference material prepared at the National Institute for Environmental Studies (NIES) of Japan, in collaboration with the National Institute of Radiological Sciences (NIRS) of Japan were determined by instrumental neutron activation analysis (INAA). Five samples (ca. 510-1000 mg) and comparative standards were irradiated for a short time (10 s) at a thermal neutron flux of 1.5 x 10(12) n cm(-2) s(-1) (pneumatic transfer) and for a long time (6 h) at a thermal neutron flux of 3.7 x 10(12) n cm(-2) s(-1) (central thimble) in the Rikkyo University Research Reactor (TRIGA Mark-II, 100 kW). The irradiated samples were measured by conventional gama-ray spectrometry using a coaxial Ge detector, and by anti-coincidence and coincidence gamma-ray spectrometry with a coaxial Ge detector and a well-type NaI(Tl) detector. The concentrations of 38 elements were determined by these methods. PMID:12945682

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

    Roč. 39, č. 2 (2015), s. 209-220. ISSN 1639-4488 R&D Projects: GA ČR(CZ) GAP504/11/0484 Institutional support: RVO:61389005 Keywords : Pb isotopes * Pb-206 * Pb-207 * Pb-208 * ICP-MS * certified reference materials * vegetation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.792, year: 2013

  8. Human urine certified reference material: Creatinine and toluene metabolites: O-cresol and hippuric acid (preliminary studies)

    Czech Academy of Sciences Publication Activity Database

    Šperlingová, I.; Dabrowská, L.; Stránský, V.; Kučera, Jan; Tichý, M.

    2005-01-01

    Roč. 355, - (2005), s. 411-411. ISSN 0009-8981 Institutional research plan: CEZ:AV0Z10480505 Keywords : certified reference material * human urine * , creatinine and toluene metabolites Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 2.149, year: 2005

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

    Roč. 39, č. 2 (2015), s. 209-220. ISSN 1639-4488 Institutional support: RVO:67985831 Keywords : Pb isotopes * 206 Pb/ 207 Pb * 208 Pb/ 206 Pb * ICP-MS * certified reference materials * vegetation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.792, year: 2013

  10. 235Uranium isotope abundance certified reference material for gamma spectrometry EC nuclear reference material 171 certification report

    International Nuclear Information System (INIS)

    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 U3O8 samples with five different 235U/U abundances, filled in cylindrical aluminium cans. The can bottom serves as window for emitted gamma radiation. The report describes how the 235U/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

  11. Development of a new ferulic acid certified reference material for use in clinical chemistry and pharmaceutical analysis

    Directory of Open Access Journals (Sweden)

    Dezhi Yang

    2015-05-01

    Full Text Available This study compares the results of three certified methods, namely differential scanning calorimetry (DSC, the mass balance (MB method and coulometric titrimetry (CT, in the purity assessment of ferulic acid certified reference material (CRM. Purity and expanded uncertainty as determined by the three methods were respectively 99.81%, 0.16%; 99.79%, 0.16%; and 99.81%, 0.26% with, in all cases, a coverage factor (k of 2 (P=95%. The purity results are consistent indicating that the combination of DSC, the MB method and CT provides a confident assessment of the purity of suitable CRMs like ferulic acid.

  12. DNA copy number concentration measured by digital and droplet digital quantitative PCR using certified reference materials.

    Science.gov (United States)

    Corbisier, Philippe; Pinheiro, Leonardo; Mazoua, Stéphane; Kortekaas, Anne-Marie; Chung, Pui Yan Jenny; Gerganova, Tsvetelina; Roebben, Gert; Emons, Hendrik; Emslie, Kerry

    2015-03-01

    The value assignment for properties of six certified reference materials (ERM-AD623a-f), each containing a plasmid DNA solution ranging from 1 million to 10 copies per μL, by using digital PCR (dPCR) with the BioMark™ HD System (Fluidigm) has been verified by applying droplet digital PCR (ddPCR) using the QX100 system (Bio-Rad). One of the critical factors in the measurement of copy number concentrations by digital PCR is the partition volume. Therefore, we determined the average droplet volume by optical microscopy, revealing an average droplet volume that is 8 % smaller than the droplet volume used as the defined parameter in the QuantaSoft software version 1.3.2.0 (Bio-Rad) to calculate the copy number concentration. This observation explains why copy number concentrations estimated with ddPCR and using an average droplet volume predefined in the QuantaSoft software were systematically lower than those measured by dPCR, creating a significant bias between the values obtained by these two techniques. The difference was not significant anymore when the measured droplet volume of 0.834 nL was used to estimate copy number concentrations. A new version of QuantaSoft software (version 1.6.6.0320), which has since been released with Bio-Rad's new QX200 systems and QX100 upgrades, uses a droplet volume of 0.85 nL as a defined parameter to calculate copy number concentration. PMID:25600685

  13. Development of a certified reference material: ethanol in water - a practical case

    Directory of Open Access Journals (Sweden)

    Vanderléa de Souza

    2006-01-01

    Full Text Available The present work describes the development of a certified reference material (CRM composed of solutions of ethanol in water in five different concentrations, and all stages necessary for the development of an CRM, according to the guidelines of ISO GUIDES 30, 31, 32, 33, 34 and 35. The development of this CRM has been determined by Inmetro Rule n. 006 of 2002, which requires that all breath alcohol analyzers being used in Brazil shall have their respective models approved and that the subsequent verifications shall be performed based on tests with solutions of ethanol in water. As a result, the development of this CRM significantly contributes to the reliability of measurements performed with breath alcohol analyzers, with stated measurement uncertainty. Equally important, this development provides society with a CRM that may have multiple applications, not restricted to the verification of breath alcohol analyzers.O presente trabalho descreve o desenvolvimento de um material de referência certificado (MRC referente a soluções de etanol em água em cinco concentrações diferentes, abordando todas as etapas necessárias para o desenvolvimento de um MRC, conforme prescreve as ISO GUIDE 30, 31, 32, 33, 34 e 35. O desenvolvimento deste MRC originou-se nas determinações da Portaria Inmetro n° 006 de 2002, que assegura que todos os etilômetros a serem utilizados no Brasil deverão ter os seus modelos aprovados, e as verificações realizadas a partir de ensaios com soluções de etanol em água. Após um treinamento, em fevereiro de 2003, no The Federal Institute for Material Research and Testing - BAM, que é um instituto metrológico alemão designado, a Dquim iniciou o processo de desenvolvimento deste MRC, o qual foi concluído em agosto de 2004. No Inmetro desenvolveu-se inicialmente o procedimento de preparo individual, onde as soluções do MRC são preparadas em garrafas de 0,5 L. Atualmente está se estudando, no Inmetro, o

  14. Preparation of zirconium and zirconium-base alloy certified reference materials JAERI-Z11 to -Z18

    International Nuclear Information System (INIS)

    The Second Sub-Committee on Zircaloy Analysis was organized in April, 1978, under the Committee on Analytical Chemistry on Nuclear Fuels and Reactor Materials, JAERI, for the renewal of zirconium and zirconium-base alloy certified reference materials ( CRM's). The Sub-Committee decided certified values of major constituents and impurities in eight reference materials ( JAERI -Z11 to -Z18 ) in July, 1983, based on the results obtained by cooperative analysis during 1978 to 1983. CRM's JAERI-Z11 to -Z14 are Zircaloy-2 in the form of disk, 32 mm in diameter and 20 mm in thickness, and useful primarily for fluorescent X-ray and emission spectrographic analysis. CRMs JAERI-Z15 and -Z16 are zirconium in the form of plate, 30 mm square and 2 mm in the thickness, and specially designed for the analysis of hafnium at trace levels : 2 to 40 μg/g. CRM's JAERI -Z17 and -Z18 are Zircaloy-2 and -4, respectively, in the form of chips, packed in a glass bottle of which content is 25 g and useful for the analysis of carbon in Zircaloy. This report describes mainly preparation of certified reference materials, and homogeneity test by neutron activation analysis and fluorescent X-ray spectrometry. CRMs JAERI-Z11 to -Z14 have been distributed with provisional certificate since July, 1979. (author)

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

    Science.gov (United States)

    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; Gascó, 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; Tarján, 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 (40K, 137Cs, 232Th, 234U, 235U, 238U, 238Pu, 239+240Pu and 241Am) were certified for this material. Information on massic activities with 95% confidence intervals is given for six other radionuclides (90Sr, 210Pb(210Po), 226Ra, 239Pu, 240Pu 241Pu). Less frequently reported radionuclides (99Tc, 129I, 228Th, 230Th and 237Np) 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. PMID:16549351

  16. 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)

    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 (4K, 137Cs, 232Th, 234U, 235U, 238U, 238Pu, 239+24Pu and 241Am) were certified for this material. Information on massic activities with 95% confidence intervals is given for six other radionuclides (9Sr, 21Pb(21Po), 226Ra, 239Pu, 24Pu 241Pu). Less frequently reported radionuclides (99Tc, 129I, 228Th, 23Th and 237Np) 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

  17. 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...

  18. Mineral oil certified reference materials for the determination of polychlorinated biphenyls from the National Metrology Institute of Japan (NMIJ)

    OpenAIRE

    Numata, Masahiko; Aoyagi, Yoshie; Matsuo, Mayumi; Ishikawa, Keiichiro; Hanari, Nobuyasu; Otsuka, Satoko; TSUDA, Yoko; Yarita, Takashi

    2008-01-01

    Four mineral oil certified reference materials (CRMs), NMIJ CRM 7902-a, CRM 7903-a, CRM 7904-a, and CRM 7905-a, have been issued by the National Metrology Institute of Japan, which is part of the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST), for the determination of polychlorinated biphenyls (PCBs). The raw materials for the CRMs were an insulation oil (CRM 7902-a and CRM 7903-a) and a fuel oil (CRM7904-a and CRM 7905-a). A solution of PCB3, PCB8, and technical...

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

    Science.gov (United States)

    Pham, M K; van Beek, P; Carvalho, F P; Chamizo, E; Degering, D; Engeler, C; Gascó, C; Gurriaran, R; Hanley, O; Harms, A V; Herrmann, J; Hult, M; Ikeuchi, Y; Ilchmann, C; Kanisch, G; Kis-Benedek, G; Kloster, M; Laubenstein, M; Llaurado, M; Mas, J L; Nakano, M; Nielsen, S P; Osvath, I; Povinec, P P; Rieth, U; Schikowski, J; Smedley, P A; Suplinska, M; Sýkora, I; Tarjan, S; Varga, B; Vasileva, E; Zalewska, T; Zhou, W

    2016-03-01

    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: (40)K, (210)Pb ((210)Po), (226)Ra, (228)Ra, (228)Th, (232)Th, (234)U, (238)U, (239)Pu, (239+240)Pu and (241)Am for IAEA-410 and (40)K, (137)Cs, (210)Pb ((210)Po), (226)Ra, (228)Ra, (228)Th, (232)Th, (235)U, (238)U, (239)Pu, (240)Pu and (239+240)Pu for IAEA-412. The CRMs can be used for quality assurance and quality control purposes in the analysis of radionuclides in sediments, for development and validation of analytical methods and for staff training. PMID:26631455

  20. Certified reference materials for testing of the presence/absence of Staphylococcus aureus enterotoxin A (SEA) in cheese.

    Science.gov (United States)

    Zeleny, Reinhard; Nia, Yacine; Schimmel, Heinz; Mutel, Isabelle; Hennekinne, Jacques-Antoine; Emteborg, Håkan; Charoud-Got, Jean; Auvray, Frédéric

    2016-08-01

    Staphylococcal enterotoxins (SEs) account for a substantial number of food-poisoning outbreaks. European legislation (Commission Regulation 1441/2007) stipulates the reference procedure for SE analysis in milk and dairy products, which is based on extraction, dialysis concentration and immunochemical detection using one of two approved assays (VIDAS(®) SET2, Ridascreen(®) SET Total). However, certified reference materials (CRMs) are lacking to support laboratories in performing reliable detection of Staphylococcus aureus enterotoxin A (SEA) in relevant matrices at sub-nanogram per gram levels. The certification of a set of three reference materials (blank and two SEA-containing materials) for testing of the presence/absence of SEA in cheese is described. The reference procedure was applied in an intercomparison with 15 laboratories, and results were reported in a qualitative manner (presence or absence of SEA in the sample). No false-negative or false-positive results were obtained. The certified values were stated as diagnostic specificity (blank material) or diagnostic sensitivity (SEA-containing materials) and were 100 % in all cases. Stability studies demonstrated suitable material stability when stored cooled or frozen. An in-house study on the recovery of SEA in the cheese materials using a double-sandwich enzyme-linked immunosorbent assay (ELISA) revealed comparable recovery values of around 45 % at the two spiking levels and in both the SEA-containing CRMs as well as blank CRM freshly spiked prior to analysis. The values were also comparable over time and among different analysts. The materials provide valuable support to laboratories for method validation and method performance verification and will increase the reliability of measuring SEA in cheese. PMID:27220526

  1. Use of INAA in the preparation of a set soil Reference Materials with certified values of total element contents

    International Nuclear Information System (INIS)

    A set of certified Reference Materials was prepared consisting of four natural agricultural soils with normal (n) and elevated (e) levels of element contents: CRM 7001 Light Sandy Soil (n), CRM 7002 Light Sandy Soil (e), CRM 7003 Silty Clay Loam (n), and CRM 7004 Loam (e). In these materials, certified and/or information values of the total contents of the elements As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mn, Ni, Pb, V and Zn, and their fractions extractable by aqua regia, boiling and cold 2M nitric acid were derived from an interlaboratory comparison in which 28 laboratories participated. Highly precise and accurate procedures of instrumental neutron activation analysis (INAA) were employed for homogeneity testing and also for certification of the total element contents. For comparation purposes, NIST SRM-2704 Buffalo River Sediment was analyzed by INAA, as well. The INAA results obtained compared very well with the certified and/or information values for four soil CRMs and also with NIST values for SRM-2704. From this agreement, a very high reliability of the new soil CRMs can be inferred. (author)

  2. Determination of benzo[a]pyrene and dibenzopyrenes in a Chinese coal fly ash certified reference material.

    Science.gov (United States)

    Masala, Silvia; Bergvall, Christoffer; Westerholm, Roger

    2012-08-15

    Air pollution from coal combustion is of great concern in China because coal is the country's principal source of energy and it has been estimated that coal combustion is one of the main sources of polycyclic aromatic hydrocarbon (PAH) emissions in the nation. This study reports the concentrations of 15 PAHs including benzo[a]pyrene, dibenzo[a,l]pyrene, dibenzo[a,e]pyrene, dibenzo[a,i]pyrene and dibenzo[a,h]pyrene in a coal fly ash certified reference material (CRM) from China. To the best of our knowledge, dibenzo[a,l]pyrene, dibenzo[a,i]pyrene and dibenzo[a,h]pyrene concentrations in coal fly ash particles have not previously been reported. Benzo[a]pyrene is the only one of the studied hydrocarbons whose concentration in the coal fly ash CRM had previously been certified. The concentration of this species measured in this present work was twice the certified value. This is probably because of the exhaustive accelerated solvent extraction method employed. Consecutive extractions indicated an extraction recovery in excess of 95% for benzo[a]pyrene. For the other determined PAHs, repeat extractions indicated recoveries above 90%. PMID:22728296

  3. Neutron activation analysis as a tool for checking homogeneity of certified reference materials

    International Nuclear Information System (INIS)

    Homogeneity of reference materials for inorganic trace analysis (Oriental Tobacco Leaves [CTA-OTL-1], Apatite Concentrate [CTA-AC-1], Virginia Tobacco Leaves [CTA-VTL-2] and Spruce Shoots [RMF II]) was studied by neutron activation analysis. Series of samples of a given nominal mass from various containers were analyzed for several elements and the results compared by Fisher''s test with analogous series of results for samples from container. Sampling variance was estimated for several elements in some of the material studied, from overall variance and components of analytical variance. The results were interpreted with the aid of Visman''s theory and Ingamell''s sampling constant. It was confirmed that Virginia Tobacco Leaves [CTA-VTL-2] is very homogeneous and can be recommended for microchemical work. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Pham, M.K. [International Atomic Energy Agency (IAEA), Marine Environment Laboratory (MEL), MC 98000 (Monaco)]. E-mail: m.pham@iaea.org; Sanchez-Cabeza, J.A.; Povinec, P.P.; Gastaud, J.; La Rosa, J.; Lee, S.-H.; Liong Wee Kwong, L.; Oregioni, B.; Wyse, E. [International Atomic Energy Agency (IAEA), Marine Environment Laboratory (MEL), MC 98000 (Monaco); Arnold, D. [Physikalisch-Technische Bundesanstalt, Braunschweig, 38116 Germany (Germany); Benmansour, M. [Centre National de l' Energie, des Sciences et des Techniques Nucleaires (CNESTEN), B.P. 1382, R.P.10001, Rabat (Morocco); Bojanowski, R. [Institute of Oceanology, Polish Academy of Sciences, PL-81-712 Sopot (Poland); Carvalho, F.P. [Instituto Tecnologico e Nuclear, Departamento de Proteccao Radiologica e Seguranca Nuclear, P-2685-953 Sacavem (Portugal); Kim, C.K. [Department of Radiological Environmental Assessment, Korea Institute of Nuclear Safety, Yo-song, Taejon 305-600, Korea (Korea); Esposito, M. [Laboratorio di Ingegneria Nucleare, Universita di Bologna, 40136 Bologna (Italy); Gasco, C.L. [CIEMAT-DIAE, Radioecologia del Medio Acuatico, 28040 Madrid (Spain); Ham, G.J. [National Radiological Protection Board, Chilton, Didcot, Oxon, OX11 0RA (United Kingdom); Hegde, A.G. [Environmental Survey Laboratory, Bhabha Atomic Research Center, Tarapur Atomic Power Station, Maharashtra 401 504 (India); Holm, E. [Department of Medical Radiation Physics, Lund University Hospital, 22185 Lund (Sweden); Jaskierowicz, D. [Lab. d' Analyses de Surveillance et d' Expertise de la Marine, Base Navale de Cherbourg, 50115 Cherbourg (France); Kanisch, G. [Federal Research Centre for Fisheries, Institute of Fisheries Ecology, 20539 Hamburg (Germany); Llaurado, M. [Lab. de Radiologia Ambiental, Dept. de Quimica Analitica, Facultat de Quimica, Universitat de Barcelona, 08028 Barcelona (Spain); Le Petit, G. [Commissariat a l' Energie Atomique, DASE/SRCE, 91680 Bruyeres-le-Chatel (France); Maruo, Y. [and others

    2006-10-15

    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 ({sup 4}K, {sup 137}Cs, {sup 232}Th, {sup 234}U, {sup 235}U, {sup 238}U, {sup 238}Pu, {sup 239+24}Pu and {sup 241}Am) were certified for this material. Information on massic activities with 95% confidence intervals is given for six other radionuclides ({sup 9}Sr, {sup 21}Pb({sup 21}Po), {sup 226}Ra, {sup 239}Pu, {sup 24}Pu {sup 241}Pu). Less frequently reported radionuclides ({sup 99}Tc, {sup 129}I, {sup 228}Th, {sup 23}Th and {sup 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.

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

    International Nuclear Information System (INIS)

    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)

  6. Determination of trace elements in certified river water reference materials by instrumental NAA using a freeze-dried preconcentration

    International Nuclear Information System (INIS)

    Trace elements in JAC 0031 and JAC 0032 certified river water reference materials prepared by the Japan Society for Analytical Chemistry (JAC) were determined by instrumental neutron activation analysis (INAA). A JAC 0031 nonadditional sample (450 ml) and an additional JAC 0032 sample (450 ml) were freeze-dried at -50degC. The dry residues were irradiated for 10 sec at a thermal neutron flux of 1.5x1012 n cm-2s-1 and 6 h at a thermal neutron flux of 3.7x1012 n cm-2s-1 at the Rikkyo University Research Reactor. The irradiated samples were measured by conventional γ-ray spectrometry using a coaxial Ge detector, and by anti-coincidence and coincidence γ-ray spectrometry with a coaxial Ge detector and a well-type NaI(Tl) detector. The concentrations of 27 elements in the JAC 0031 and 29 elements in the JAC 0032 were determined by these methods. The determined values were in good agreement with the certified values of 9-14 elements. (author)

  7. Determination of hexavalent chromium in plastic certified reference materials by X-ray absorption fine structure analysis

    Science.gov (United States)

    Ohata, Masaki; Matsubayashi, Nobuyuki

    X-ray absorption fine structure (XAFS) analysis with transmission mode was used to determine the percentages of hexavalent chromium {Cr(VI)} in total Cr in plastic certified reference materials (CRMs). Cr-K edge X-ray absorption near-edge structure (XANES) spectra were observed and the normalized pre-edge peaks of the spectrum where absorption data was summed was acquired for the determination of Cr(VI). Examination of different number of data point and range of photon energy for summed absorption of the pre-edge peak resulted in reproducible absorption data, though the measurements were carried out at different beam time and beam line. The concentrations of Cr(VI) in the plastic CRMs were also estimated from both the certified value of total Cr and the determined percentage of Cr(VI). The analytical procedure and the estimated concentrations can be useful for the determination of Cr(VI) in plastics with respect to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

  8. Determination of hexavalent chromium in plastic certified reference materials by X-ray absorption fine structure analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ohata, Masaki, E-mail: m-oohata@aist.go.jp [Inorganic Standard Section, Inorganic Analytical Chemistry Division, National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST) (Japan); Matsubayashi, Nobuyuki [Super-Spectroscopy System Research Group, Research Institute of Instrumentation Frontier (RIIF), National Institute of Advanced Industrial Science and Technology (AIST) (Japan)

    2014-03-01

    X-ray absorption fine structure (XAFS) analysis with transmission mode was used to determine the percentages of hexavalent chromium {Cr(VI)} in total Cr in plastic certified reference materials (CRMs). Cr-K edge X-ray absorption near-edge structure (XANES) spectra were observed and the normalized pre-edge peaks of the spectrum where absorption data was summed was acquired for the determination of Cr(VI). Examination of different number of data point and range of photon energy for summed absorption of the pre-edge peak resulted in reproducible absorption data, though the measurements were carried out at different beam time and beam line. The concentrations of Cr(VI) in the plastic CRMs were also estimated from both the certified value of total Cr and the determined percentage of Cr(VI). The analytical procedure and the estimated concentrations can be useful for the determination of Cr(VI) in plastics with respect to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

  9. Evaluation of ABS resin disk certified reference materials for heavy metal analysis by x-ray fluorescence analysis

    International Nuclear Information System (INIS)

    ABS resin disk certified reference materials (CRMs) for heavy-metal analysis (NMIJ CRM 8105-a, NMIJ CRM 8106-a, NMIJ CRM 8115-a and NMIJ CRM 8116-a) were evaluated using an energy dispersive X-ray fluorescence (ED-XRF) analysis. The homogeneities of elements for both among-disks and within-disk were evaluated by ED-XRF analysis without any sample pre-treatment, which were similar to those evaluated by ICP-MS analysis after a sample digenstion procedure. The normalized XRF sensitivities for Cd, Cr and Pb in different ABS resin disk CRMs were compared, and the differences among them for those ABS resin disks that have similar matrices were observed. Moreover, Hg in those ABS resin disk CRMs was stable for long-term X-ray irradiation during ED-XRF analysis. (author)

  10. Laser induced breakdown spectroscopy for fast elemental analysis and sorting of metallic scrap pieces using certified reference materials

    International Nuclear Information System (INIS)

    A setup utilizing laser induced breakdown spectroscopy (LIBS) for performing elemental analysis in order to classify metallic samples is currently under construction. The setup uses short laser pulses to locally ablate the sample and create luminous plasmas. The emitted light is analyzed spectroscopically for instantaneous determination of the elemental composition. A table-top system based on a compact CCD spectrometer has been constructed and combined with fast software in order to test the concept of remote, single shot material classification with LIBS. Certified reference materials with known elemental compositions were used in the laboratory tests. We report on successful laboratory tests in which samples were classified using an analysis based on optical emission following a single laser pulse and with an operating distance of approximately 1 m. Details regarding field tests of this versatile and promising technique are discussed. - Highlights: ► We give a short background to the area of metallic scrap recycling. ► We present the development of an automatic LIBS-based system for material analysis. ► We present experimental data from laboratory results. ► We discuss the possibility of surface cleaning through laser ablation with this setup.

  11. IRMM-1000a and IRMM-1000b. Uranium reference materials certified for the production date based on the 230Th/234U radiochronometer. Part II. Certification

    International Nuclear Information System (INIS)

    The IRMM-1000a and IRMM-1000b uranium reference materials, of 20 and 50 mg uranium, respectively, were produced by the European Commission Joint Research Centre's Institute for Reference Materials and Measurements (EC-JRC-IRMM) in collaboration with the Institute for Transuranium Elements (EC-JRC-ITU). They are novel uranium reference materials certified for the production date based on the 230Th/234U radiochronometer, i.e. the date of the last chemical separation of these two radionuclides. The certified reference value and its uncertainty, homogeneity and stability of the material were established in accordance with the ISO Guide 34:2009 and the 'Guide to the Expression of Uncertainty in Measurement'. (author)

  12. Validation of a liquid chromatographic method for determination of related substances in a candidate certified reference material of captopril

    Directory of Open Access Journals (Sweden)

    Raquel Nogueira

    2011-06-01

    Full Text Available This paper describes the validation of a reversed-phase high performance liquid chromatography method (RP-HPLC with diode array detection (DAD for determination of related substances (impurities from organic synthesis and degradation products of captopril according to the Brazilian Pharmacopeia IV. The aim of this study was to guarantee the method accuracy for quantification of related substances, an essential requisite to determine, using the mass balance approach, the captopril content in the first Brazilian certified reference material (CRM of an active pharmaceutical ingredient (API, developed by Inmetro. The captopril instability in solution is discussed and the captopril content determined by mass balance is compared to the results from titration and differential scanning calorimetry (DSC.Este artigo descreve a validação de método de cromatografia líquida de alta eficiência em fase reversa (CLAE-RP com detector de fotodiodos (DAD para determinação de substâncias relacionadas (impurezas orgânicas de síntese e produtos de degradação de captopril segundo Farmacopéia Brasileira IV ed. Este estudo teve como objetivo garantir que o método é capaz de quantificar com exatidão o teor de substâncias relacionadas, um requisito essencial para que o teor de captopril seja determinado por balanço de massa no primeiro material de referência certificado (MRC de fármacos brasileiro, o qual foi desenvolvido pelo Inmetro. A instabilidade do captopril em solução é discutida em detalhes e o teor de captopril determinado por balanço de massa é comparado com aqueles obtidos por titulação e por calorimetria exploratória diferencial (DSC.

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

    International Nuclear Information System (INIS)

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

  14. Impurity analyses of high-purity carbon monoxide gas using micro gas chromatography for development as a certified reference material.

    Science.gov (United States)

    Matsumoto, Nobuhiro; Watanabe, Takuro; Kato, Kenji

    2013-03-22

    High-purity carbon monoxide (CO) gas as a certified reference material (CRM) was analyzed using a micro gas chromatograph (micro-GC) with a micro thermal conductivity detector. The main reason to select the micro-GC was its compact size to provide a safe experimental environment. Thus, both the CO gas cylinder and the micro-GC were placed inside a draft shield with a limited small space. Peaks of several impurities were found in chromatograms of the micro-GC. The main impurities in the CO gas were helium, hydrogen, oxygen, nitrogen and carbon dioxide. It was found that helium was the impurity of the highest concentration. High-accuracy calibration gas mixtures were used to construct calibration lines for the micro-GC. The mixtures were precisely prepared by the gravimetric blending method. Calibration lines had enough linearity and accuracy for quantitative analyses of the impurities. The values of detection limit of the impurities were 0.7-4μmol/mol. The purity of the high-purity CO gas was around 99.996%, which was the value estimated from the sum of the concentrations of the impurities. PMID:23415447

  15. k0-INAA for APM samples collected in period of June 2004 - March 2005 and some marine certified reference materials

    International Nuclear Information System (INIS)

    The airborne particulate matter (APM) samples have been collected in 2004 using two types of polycarbonate membrane filter PM2.5 and PM2.5-10 at two sites of industrial (Ho Chi Mihn City) and rural (Dateh) regions in south of Vietnam. Three marine certified reference materials have been selected to establish a k0-NAA procedure for marine samples. The concentration of trace multi-element in the samples has been determined by the k0-INAA procedure using Ko-DALAT software developed in Dalat NRI. About 28 elements in 224 APM samples collected at two areas of Dateh and HCMC of Vietnam in period from June, 2004 to March, 2005 were presented in report. The statistical analysis was applied to the data set to investigate the pollution source at sampling sites. The results proved that the k0-NAA on the Dalat research reactor is a reliable and effective analytical technique for characterization of trace multi-element in APM and marine samples for air and marine environmental pollution study in Vietnam. (author)

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

    International Nuclear Information System (INIS)

    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

  17. Determination of reference values of element contents in certified reference material SWCNT-1 by INAA a PGAA

    Czech Academy of Sciences Publication Activity Database

    Kučera, Jan; Sturgeon, R. E.; Grinberg, P.; Oflaz, R.; Paul, R. L.; Bennett, J. W.; De Nadai Fernandes, E. A.; Kubešová, Marie; Bacchi, M. A.; Stopic, A. J.

    Vol. 5. Český Těšín: 2 THETA, 2014 - (Helán, V.), s. 35-41 ISBN 978-80-86380-73-5. [Referenční materiály a mezilaboratorní porovnání zkoušek V. Valtice (CZ), 05.11.2014-07.11.2014] R&D Projects: GA ČR(CZ) GBP108/12/G108; GA MŠk LM2011019 Institutional support: RVO:61389005 Keywords : carbon nanotubes * neutron activation analysis Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders

  18. IRMM-1000a and IRMM-1000b: uranium reference materials certified for the production date based on the 230Th/234U radiochronometer Part II: Certification

    OpenAIRE

    VENCHIARUTTI CELIA; VARGA ZSOLT; Richter, Stephan; Nicholl, Adrian; KRAJKO JUDIT; JAKOPIC Rozle; Mayer, Klaus; AREGBE Yetunde

    2015-01-01

    The IRMM-1000a and IRMM-1000b uranium reference materials, of 20 mg uranium and 50 mg uranium, respectively, were produced by the European Commission Joint Research Centre’s Institute for Reference Materials and Measurements (EC-JRC-IRMM) in collaboration with the Institute for Transuranium Elements (EC-JRC-ITU). They are the first uranium reference materials certified for the production date based on the 230Th/234U radiochronometer, i.e. the date of the last chemical separation of these two ...

  19. Certified reference material for quantification of polycyclic aromatic hydrocarbons and toxic elements in tunnel dust (NMIJ CRM 7308-a) from the National Metrology Institute of Japan

    Energy Technology Data Exchange (ETDEWEB)

    Itoh, Nobuyasu; Inagaki, Kazumi; Narukawa, Tomohiro; Aoyagi, Yoshie; Narushima, Izumi; Koguchi, Masae; Numata, Masahiko [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba, Ibaraki (Japan)

    2011-11-15

    The National Metrology Institute of Japan has issued a certified reference material of tunnel dust for polycyclic aromatic hydrocarbons (PAHs) and toxic element analyses. PAH certification was performed using isotope dilution mass spectrometry with deuterium-labeled PAHs as internal standards. Three extraction techniques (microwave-assisted extraction with toluene/methanol, Soxhlet extraction with toluene, and pressurized liquid extraction with toluene) were used, and the extracts were measured by gas chromatography/mass spectrometry with two different columns. For values of PAHs, 11 PAHs are provided as certified values between 0.294 and 20.3 mg/kg, and five PAHs are provided as information values. Certified values of five toxic elements (Cr, Ni, Pb, Mn, and Cd) obtained from microwave-assisted digestions and a combination of measurement techniques are also provided between 43.4 and 10.71 x 10{sup 3} mg/kg. (orig.)

  20. Certified reference material for quantification of polycyclic aromatic hydrocarbons and toxic elements in tunnel dust (NMIJ CRM 7308-a) from the National Metrology Institute of Japan

    International Nuclear Information System (INIS)

    The National Metrology Institute of Japan has issued a certified reference material of tunnel dust for polycyclic aromatic hydrocarbons (PAHs) and toxic element analyses. PAH certification was performed using isotope dilution mass spectrometry with deuterium-labeled PAHs as internal standards. Three extraction techniques (microwave-assisted extraction with toluene/methanol, Soxhlet extraction with toluene, and pressurized liquid extraction with toluene) were used, and the extracts were measured by gas chromatography/mass spectrometry with two different columns. For values of PAHs, 11 PAHs are provided as certified values between 0.294 and 20.3 mg/kg, and five PAHs are provided as information values. Certified values of five toxic elements (Cr, Ni, Pb, Mn, and Cd) obtained from microwave-assisted digestions and a combination of measurement techniques are also provided between 43.4 and 10.71 x 103 mg/kg. (orig.)

  1. Preparation and certification of certified reference materials JAERI-Z21, Z22 and Z23 for analysis of zirconium and its alloys

    International Nuclear Information System (INIS)

    The Sub-Committee on Chemical Analysis of Nuclear Materials was organized in April 1987, under the Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI, for renewal of certified reference materials of zirconium base alloys and zirconium metal. Collaborative analysis was carried out among ten participating laboratories for the certification of the JAERI CRMs Z21 to Z23. As a results of the collaborative works, the certified values for sixteen elements (Sn, Fe, Ni, Cr, Hf, Al, Si, Co, Cu, Ti, Mn, Pb, U, Cd, B and W) in the CRMs were given. In this report, preparation of raw materials, homogeneity test, chemical analysis for certification by collaborative works during April 1987 to March 1990 are described. (author)

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

    International Nuclear Information System (INIS)

    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. Electrothermal atomic absorption spectrometric determination of vanadium in extracts of soil and sewage sludge certified reference materials after fractionation by means of the Communities Bureau of Reference modified sequential extraction procedure

    International Nuclear Information System (INIS)

    A modified three-step sequential extraction procedure proposed by the Commission of European Communities Bureau of Reference (BCR) was applied to certified reference materials of three different soil groups (rendzina, luvisol, cambisol) and sewage sludge of different composition originating from a municipal water treatment plant in order to assess potential mobility and the distribution of vanadium in the resulting fractions. Analysis of the extracts was carried out by electrothermal atomic absorption spectrometry with Zeeman background correction using transversely heated graphite atomizers. Extracts showed significant matrix interferences which were overcome by the standard addition technique. The original soil and sludge certified reference materials (CRMs) and the extraction residue from the sequential extraction were decomposed by a mixture of HNO3-HClO4-HF in an open system. The content of V determined after decomposition of the samples was in very good agreement with the certified total values. The accuracy of the sequential extraction procedure was checked by comparing the sum of the vanadium contents in the three fractions and in the extraction residue with the certified total content of V. The amounts of vanadium leached were in good correlation with the certified total contents of V in the CRMs of soils and sewage sludge. In the soils examined, vanadium was present almost entirely in the mineral lattice, while in the sewage sludge samples 9-14% was found in the oxidizable and almost 25% in the reducible fractions. The recovery ranged from 93-106% and the precision (RSD) was below 10%

  4. A certified plasmid reference material for the standardisation of BCR-ABL1 mRNA quantification by real-time quantitative PCR

    OpenAIRE

    White, Helen; DEPREZ LIESBET; Corbisier, Philippe; HALL Victoria; Lin, Feng; Mazoua, Stephane; TRAPMANN Stefanie; AGGERHOLM Annie; Andrikovics, Hajnalka; AKIKI Susanna; Barbany, Gisela; Boeckx, Nancy; Bench, Anthony; CATHERWOOD Mark; Cayuela, Jean-Michel

    2014-01-01

    Serial quantification of BCR-ABL1 mRNA is an important therapeutic indicator in chronic myeloid leukaemia, but there is a substantial variation in results reported by different laboratories. To improve comparability, an internationally accepted plasmid certified reference material (CRM) was developed according to ISO Guide 34:2009. Fragments of BCR-ABL1 (e14a2 mRNA fusion), BCR and GUSB transcripts were amplified and cloned into pUC18 to yield plasmid pIRMM0099. Six different linearised plasm...

  5. The validation of Kayzero-assisted NAA in Budapest, Rez, and Ljubljana via the analysis of three BCR certified reference materials.

    Science.gov (United States)

    De Corte, F; van Sluijs, R; Simonits, A; Kucera, J; Smodis, B; Byrne, A R; De Wispelaere, A; Bossus, D; Frána, J; Horák, Z; Jaćimović, R

    2001-05-01

    After installation and calibration of k0-assisted NAA in three Central European research institutes (AEKI-Budapest, NPI-Rez, and IJS, Ljubljana), its validation was established via the analysis of three BCR certified reference materials. The matrices of choice were: CRM 277 estuarine sediment, CRM 038 coal fly ash from pulverized coal, and CRM 101 spruce needles. For some elements, e.g. Zn, Cd, and Hg, the analyses were not only performed instrumentally (INAA), but also in the radiochemical mode (RNAA). The work was performed in the framework of a European Copernicus Project. PMID:11393234

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

    OpenAIRE

    Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi

    2006-01-01

    A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with γ-ray irradiation. The material was re-mixed and packaged into 250 gla...

  7. New Polish Certified Reference Materials for inorganic trace analysis: corn flour (INCT-CF-3) and soya bean flour (INCT-SBF-4)

    International Nuclear Information System (INIS)

    Preparation and certification of two new Polish reference materials (CRMs) for inorganic trace analysis: Corn Flour (INCT-CF-3) and Soya Bean Flour (INCT-SBF-4) have been presented. The materials were prepared and certified in the Institute of Nuclear Chemistry and Technology, Warsaw (INCT). Instrumental neutron activation analysis (INAA) was applied to homogeneity and stability studies. Homogeneity tests have shown that both materials are homogeneous for the sample mass 3 100 mg. The results of trend analysis have shown that the materials are stable. Uncertainty caused by instability and, consequently, shelf life of the materials have been estimated. Certification was based on the statistical evaluation of results obtained in worldwide interlaboratory comparison, in which 92 laboratories from 19 countries participated. Results for CRM distributed by the organizer and analyzed together with the intercomparison samples as well as results by definitive methods for selected elements based on radiochemical neutron activation analysis (RNAA) were also employed in the certification process. The contents of 16 and 22 elements were certified in Corn Flour and Soya Bean Flour, respectively. Additional information values for 14 elements in INCT-CF-3 and 9 elements in INCT-SBF-4 were given. (authors)

  8. Production and certification of an equal atom plutonium isotopic standard - the New Brunswick Laboratory certified reference material (CRM) No. 128

    International Nuclear Information System (INIS)

    The US Department of Energy (DOE), New Brunswick Laboratory (NBL) has produced an equal atom 239Pu/242Pu isotopic standard, NBL CRM No. 128. Provisional certification of this standard relative to uranium was completed in 1984 and the material made available for distribution to the nuclear community. Certification of the 239Pu/242Pu ratio on an absolute basis has now been accomplished using highly accurate and precise chemical and mass spectrometric measurement techniques. The absolute certification of NBL CRM No. 128 has established it as the primary reference for calibrating the measurement of plutonium isotopic ratios

  9. Comparative study of optimised BCR sequential extraction scheme and acid leaching of elements in the certified reference material NIST 2711

    International Nuclear Information System (INIS)

    The optimised BCR sequential extraction procedure and a 4 h 1 mol L-1 HCl partial extraction have been performed on the NIST 2711 reference material for a suite of 12 elements (Cd, Sb, Pb, Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, As) using magnetic sector ICP-MS. A pseudo-total aqua regia digest of NIST 2711 has also been undertaken for quality assurance purposes, and comparison of the sum of the four BCR fractions, which included an aqua regia digest on the residue, with the pseudo-total aqua regia digest has been used to assess the accuracy of the BCR partitioning approach. As a result of this work, discrepancies between previous studies about BCR partitioning of elements in NIST 2711 have been discussed and an increase in confidence about the use of BCR partitioning scheme on seven elements (Cd, Pb, Al, Mn, Fe, Cu, Zn) in this standard material has been obtained. On the other hand, BCR partitioning for Sb, Cr, Co, Ni and As has been provided for the first time. Partial extraction results are also reported for the same 12 elements analysed by the optimised BCR procedure, with the partial extraction results exhibiting a strong correlation with the sum of the three labile steps of the BCR procedure

  10. Quantitative Analysis of Plutonium Content in Particles Collected from a Certified Reference Material by Total Nuclear Reaction Energy (Q Value) Spectroscopy

    Science.gov (United States)

    Croce, M. P.; Hoover, A. S.; Rabin, M. W.; Bond, E. M.; Wolfsberg, L. E.; Schmidt, D. R.; Ullom, J. N.

    2016-08-01

    Microcalorimeters with embedded radioisotopes are an emerging category of sensor with advantages over existing methods for isotopic analysis of trace-level nuclear materials. For each nuclear decay, the energy of all decay products captured by the absorber (alpha particles, gamma rays, X-rays, electrons, daughter nuclei, etc.) is measured in one pulse. For alpha-decaying isotopes, this gives a measurement of the total nuclear reaction energy (Q value) and the spectra consist of well-separated, narrow peaks. We have demonstrated a simple mechanical alloying process to create an absorber structure consisting of a gold matrix with small inclusions of a radioactive sample. This absorber structure provides an optimized energy thermalization environment, resulting in high-resolution spectra with minimal tailing. We have applied this process to the analysis of particles collected from the surface of a plutonium metal certified reference material (CRM-126A from New Brunswick Laboratory) and demonstrated isotopic analysis by microcalorimeter Q value spectroscopy. Energy resolution from the Gaussian component of a Bortels function fit was 1.3 keV FWHM at 5244 keV. The collected particles were integrated directly into the detector absorber without any chemical processing. The ^{238}Pu/^{239}Pu and ^{240}Pu/^{239}Pu mass ratios were measured and the results confirmed against the certificate of analysis for the reference material. We also demonstrated inter-element analysis capability by measuring the ^{241}Am/^{239}Pu mass ratio.

  11. Quantitative Analysis of Plutonium Content in Particles Collected from a Certified Reference Material by Total Nuclear Reaction Energy (Q Value) Spectroscopy

    Science.gov (United States)

    Croce, M. P.; Hoover, A. S.; Rabin, M. W.; Bond, E. M.; Wolfsberg, L. E.; Schmidt, D. R.; Ullom, J. N.

    2016-03-01

    Microcalorimeters with embedded radioisotopes are an emerging category of sensor with advantages over existing methods for isotopic analysis of trace-level nuclear materials. For each nuclear decay, the energy of all decay products captured by the absorber (alpha particles, gamma rays, X-rays, electrons, daughter nuclei, etc.) is measured in one pulse. For alpha-decaying isotopes, this gives a measurement of the total nuclear reaction energy (Q value) and the spectra consist of well-separated, narrow peaks. We have demonstrated a simple mechanical alloying process to create an absorber structure consisting of a gold matrix with small inclusions of a radioactive sample. This absorber structure provides an optimized energy thermalization environment, resulting in high-resolution spectra with minimal tailing. We have applied this process to the analysis of particles collected from the surface of a plutonium metal certified reference material (CRM-126A from New Brunswick Laboratory) and demonstrated isotopic analysis by microcalorimeter Q value spectroscopy. Energy resolution from the Gaussian component of a Bortels function fit was 1.3 keV FWHM at 5244 keV. The collected particles were integrated directly into the detector absorber without any chemical processing. The ^{238} Pu/^{239} Pu and ^{240} Pu/^{239} Pu mass ratios were measured and the results confirmed against the certificate of analysis for the reference material. We also demonstrated inter-element analysis capability by measuring the ^{241} Am/^{239} Pu mass ratio.

  12. Development of a Certified Reference Material for Lyophilized Vitamin K 1%维生素 K1冻干标准物质的研制

    Institute of Scientific and Technical Information of China (English)

    张晓光; 黄挺; 张伟; 黄亮; 全灿; 李红梅; 杨屹

    2015-01-01

    采用二甲基亚砜(DMSO)作为冻干标准物质的溶剂,以重量法准确配制维生素 K1/ DMSO 溶液,再进行分装、冷冻干燥,经定性分析、定值分析、均匀性检验、稳定性考察和不确定度评定,研制了维生素 K1冻干标准物质。以维生素 K1纯度标准物质溶液为校准品,对得到的冻干物质进行了高效液相色谱法定值分析,冻干标准物质的准确定值结果为0.96 mg/ mL,相对扩展不确定度为7%。建立的维生素 K1冻干标准物质研制方法,对于临床检验中维生素 K1的准确测定和相关疾病的正确诊断治疗以及维生素 K1长期保存具有重要意义。%Dimethyl sulfone( DMSO)is firstly applied as the solvent for a lyophilized certified reference material (CRM). Vitamin K1 / DMSO solution is prepared by gravimetry,and is sub-divided and lyophilized,the lyophilized vitamin K1 CRM is developed through qualitative analysis,quantitative analysis,homogeneity study,stability study and uncertainty evaluation. Certified value of lyophilization vitamin K1 is analyzed by high performance liquid chromatography method, using the vitamin K1 purity CRM as a calibrant. The certified value is 0. 96 mg/ mL,with the relative expanded uncertainty of 7% . The method of CRM lyophilized vitamin K1 makes great significance for the accurate determination the disease in clinical examination and the long-term preservation of vitamin K1 .

  13. Characterization and Uncertainty Assessment of a Certified Reference Material of Chloramphenicol in Methanol (GBW(E)082557)

    Science.gov (United States)

    Zhou, Jian; Song, Yinqing; Wang, Tongtong

    2016-01-01

    Prior to preparation of CRM candidate of chloramphenicol in methanol with a concentration of 100 mg/L, two independent methods including mass balance (MB) and quantitative nuclear magnetic resonance (qNMR) were employed to precisely measure the mass fraction of pure chloramphenicol materials. The mass fraction was assigned to be 99.8% with uncertainty of 0.3%. Homogeneity testing and stability study of chloramphenicol in methanol were examined by using high performance liquid chromatography. Additionally, the uncertainties originating from the process of CRM development were comprehensively evaluated. The experimental results indicate that the property value of this CRM is homogeneous and stable at 4°C for at least six months. The new CRM (GBW(E)082557) can be applicable to calibration of instrument and assurance of accuracy and comparability of results in routine measurement. PMID:27493666

  14. Characterization and Uncertainty Assessment of a Certified Reference Material of Chloramphenicol in Methanol (GBW(E)082557).

    Science.gov (United States)

    Yang, Mengrui; Wang, Min; Zhou, Jian; Song, Yinqing; Wang, Tongtong

    2016-01-01

    Prior to preparation of CRM candidate of chloramphenicol in methanol with a concentration of 100 mg/L, two independent methods including mass balance (MB) and quantitative nuclear magnetic resonance (qNMR) were employed to precisely measure the mass fraction of pure chloramphenicol materials. The mass fraction was assigned to be 99.8% with uncertainty of 0.3%. Homogeneity testing and stability study of chloramphenicol in methanol were examined by using high performance liquid chromatography. Additionally, the uncertainties originating from the process of CRM development were comprehensively evaluated. The experimental results indicate that the property value of this CRM is homogeneous and stable at 4°C for at least six months. The new CRM (GBW(E)082557) can be applicable to calibration of instrument and assurance of accuracy and comparability of results in routine measurement. PMID:27493666

  15. Determining sample alignment in x-ray reflectometry using thickness and density from GaAs/AlAs multilayer certified reference materials

    International Nuclear Information System (INIS)

    X-ray reflectometry (XRR) provides researchers and manufacturers with a non-destructive way to determine thickness, roughness and density of thin films deposited on smooth substrates. Due to the nested nature of equations modeling this phenomenon, the inter-relation between instrument alignment and parameter estimation accuracy is somewhat opaque. In this study, we intentionally shift incident angle information from a high-quality XRR data set and refine a series of shifted data sets using an identical structural model to assess the effect this angle misalignment has on parameter estimation. We develop a series of calibration curves relating angle misalignment to variation in layer thickness and density for a multilayer GaAs/AlAs Certified Reference Material on a GaAs substrate. We then test the validity and robustness of several approaches of using known thickness and density parameters from this structure to calibrate instrument alignment. We find the highest sensitivity to and linearity with, measurement misalignment from buried AlAs and GaAs layers, in contrast to the surface layers, which show the most variability. This is a fortuitous result, as buried AlAs and GaAs exhibit the highest long-term stability in thickness. Therefore, it is indeed possible to use reference thickness estimates to validate XRR angle alignment accuracy. Buried layer mass density information also shows promise as a robust calibration approach. This is surprising, as electron density of buried layers is both a highly-correlated phenomenon and a subtle component within the XRR model. (paper)

  16. Certification of the Deuterium-to-Hydrogen (D/H) amount-of-substance ratio in a 1,1,3,3 - tetramethylurea batch: Certified Reference Material STA-003m

    OpenAIRE

    Zeleny, Reinhard

    2013-01-01

    This report describes the production of a tetramethylurea (TMU) reference material (STA-003m), certified for its deuterium-to-hydrogen (D/H) amount-of-substance ratio. The material is to be used as an internal standard in site-specific natural isotope fractionation – nuclear magnetic resonance (SNIF-NMR) spectrometry measurements for determining the D/H amount-of-substance ratios of ethanol distilled from wines, an important measure in wine authenticity testing (Commission Regulation 2676/90)...

  17. 法医DNA标准物质STR位点等位基因分型定值研究%Certified value study for alleles on STR loci of forensic DNA reference materials

    Institute of Scientific and Technical Information of China (English)

    赵兴春; 孙敬; 印佳; 王燕; 姜伯玮; 高运华; 叶健

    2012-01-01

    为探讨法医DNA标准物质STR位点等位基因分型的定值和溯源,利用有机法提取法医DNA标准物质备选所用细胞基因组DNA,以其为模板进行STR复合扩增,制备获得等位基因分型片段并测序分析,成功获得法医DNA标准物质备选所用细胞STR位点等位基因分型的定值.对STR位点等位基因分型进行定值研究可以作为法医DNA标准物质溯源研究的有效途径之一.%In order to develop the certified value and traceability for the alleles on STR loci of forensic DNA reference materials, the genomic DNA of the cells was extracted and amplified for preparing the forensic DNA reference materials. Then the allelic DNA was prepared, sequenced and valuated. Finally the value for the alleles on STR loci of the cells was certified. The certified value for the alleles on STR loci can work as an effective approach for the traceability of forensic DNA reference materials.

  18. 冻干人尿中汞成分分析标准物质的研制%Development of the certified reference material of mercury in lyophilized human urine

    Institute of Scientific and Technical Information of China (English)

    赵玮; 张福钢; 李春伶; 杜会芳; 潘亚娟; 张敬; 闫慧芳

    2011-01-01

    Objective To develop the certified reference material of mercury in lyophilized human urine. Methods Human urine samples from normal level mercury districts were filtered, homogenized,dispensed, lyophilized and radio-sterilized. Homogeneity test, stability inspection and certification were conducted using a atom fluorescence spectrophotometric method. The physical and chemical stability of the certified reference material were assessed for 18 months. The certified values are based on analysis made by three independent laboratories. Results The certified values are as follows: low level was (35.6±2.1)μg/L,high level was (50.5±3.0) μg/l. Conclusion The certified reference material of mercury in lyophilized human urine in this research reached the national certified reference material requirements and could be used for the quality control.%目的 研制冻干人尿中汞成分分析标准物质.方法 冻干尿由正常人尿经过滤、加标、混匀、分装、冷冻干燥、辐射灭菌制备而成,使用原子荧光测定方法 对其均匀性和稳定性进行检验,由3家实验室用准确可靠的方法 确定标准值,并对尿中汞研制物的不确定度进行分析.结果 本研制物均匀性良好,-20 ℃保存可稳定18个月,2个水平的量值及不确定度分别为(35.6±2.1)和(50.5±3.0)μg/L.结论 尿中汞成分分析标准物质各项指标符合的要求,可用于实验室检测的质量控制.

  19. Development of a certified reference material for calibration of DSC and DTA below room temperature: NMIJ CRM 5401-a, Cyclohexane for Thermal Analysis

    International Nuclear Information System (INIS)

    Highlights: • We developed a new CRM for quality assurance of DSC and DTA below room temperature. • Certified values are temperatures and enthalpies of two phase transitions. • Certified values agree with literature values. • Certified values are determined by adiabatic calorimetry and traceable to the SI. • Purity of this CRM was confirmed more than 0.9999. - Abstract: For the quality assurance of performance of differential scanning calorimeters (DSC) and differential thermal analyzers (DTA) below room temperature, we have developed “NMIJ CRM 5401-a, Cyclohexane for Thermal Analysis” applicable to calibration of DSC and DTA in the low temperature. Adiabatic calorimetry was used to measure the temperatures and enthalpies of solid–solid phase transition and fusion as certified values, and to determine the purity in amount of substance fraction as information. The certified values are consistent with their corresponding literature values within expanded uncertainties and have traceability to the SI. Purity in amount of substance fraction was measured by fractional melting method based on freezing point depression method and was confirmed to be more than 0.9999. NMIJ CRM 5401-a was produced based on a quality system in compliance with ISO Guide 34: 2000. We demonstrate the usefulness of NMIJ CRM 5401-a in the calibration, quality control, and validation aspects of DSC and DTA

  20. Preparation of the new certified reference material Virginia Tobacco Leaves (CTA-VTL-2) and development of suitable methods for checking the homogeneity

    International Nuclear Information System (INIS)

    The aim of this project in the long run has been reparation of a new biological reference material: Tobacco leaves of the 'Virginia' type and its certification for the content of possibly great number of trace elements. Further aims have been: development of the suitable methods for checking the homogeneity with the special emphasis on homogeneity of small samples and the critical analysis of the performance of various analytical techniques

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

    Science.gov (United States)

    Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi

    2007-04-01

    A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with gamma-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 degrees C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS)-SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with 118Sn-enriched organotin compounds synthesized from 118Sn-enriched metal used as a spike. The 118Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the 118Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44+/-3 microg kg(-1) as Sn, DBT 51 +/- 2 microg kg(-1) as Sn, MBT 67 +/- 3 microg kg(-1) as Sn, TPhT 6.9 +/- 1.2 microg kg(-1) as Sn, and DPhT 3.4 +/- 1.2 microg kg(-1) as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds. PMID:16874473

  2. Development of Certified Reference Material of Wheat Powder for Analysis of Nutritional Ingredients%小麦粉营养成分分析标准物质的研制

    Institute of Scientific and Technical Information of China (English)

    蒋子刚; 应劼; 顾金炎; 张保国; 张伟萍; 陆慧

    2000-01-01

    A certified reference material of wheat powder for the analysis of twenty nutritional ingredients was prepared by means of peeling, crushing and sifting the wheat seed ″ Yang Mai No 1″, cultivated by Crop Institute of Shanghai Academy of Agricultural Science. The stabile period of the certified reference material is more than seven years after it was irradiated by 60Co γ _ ray. Its homogeneity is good according to F _ test and t _ test. The twenty nutritional ingredients include crude protein, crude starch, crude fat, total amino acid, and individual amino acid: aspartic acid, threonine, serine, glutamic acid, proline, glycine, alanine, valine, methionine, isoleucine, leucine, tyrosine, phenylalanine, lysine, histidine and arginine. Its stability, homogeneity and uncertainty of definite values for the nutritional ingredients fit the technological requirements of certified reference material. Its qualification of GBW has been approved.%进行了小麦粉营养成分分析标准物质的研制。选用上海农业科学院作物研究所培育的“杨麦一号”小麦种子经脱壳、粉碎、过筛,用60Co γ射线照射使其贮存稳定期达7年以上;用数理统计F检验法和t检验法检验证明其均匀性良好;由9个单位共同协作定值,共定值137组, 548个数据,经统计检验,小麦粉中粗蛋白质、粗淀粉、粗脂肪、氨基酸总量、天门冬氨酸、苏氨酸、丝氨酸、谷氨酸、脯氨酸、甘氨酸、丙氨酸、缬氨酸、蛋氨酸、异亮氨酸、亮氨酸、酪氨酸、苯丙氨酸、赖氨酸、组氨酸、精氨酸共20个营养成分定为标准值。所研制的标准物质其稳定性、均匀性及营养成分定值的不确定度均符合国家级标准物质技术指标,已被批准为国家级标准物质。

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-04-15

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

  4. Preparation of the Certified Reference Material of Potassium Permanganate Solution%高锰酸钾溶液标准物质的研制

    Institute of Scientific and Technical Information of China (English)

    梁秀丽; 张坤; 王爱萍; 李本涛; 王学琴; 姚旭霞; 刘立君

    2013-01-01

    Preparation process of potassium permanganate solution standard material was introduced. Weighing titrimetric method was used for certification. The homogeneity and stability of potassium permanganate solution standard material were examined. The results indicated that the standard material was homogeneous and the value stated was valid for a period of 6 month. The stated value of it was c( 1 / 5 KMnO4)=0.100 7 mol / kg(k=2). The standard material meets the requirements of the secondary level of standard material and it has been authorized for the state-level standard material.%介绍高猛酸钾溶液标准物质的研制过程.对研制的溶液标准物质进行了均匀性和稳定性考察.结果表明,该标准物质均匀性良好,定值稳定期为6个月.用称量滴定法定值,定值结果为c(1/5KMnO4)=0.1007 mol/kg(k=2).该标准溶液满足二级标准物质的技术要求,已被批准为国家级二级标准物质.

  5. Preparação de um material de referência certificado para controle de agrotóxicos em hortifrutigranjeiros: estudo da homogeneidade Preparation of a certified reference material for pesticide control in the cultivation of fruits and vegetables: a homogeneity study

    Directory of Open Access Journals (Sweden)

    Maria Helena Wohlers Morelli Cardoso

    2010-06-01

    Full Text Available Neste trabalho são apresentados os esforços para garantir a homogeneidade de um material de referência. Níveis residuais (mg.kg-1 de quatro agrotóxicos (γ-HCH, fenitrotiona, clorpirifós e procimidona foram adicionados à polpa de tomate com o objetivo de se preparar um material de referência certificado. As propriedades mais importantes desses materiais são a homogeneidade e a estabilidade. Antes de serem enviados a outros laboratórios, os materiais de referência precisam ter sua homogeneidade verificada. Nas etapas prévias, amostras foram avaliadas de modo a prover dados sobre o tratamento mais adequado para minimizar a variabilidade analítica do lote preparado e garantir a qualidade da amostra candidata a material de referência certificado, tão bem como a estimativa da incerteza associada à homogeneidade. A análise de variância fornece informações sobre a variabilidade do lote preparado e o grau de invariabilidade da amostra fortificada. Depois da preparação, as amostras foram expostas à radiação gama na dose de 2 kGy e submetidas a um estudo interlaboratorial para certificação. As concentrações certificadas dos agrotóxicos após caracterização foram 0,191 ± 0,047 mg.kg-1; 0,192 ± 0,068 mg.kg-1; 0,225 ± 0,076 mg.kg-1e 0,177 ± 0,051 mg.kg-1 para o γ-HCH, a fenitrotiona, clorpirifós e procimidona respectivamente.This study reports on the efforts to ensure homogeneity of certified reference materials. Residues of four pesticides (γ-HCH, fenitrothion, chlorpyrifos, and procymidone were added to tomato pulp in order to produce reference materials. The two most important properties of such materials are known to be homogeneity and stability. Before being shipped to other laboratories, reference materials must have their homogeneity certified. As part of a preliminary study, hundreds of samples were investigated in order to provide data on the most suitable treatments to minimize analytical variability and

  6. Effect of long-time X-ray irradiation on Cr and Hg in a polypropylene disk certified reference material observed during measurements by X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    The effect of long-time X-ray irradiation on Cr and Hg in a polypropylene disk certified reference material (PP disk CRM, NMIJ CRM 8136-a) during measurements by X-ray fluorescence (XRF) spectrometry was examined in the present study. The XRF intensities of Cr (Kα), Hg (Lα) and Pb (Lα), obtained by an energy-dispersive (ED)-XRF spectrometer, showed the different intensity trends and the obtained XRF intensity ratios of Cr/Pb and Hg/Pb revealed decreasing and constant ratios, respectively, for long-time X-ray irradiation of up to 430 h. A similar decreasing trend of the Cr/Pb intensity ratio was also observed by wavelength-dispersive (WD)-XRF measurements for 120 h. Moreover, Cr, Hg and Pb in the PP disks obtained after long-time measurements by the WD-XRF spectrometer were measured by an ED-XRF spectrometer, and the loss of Cr was confirmed. From these results, Cr in the PP disk CRM, whose chemical form was an organometallic compound, was considered to be possibly lost during the XRF analysis for long-time or frequent measurements. (author)

  7. Stability evaluation and chemical characterization of different vegetable oils viewing the search for candidates for certified reference materials for bio diesel; Avaliacao da estabilidade e caracterizacao quimica de diferentes oleos vegetais visando a busca de candidatos a materiais de referencia certificado (MRC) para biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Cruz, Georgiana F. da; Fonseca, Mauricio G.; Goncalves, Lenise V.F.; Silva, Regina Celia F. da; Silva, Fernanda M.R. da; Rodrigues, Janaina M. [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (LABOR/INMETRO), Duque de Caxias, RJ (Brazil). Lab. de Analises Organicas; Leal, Rodrigo V.P. [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (LAMBOC/INMETRO), Duque de Caxias, RJ (Brazil). Lab. de Motores, Combustiveis e Lubrificantes], Email: rvleal@inmetro.gov.br; Cunha, Valnei S. [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (DIMCI/INMETRO), Duque de Caxias, RJ (Brazil). Diretoria de Metrologia Cientifica e Industrial

    2009-07-01

    Viewing the characterization of the various vegetable oils aiming to obtain a data bank that allows the production of certified reference materials for bio diesel of different blends, a study of chemical-physical characterization of different oils and derivative of bio diesel.

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

    International Nuclear Information System (INIS)

    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. Characterization of the NIST seaweed Standard Reference Material

    DEFF Research Database (Denmark)

    Outola, I.; Filliben, J.; Inn, K.g.W.; Rosa, J. La; McMahon, C.A.; Peck, G.A.; Twining, J.; Tims, S.G.; Fifield, L.K.; Smedley, P.; Antón, M.P.; Gascó, C.; Povinec, P.; Pham, M.K.; Raaum, A.; Wei, H.-J.; Krijger, G.C.; Bouisset, P.; Litherland, A.E.; Kieser, W.E.; Betti, M.; Heras, L. Aldave de las; Hong, G.H.; Holm, E.; Skipperud, L.; Harms, A.V.; Arinc, A.; Youngman, M.; Arnold, D.; Wershofen, H.; Sill, D.S.; Bohrer, S.; Dahlgaard, H.; Croudace, I.W.; Warwick, P.E.; Ikäheimonen, T.K.; Klemola, S.; Vakulowsky, S.M.; Sanchez-Cabeza, J.A.

    The National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) for seaweed was developed through an interlaboratory comparison with 24 participants from 16 countries. After evaluating different techniques to calculate certified values for the radionuclides, the median...

  10. New reference materials improvement of methods of measurements

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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

  12. Reference materials and representative test materials: the nanotechnology case

    International Nuclear Information System (INIS)

    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).

  13. Preparation and certification of the human hair reference material

    International Nuclear Information System (INIS)

    The preparation of the human hair reference material and the steps taken to confirm its homogeneity and stability as well as its certification are described. Certified values for 17 elements, which are of importance for human health, and reference values for the other 13 elements are provided for this material. (author)

  14. A DANREF certified reference plastic for measurement of overall migration into the food simulant olive oil by single sided testing

    DEFF Research Database (Denmark)

    Lund, K. H.; Lillemark, L.; Petersen, Jens Højslev

    2000-01-01

    (CEN) [1, 2, 3] with exposure of the coextrudate to olive oil for 10 days at 40 degrees C. After an initial preliminary interlaboratory study eight laboratories participated in the certification round, and two different methods were used to obtain single sided exposure of the plastic to the oil. The...... certified value was determined as the mean of laboratory mean values. No outliers were found. A reference value of 8.6 mg/dm(2) +/- 1.4 mg/dm(2) (+/- half width of the 95% confidence interval) was obtained which is within the range relevant for the regulatory limit (10 mg/dm(2)), making this reference...... material suitable for laboratories measuring according to the EU overall migration limit [4]. The material has been found stable over 45 months....

  15. Development and use of reference materials and quality control materials

    International Nuclear Information System (INIS)

    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. Preparation and characterization of the fish reference material

    International Nuclear Information System (INIS)

    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)

  17. 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)

  18. Certification of reference materials for the determination of alkylphenols.

    Science.gov (United States)

    Hanari, Nobuyasu; Ishikawa, Keiichiro; Shimizu, Yoshitaka; Otsuka, Satoko; Iwasawa, Ryoko; Fujiki, Naomi; Numata, Masahiko; Yarita, Takashi; Kato, Kenji

    2015-04-01

    Certified reference materials (CRMs) are playing an increasingly important role in national and international standardizing activities. In Japan, primary standard solutions for analyses of endocrine disrupters are supplied under the national standards dissemination system named the Japan Calibration Service System (JCSS). For the traceability on reference materials used for preparation of the primary standard solutions based on the JCSS, the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has developed and certified high-purity reference materials of alkylphenols as NMIJ CRMs, such as 4-n-nonylphenol, 4-tert-octylphenol, 4-n-heptylphenol, 4-tert-butylphenol, and 2,4-dichlorophenol. Thereafter, it is essential to determine the alkylphenols by using these solutions based on the JCSS for environmental monitoring and risk assessments because analytical values obtained by using the solutions can ensure the reliability and traceability of the chemical analyses. PMID:25656848

  19. A certified reference material for the scratch test

    OpenAIRE

    Jacobs, R.; Meneve, J.; Dyson, G.; Teer, D. G.; Jennett, N.M.; P Harris; Stebut, J. von; Comte, C.; Feuchter, P.; Cavaleiro, A; Ronkainen, H.; Holmberg, K; Beck, U.; Reiners, G.; Ingelbrecht, C. D.

    2003-01-01

    Adhesion and other mechanical behaviour of coatings is at present routinely tested in industry and research organisations using the scratch test. The test has been the subject of a European Standard prEN 1071-3:2000 established by the European Standards Committee CEN TC184 WG5. A previous European project on the development and validation of test methods for thin hard coatings--FASTE--revealed that uncertainties in the Rockwell C stylus tip shape represent a major source of error for the scra...

  20. Development of thoria certified reference materials-role of NFC

    International Nuclear Information System (INIS)

    The present paper discusses the different phases of Inter Laboratory Comparison Experiments (ILCE) program for development of thoria CRMs with a special emphasis on the role played by Control Laboratory, NFC. The preparation of ThO2 CRMs along with their importance in analysis is also explained in the paper. (author)

  1. Preparation and certification of Sargasso seaweed reference material

    International Nuclear Information System (INIS)

    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. (author)

  2. 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.

  3. Nuclear measurements and reference materials

    International Nuclear Information System (INIS)

    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 235U 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 7Li and were started for the tritium production cross-section of 9Be. Reference materials of uranium minerals and ores were prepared. Special nuclear targets were prepared. A batch of 250 g of Pu02 was characterized in view of certification as reference material for the elemental assay of plutonium

  4. 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.

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

    International Nuclear Information System (INIS)

    An intercomparison exercise to determine the 14C 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 14C 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.

  6. Transuranium reference measurements and reference materials

    International Nuclear Information System (INIS)

    During the 30 years of its existence, the Central Bureau for Nuclear Measurements has been involved in numerous high-accuracy investigations of mainly nuclear properties of elements important for the nuclear fuel cycle and for application of relevant radionuclides. This paper reports that these studies were made possible by the availability of particle accelerators (150-MeV electron linear accelerator; 3.7- and 7-MV Van de Graaff accelerators) as neutron sources and the use of specialized laboratories for the preparation, characterization, and manipulation of radioactive samples. Examples of investigations with plutonium and neptunium are capture and fission cross sections of 239Pu at very low energies, spontaneous fission fragment mass and energy distributions of 242Pu at very low energies, spontaneous fission fragment mass and energy distributions of 242Pu, alpha-particle and gamma-ray spectra of 237Np, half-life of 241Pu, use of 237Np in reactor neutron dosimetry, preparation and characterization of plutonium oxide reference materials for nondestructive analysis, and demonstration of the potential of synthetic isotope mixtures for analytical control of the nuclear fuel cycle

  7. 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.)

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

    International Nuclear Information System (INIS)

    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 235U/U - and 238U/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

  9. The new IAEA reference material: IAEA-434 technologically enhanced naturally occurring radioactive materials (TENORM) in phosphogypsum

    Energy Technology Data Exchange (ETDEWEB)

    Shakhashiro, A., E-mail: A.Shakhashiro@iaea.or [International Atomic Energy Agency, Agency' s Laboratories, Vienna International Center, PO Box 100, A-1400 Vienna (Austria); Sansone, U. [International Atomic Energy Agency, Agency' s Laboratories, Vienna International Center, PO Box 100, A-1400 Vienna (Austria); Wershofen, H. [Environmental Radioactivity, PTP, Braunschweig (Germany); Bollhoefer, A. [Environmental Radioactivity, Department of the Environment and Heritage, Darwin (Australia); Kim, C.K. [International Atomic Energy Agency, Agency' s Laboratories, Vienna International Center, PO Box 100, A-1400 Vienna (Austria); Kim, C.S. [Department of Environmental Radioactivity Assessment, Korea Institute of Nuclear Safety, Daejeon, Republic of Korea (Former collaborator) (Korea, Republic of); Kis-Benedek, G. [International Atomic Energy Agency, Agency' s Laboratories, Vienna International Center, PO Box 100, A-1400 Vienna (Austria); Korun, M. [Jozef Stefan Institute, Ljubljana (Slovenia); Moune, M. [LNE-LNHB, Laboratoire National Henri Becquerel, Gif-sur-Yvette Cedex (France); Lee, S.H. [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of); Tarjan, S. [Central Radiological Laboratory, Hungarian Agricultural Authority, Budapest (Hungary); Al-Masri, M.S. [Atomic Energy Commission of Syria, Damascus (Syrian Arab Republic)

    2011-01-15

    A reliable determination of Technologically Enhanced Naturally Occurring Radioactive Materials in phosphogypsum is necessary to comply with radiation protection and environmental regulations. In this respect, a new phosphogypsum reference material was produced and certified to assist in the validation of analytical methods and the quality assurance of produced analytical results. This paper presents the sample preparation methodology, material homogeneity assessment, characterization campaign results and assignment of property values, and associated uncertainties. The reference values and associated uncertainties for Pb-210, Ra-226, Th-230, U-234 and U-238 were established based on consensus values calculated from analytical results reported by three National Metrology Institutes and five expert laboratories.

  10. Certification of elements in and use of standard reference material 3280 multivitamin/multielement tablets

    Science.gov (United States)

    Standard Reference Material (SRM) 3280 Multivitamin/Multielement Tablets was issued by the National Institute of Standards and Technology (NIST) in 2009 and has certified and reference mass fraction values for 13 vitamins, 26 elements, and 2 carotenoids. Elements were measured using two or more ana...

  11. 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.

  12. 40 CFR 1042.910 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... reference as prescribed in 5 U.S.C. 552(a) and 1 CFR part 51. Anyone may inspect copies at the U.S. EPA, Air... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Reference materials. 1042.910 Section... Other Reference Information § 1042.910 Reference materials. Documents listed in this section have...

  13. Radium-226 in certified uranium reference ores DL-1a, BL-4a, DH-1a and BL-5

    International Nuclear Information System (INIS)

    Radium-226 radioactivity in uranium reference ores BL-4a and BL-5 and uranium-thorium reference ores DL-1a and DH-1a was determined in an interlaboratory program. Twelve of thirteen participants used certified radium solutions from the United States National Bureau of Standards (NBS) for calibration purposes. Recommended values of sup(226)Ra activity and associated parameters were calculated by statistical treatment of the results. In all cases, the recommended values are within 2 percent of activities predicted assuming secular equilibrium in the sup(238)U decay series. The recommended values for radium activity are 1.40, 15.5, 31.5 and 857 Bq/ for DL-1a, BL-4a, DH-1a and BL-5, respectively

  14. Reference to the Safety Engineering Undergraduate Courses to Improve the Subjects and Contents of the Certified Safety Engineer Qualification and Examination System of China

    OpenAIRE

    Haibin Qiu; Shanghong Shi; Tingdi Zhao; Yiwei Qiao; Jiangshi Zhang

    2013-01-01

    The aim of this paper is to recommend that the subjects and contents of certified safety engineers use safety engineering undergraduate curriculum system for reference. Human resources play an important role in accident prevention and loss control. Education on safety engineering develops quickly in China. Moreover, the State Administration of Work Safety and the National Human Resources and Social Security Ministry have implemented a certified safety engineer qualification and examination sy...

  15. Primary certification of reference material for electrolytic conductivity of bioethanol

    Science.gov (United States)

    da Silva, L. F.; Gomes, M. R. F.; Cassini, G. C.; Faria, A. C. V.; Fraga, I. C. S.

    2016-07-01

    Nowadays the preservation of the planet is spreading into the international scene with the use of renewable energy sources such as bioethanol. The challenge is to guarantee the quality of produced bioethanol, and the electrolytic conductivity (EC) is one of the specified parameters for this purpose. However, is necessary to demonstrate the metrological traceability of the measurement results for EC in this matrix. This study presents the certification of a reference material for EC in bioethanol by using only primary measurements. The value of primary certified reference material (CRM) is (0.77 ± 0.06) µS.cm-1, and its use will provide the metrological traceability needed for measurement results in laboratories.

  16. Bisphenol A polycarbonate as a reference material

    Science.gov (United States)

    Hilado, C. J.; Cumming, H. J.; Williams, J. B.

    1977-01-01

    Test methods require reference materials to standardize and maintain quality control. Various materials have been evaluated as possible reference materials, including a sample of bisphenol A polycarbonate without additives. Screening tests for relative toxicity under various experimental conditions were performed using male mice exposed to pyrolysis effluents over a 200-800 C temperature range. It was found that the bisphenol A polycarbonate served as a suitable reference material as it is available in large quantities, and does not significantly change with time.

  17. 40 CFR 1043.100 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... in 5 U.S.C. 552(a) and 1 CFR part 51. Anyone may inspect copies at the U.S. EPA, Air and Radiation... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Reference materials. 1043.100 Section... § 1043.100 Reference materials. Documents listed in this section have been incorporated by reference...

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

    International Nuclear Information System (INIS)

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

  19. 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)

  20. Preparation and characterization of standard reference material 1849 infant/adult nutritional formula.

    Science.gov (United States)

    Sharpless, Katherine E; Lindstrom, Richard M; Nelson, Bryant C; Phinney, Karen W; Rimmer, Catherine A; Sander, Lane C; Schantz, Michele M; Spatz, Rabia O; Thomas, Jeanice Brown; Turk, Gregory C; Wise, Stephen A; Wood, Laura J; Yen, James H

    2010-01-01

    Standard Reference Material (SRM) 1849 Infant/Adult Nutritional Formula has been issued by the National Institute of Standards and Technology (NIST) as a replacement for SRM 1846 Infant Formula, issued in 1996. Extraction characteristics of SRM 1846 have changed over time, as have NIST's analytical capabilities. While certified mass fraction values were provided for five constituents in SRM 1846 (four vitamins plus iodine), certified mass fraction values for 43 constituents are provided in SRM 1849 (fatty acids, elements, and vitamins) and reference mass fraction values are provided for an additional 43 constituents including amino acids and nucleotides, making it the most extensively characterized food-matrix SRM available from NIST. PMID:20922961

  1. Elemental determinations in NBS 1633A Fly Ash Standard Reference material using INAA PGNAA

    Energy Technology Data Exchange (ETDEWEB)

    Vogt, J.R.; Schlegel, S.C. (Missouri Univ., Columbia (USA). Research Reactor Facility)

    1985-02-01

    INAA was used for the determination of 23 elements, and prompt gamma neutron activation analysis (PGNAA) for the determination of 10 elements in U.S. National Bureau of Standards (NBS) 1633A Fly Ash Standard Reference Material. The results are in excellent agreement with the limited number of NBS certified values available.

  2. Use of gelatin gels as a reference material for performance evaluation of meat shear force measurements

    Science.gov (United States)

    Establishing standards for meat tenderness based on Warner-Bratzler shear force (WBSF) is complicated by the lack of methods for certifying WBSF testing among texture systems or laboratories. The objective of this study was to determine the suitability of using gelatin gels as a reference material ...

  3. QUALITY AND PERFORMANCE EVALUATION OF REFERENCE MATERIALS FOR THE DETERMINATION OF NUTRIENTS IN FOODS

    Science.gov (United States)

    Certified reference materials (CRMs) play a critical role in validating the accuracy of analytical data and have been used extensively in the USDA's ongoing National Food and Nutrient Analysis Program (NFNAP), which generates contract analytical food composition data for inclusion in the USDA Nation...

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

    International Nuclear Information System (INIS)

    The ko-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

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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

  7. 40 CFR 86.1 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ....C. 552(a) and 1 CFR part 51. To enforce any edition other than that specified in this section, a... 40 Protection of Environment 18 2010-07-01 2010-07-01 false Reference materials. 86.1 Section 86.1... EMISSIONS FROM NEW AND IN-USE HIGHWAY VEHICLES AND ENGINES § 86.1 Reference materials. Link to an...

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

    International Nuclear Information System (INIS)

    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

  9. 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.

  10. Developing a matrix reference material for screening of transgenic rice.

    Science.gov (United States)

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

    2015-12-01

    Certified reference materials (CRMs) that are compatible with detection methods are needed to detect genetically modified organisms (GMOs). Screening is the first detection step in determining the possible presence of GMO ingredients in food or feed; however, screening has been hindered by the lack of GMO CRMs. In this study, transgenic rice materials were developed via the transformation of a construct harboring 11 commonly used screening elements. Digital PCR was utilized to identify a homozygous single-copy line termed SDrice. The qualitative detections of 11 elements in 21 transgenic materials demonstrated that the genomic DNA of the SDrice was suitable for use as a positive control in the screening of GMO ingredients. The suitability of SDrice as reference material was further checked by testing the sensitivity of 11 known conventional PCR assays, ranging from 10 to 50 copies of the SDrice genome. The standard curves that were created using SDrice DNA series as calibrators all exhibited good linearities in the relationships of the Ct values with the template copy numbers in these 11 real-time PCR assays. The LODs of the real-time PCR assays were estimated to be two to five copies of the SDrice genome. Comparisons of the SDrice with other GM rice revealed that significant differences existed in both the intercepts of the standard curves and the ΔCt values of the exogenous and reference genes for the P-35S, T-nos, HPT, T-35S, and Bar assays; the SDrice was not fit for quantification of other GM rice events. This study provided a matrix reference material (RM) that was suitable for screening GM rice, determination of sensitivity and a LOD of PCR assays, and overcame some of the drawbacks of plasmid DNA as reference material. PMID:26462921

  11. Roadmap for radioanalytical reference and performance evaluation materials for current and emerging issues

    International Nuclear Information System (INIS)

    Reference materials are fundamental tools for radiochemistry measurements laboratories to establish and evaluate analytical methods, test measurement capabilities, quantify radionuclides, compare analytical results, and establish legal confidence defensibility in measurement results. Over the past decades the focus of low-level environmental reference material producers have adapted to evolving national and international priorities and needs. This document provides a Roadmap of high priority current and future low-level radionuclide Certified Reference and Performance Evaluation Materials that subject-matter experts have identified at NIST and other public workshops (Blueprints) as crucial to metrologists and program directors to address national and international issues. (author)

  12. Standard reference materials for foods and dietary supplements.

    Science.gov (United States)

    Sharpless, Katherine E; Thomas, Jeanice Brown; Christopher, Steven J; Greenberg, Robert R; Sander, Lane C; Schantz, Michele M; Welch, Michael J; Wise, Stephen A

    2007-09-01

    Well-characterized certified reference materials are needed by laboratories in the food testing, dietary supplement, and nutrition communities to facilitate compliance with labeling laws and improve the accuracy of information provided on product labels, so that consumers can make good choices. As a result of the enactment of the Nutrition Labeling and Education Act of 1990 and the Infant Formula Act of 1980, the National Institute of Standards and Technology (NIST) worked to develop a series of food-matrix standard reference materials (SRMs) characterized for nutrient concentrations. These include SRM 1544 Fatty Acids and Cholesterol in a Frozen Diet Composite, SRM 1546 Meat Homogenate, SRM 1548a Typical Diet, SRM 1566b Oyster Tissue, SRM 1846 Infant Formula, SRM 1946 Lake Superior Fish Tissue, SRM 1947 Lake Michigan Fish Tissue, SRM 2383 Baby Food Composite, SRM 2384 Baking Chocolate, SRM 2385 Slurried Spinach, and SRM 2387 Peanut Butter. With the enactment of the Dietary Supplement Health and Education Act of 1994, NIST has been working to develop suites of dietary supplement SRMs characterized for active and marker compounds and for toxic elements and pesticides, where appropriate. An updated SRM 1588b Organics in Cod Liver Oil, a suite of ephedra-containing materials (SRMs 3240-3245), a carrot extract in oil (SRM 3276), and a suite of ginkgo-containing materials (SRMs 3246-3248) are available. Several other materials are currently in preparation. Dietary supplements are sometimes provided in forms that are food-like; for these, values may also be assigned for nutrients, for example SRM 3244 Ephedra-Containing Protein Powder. Both the food-matrix and dietary supplement reference materials are intended primarily for validation of analytical methods. They may also be used as "primary control materials" in assignment of values to in-house (secondary) control materials to confirm accuracy and to establish measurement traceability to NIST. PMID:17534610

  13. Characterization of nanoparticles as candidate reference materials

    International Nuclear Information System (INIS)

    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)

  14. Characterization of nanoparticles as candidate reference materials

    Energy Technology Data Exchange (ETDEWEB)

    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., E-mail: smlandi@inmetro.gov.br [Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMETRO), Rio de Janeiro, RJ (Brazil)

    2013-07-01

    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. Validation Test For The Result Of Neutron Activation Analysis With Standard Reference Material

    International Nuclear Information System (INIS)

    The validity test with standard reference material is necessary to ensure the result analysis of samples. The analysis of CRM No.8 (Vehicle Exhaust Particulates) and SRM 1646a (Estuary Sediment) has been done in P2TRR. These analysis is intended to validate the analysis result done in NAA laboratory of P2TRR. For the CRM No. 8, is elements of the 30 certified elements were successfully analyzed Meanwhile, for SRM 1646a, 21 elements of the 39 certified elements were completely investigated The quantitative analysis showed the relative difference of 2% - 15% compared to the certificate

  16. Reference materials for microanalytical nuclear techniques

    International Nuclear Information System (INIS)

    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. 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

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

    International Nuclear Information System (INIS)

    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)

  19. Reference material for natural radionuclides in glass designed for underground experiments

    OpenAIRE

    Povinec, P.; PHAM M. K.; Busto, J.; Cerna, C.; Degering, D.; Y. Hamajima; Holy, K.; Hult, Mikael; Jeskovsky, M.; Koehler, M; Kovacik, A.; Laubenstein, Matthias; Loaiza, P.; Mamedov, F.; Marquet, C.

    2015-01-01

    A reference material designed for the determination of natural radionuclides in solid samples (glass pellets) is described and the results of certification are presented. The material has been certified for 7 natural radionuclides (40K, 226Ra, 228Ra, 228Th, 232Th, 235U and 238U). An information value is given for 210Pb. Radon (222Rn) emanation experiments showed results comparable within participating laboratories, however, the number of data and precision was too low to carry out a certifica...

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

    International Nuclear Information System (INIS)

    Reliable isotope measurements of nuclear material and the availability of reference materials with small uncertainties in the certified values are of great importance for safeguarding of nuclear materials. They provide the basis for a credible measurement system in the verification of states declarations of their nuclear activities. Worldwide needs for continued and improved Isotopic Reference Materials (IRM) are the main reason for developments of new nuclear reference materials at IRMM. Measurement capabilities of laboratories have evolved considerably over the years, along with progress in modern analytical techniques. Some plutonium reference materials, however, have been on the market for decades and they need to be re-certified to smaller uncertainties. Moreover, new reference materials with appropriately small uncertainties in the certified values need to be made available enabling measurement laboratories to reduce their combined measurement uncertainties. Such high quality plutonium isotopic reference materials are essential for laboratories striving to meet the International Target Values for Measurement Uncertainties in Safeguarding Nuclear Materials (ITVs). The preparation and the certification of such materials are demanding and challenging tasks that require state-of-theart measurement procedures and equipment. The Institute for Reference Materials and Measurements (IRMM) has repeatedly demonstrated its capabilities in plutonium analysis and represents one of the few institutes that supplies plutonium IRMs worldwide. An inter-calibration campaign has been set up at IRMM inter-linking selected plutonium spike IRMs. In the scope of this compatibility study, new reference materials have been prepared for Isotope Dilution Mass Spectrometry (IDMS) in nuclear fuel cycle measurements. A new series of large-sized dried (LSD) spikes, IRMM- 1027n, has been prepared and certified for plutonium and uranium amount content and isotopic composition. These mixed

  1. 49 CFR 171.7 - Reference material.

    Science.gov (United States)

    2010-10-01

    ... sections in which the material is referenced. Source and name of material 49 CFR reference American.../publications.com; AAR Manual of Standards and Recommended Practices, Section C—Part III, Specifications for..., AND DEFINITIONS Applicability, General Requirements, and North American Shipments § 171.7...

  2. Trace element determination in a mussel reference material using short irradiation instrumental neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Edson G.; Seo, Daniele; Vasconcellos, Marina B.A.; Saiki, Mitiko, E-mail: emoreira@ipen.b, E-mail: mbvascon@ipen.b, E-mail: mitiko@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    The production of certified reference materials in Brazil, and the consequent availability to national end users, is an important task for the enhancement of Metrology in Chemistry status in the country, as these materials are used for method validation, equipment calibration and for establishing metrological traceability links. In this study, Instrumental Neutron Activation Analysis (INAA) was applied to the determination of magnesium, manganese and vanadium in a mussel reference material produced at IPEN-CNEN/SP. For the determination of these elements via the comparative INAA method, the respective analytical radionuclides, {sup 27}Mg, {sup 56}Mn, and {sup 52}V, are short lived and then, short irradiations are used. The main advantage over longer irradiation methods is the faster output of analytical results. Six subsamples from two bottles of the Perna perna mussel reference material were analyzed. Each subsample was simultaneously irradiated with elemental standards for 10 s at the IEA - R1 research nuclear reactor through a pneumatic transfer system. After suitable decay periods, gamma radioactivity measurements were carried out, using a hyperpure germanium detector. The accuracy of the method was checked by using the NIST SRM 1566b - 'Oyster Tissue' certified reference material. The comparison of the obtained results to the robust mean of the interlaboratorial collaborative trial used for the characterization of the mussel reference material showed that the short irradiation INAA method is suitable for the characterization of new reference materials. (author)

  3. Trace element determination in a mussel reference material using short irradiation instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    The production of certified reference materials in Brazil, and the consequent availability to national end users, is an important task for the enhancement of Metrology in Chemistry status in the country, as these materials are used for method validation, equipment calibration and for establishing metrological traceability links. In this study, Instrumental Neutron Activation Analysis (INAA) was applied to the determination of bromine, chlorine, magnesium, manganese, potassium and vanadium in a mussel reference material produced at IPEN-CNEN/SP. For the determination of these elements via the comparative INAA method, the respective analytical radionuclides, 80Br, 38Cl, 27Mg, 56Mn, 42K and 52V, are short lived and then, short irradiations are used. Six subsamples from two bottles of the Perna perna mussel reference material were analyzed. Each subsample was simultaneously irradiated with elemental standards for 10 s at the IEA-R1 research nuclear reactor through a pneumatic transfer system. After suitable decay periods, gamma radioactivity measurements were carried out, using a hyperpure germanium detector. The accuracy of the method was checked by using the NIST SRM 1566b-'Oyster Tissue' certified reference material. The comparison of the results obtained in this study to the robust mean of the interlaboratorial collaborative trial used for the characterization of the mussel reference material was performed via z-score tests. The comparison showed that the short irradiation INAA method is suitable for the characterization of new reference materials. (author)

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

    International Nuclear Information System (INIS)

    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)

  5. Preparation of two uranium glass reference materials for fission-track dating of geological samples

    International Nuclear Information System (INIS)

    The European Commission produced and certified uranium glass for fission-track dating in 1996 (Reference Material IRMM-540). This material is now out of stock and a project for the preparation of two new reference glasses is underway. The new glasses, containing nominally 15 and 55 mg kg-1 uranium, were prepared from blended oxide powder, and cast using an improved method, which minimised micro-scale defects and optimised the yield. Glass rods were produced which were then cut into discs of 2 mm thickness and 15 mm diameter and subsequently polished. Uranium homogeneity and fission-track stability are critical properties of the glass. An extensive study was carried out to verify the homogeneity by fission-track counting, investigating both within-disc and between disc effects, and to investigate potential track fading due to thermal annealing. No evidence of uranium heterogeneity was detected. The stability study, using an 'isochronous' method, in which all measurements are made at the end of exposure to artificial ageing, is still underway. The reference material will be certified for isotopic composition (natural), uranium mass fraction and neutron fluence (one disc out of each set of three will be irradiated, together with a mica foil, to induce fission tracks in a certified fluence). The reference materials will be released as IRMM-540R (15 mg kg-1 U) and IRMM-541 (55 mg kg-1 U)

  6. The certification of a new paint reference material

    International Nuclear Information System (INIS)

    The use of paint as a coating for toys intended for sale on the European market is controlled by a European Standard (EN 71-3: 1994 - European Commission to produce a new paint reference material which can be used to validate the test methods given in the European Standard. The migration of elements from painted panels and comminuted paint produced by the Laboratory of the Government Chemist, (U.K.) was studied. Several methods were used in this certification exercise and this work reports the results of neutron activation analysis and inductively coupled plasma mass spectrometry to determine the migration of As, Ba, Cd, Cr, Hg, Pb, Se and Sb into a simulated stomach environment. Replicate extracts obtained from paint samples gave a precision of within 10% for most elements by both analytical techniques for the paint panels and for the comminuted paint sample. This preliminary study has shown that the standard method can provide reproducible results for each of the paint materials studied and indicates that the study should be continued to produce a fully certified paint reference material. (author)

  7. 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.

  8. Characterization of Standard Reference Material 2940, Mn-ion-doped glass, spectral correction standard for fluorescence

    International Nuclear Information System (INIS)

    Standard Reference Material (SRM) 2940 is a cuvette-shaped, Mn-ion-doped glass, recommended for use for relative spectral correction of emission and day-to-day performance validation of steady-state fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum were explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy, temperature coefficient of fluorescence intensity, and fluorescence lifetimes. Long and short lifetime components of the fluorescence displayed different emission spectra, making the certified spectrum useful with fluorescence instruments employing continuous excitation only. The expanded uncertainties in the certified spectrum are about 5% around the peak maximum at 620 nm, using an excitation wavelength of 412 nm. The SRM also exhibits a strong resistance to photodegradation, with no measurable decrease in fluorescence intensity even after 17 h of irradiation with the visible light from a Xe lamp

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

    International Nuclear Information System (INIS)

    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

  10. Development of solid radium-226 reference materials

    International Nuclear Information System (INIS)

    Radium-226 reference materials having a matrix similar to soil or tailings samples are not available in sufficient quantity for use by remedial-action contractors to calibrate their laboratory gamma-ray spectrometers. Such reference materials are needed to provide uniform standardization among measurements made by remedial-action contractors. A task, therefore, was undertaken to prepare about 200 pounds each of three different concentrations of radium-226 reference materials by diluting tailings with high-purity silica. Target values for radium-226 content were 50, 15, and 5 pCi/g. The radium-226 content of the reference materials was measured by C.W. Sill of EG and G Idaho, Inc., Idaho Falls, using a high- resolution alpha spectrometry technique standardized with National Bureau of Standards (NBS) standard 4961. A summary of this technique is provided in Appendix A of this report. An independent measurement of the radium-226 content was conducted by Bendix Field Engineering Corporation (Bendix), Grand Junction, Colorado, using a high-resolution Ge(Li) detector, which was calibrated using the New Brunswick Laboratory (NBL) 100-A Series standards. The Ge(Li) detector has also been used to determine the radium-226 content in the calibration models at the Grand Junction facility; these models are used by remedial-action contractors for calibration of borehole logging gamma-ray probes. 8 references, 12 tables

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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 Na2CO3. 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.

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

    International Nuclear Information System (INIS)

    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

  14. AQCS 1989 - Intercomparison runs reference materials

    International Nuclear Information System (INIS)

    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

  15. Preliminary rare earth determinations on 14 Brazilian and one Venezuelan reference geological material

    International Nuclear Information System (INIS)

    The contents of 13 Rare Earth Elements (REE) in the 12 Instituto de Pesquisas Tecnologicas (IPT), 2 Centro de Tecnologia Mineral's (CETEM) and 1 Venezuelan geological reference materials were determined by Inductively Coupled Plasma (ICP). Among the 15 analysed samples, the clays IPT-28, IPT-30 and IPT-42 are the only samples that have REE reported in the literature, and comparisons with our results were made. While the certified elements of these reference materials made them very valuable for laboratory control in mining and industry, their value could be greatly enhanced if trace elements data of geochemical interest were available. (author)

  16. AQCS 1990. Intercomparison runs, reference materials

    International Nuclear Information System (INIS)

    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

  17. Certification of uranium hexafluoride reference materials for isotopic composition

    International Nuclear Information System (INIS)

    The IRMM-019 to IRMM-029 series of uranium hexafluoride materials is certified for the isotopic composition. After conversion into uranyl nitrate solution, certification and homogeneity measurements were performed by thermal ionization mass spectrometry. Analyses were performed by Modified Total Evaporation and for some materials the major isotope amount ratio n(235U)/n(238U) was measured using a n(233U)/n(236U) double spike. Measurements were confirmed by UF6 gas source mass spectrometry. Major isotope amount ratios were certified with relative expanded uncertainties (k = 2) of 0.015-0.030 % and the minor isotope amount ratios n(234U)/n(238U) and n(236U)/n(238U) were certified with relative expanded uncertainties of 0.02-3 %. (author)

  18. Neutron activation analysis of reference materials

    International Nuclear Information System (INIS)

    The importance is pointed out of neutron activation analysis in the preparation of reference materials, and studies are reported conducted recently by UJV. Instrumental neutron activation analysis has been used in testing homogeneity and in determining 28 elements in newly prepared reference standards of coal fly ash designated ENO, EOP and ECH. For accuracy testing, the same method was used in the analysis of NBS SRM-1633a Trace Elements in Coal Fly Ash and IAEA CRM Soil-5 and RM Soil-7. Radiochemical neutron activation analysis was used in determining Cd, Cu, Mn, Mo, and Zn in biological materials NBS SRM-1577 Bovine Liver, Bowen's Kale and in IAEA RM Milk Powder A-11 and Animal Muscle H-4. In all instances very good precision and accuracy of neutron activation analysis results were shown. (author)

  19. AQCS intercomparison runs, reference materials 1991

    International Nuclear Information System (INIS)

    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

  20. Natural matrix radioactivity standards and reference materials

    International Nuclear Information System (INIS)

    Although the precise definition of Natural Matrix Standard (NMS) and Natural Matrix Reference Material (NMRM) remain somewhat unclear, few doubt their extreme usefulness in virtually all programs involving measurements of radioacitivity. Rigorous quality assurance/quality control is difficult, if not impossible, particularly in studies requiring radiochemical/radiometric analyses of environmental matrices, when lacking good NMSs and NMRMs. A fairly comprehensive range of these materials is now available internationally, at a reasonable cost. Progress on the National Bureau of Standards NMS program as well as EML's Quality Assessment Program are discussed. In addition 99Tc in vegetation is presented as a specific example of the methodology of preparing a NMRM. (orig.)

  1. 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)

  2. Nuclear microprobe analysis of the standard reference materials

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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)

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

    International Nuclear Information System (INIS)

    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)

  5. Reference and testing materials available from the Materials Characterization Center

    International Nuclear Information System (INIS)

    A major responsibility of the Materials Characterization Center (MCC) is to acquire and distribute reference and testing materials endorsed by DOE, for use in research and development in nuclear waste management. MCC standard materials provide a common basis for data obtained in waste repository development work, thereby assisting in developing a defensible database of known accuracy and precision. Homogeneity of standard materials is of particular importance. MCC emphasizes homogeneity of composition and physical characteristics of the standard materials, using statistical methods in sampling procedures and evaluation of analytical data. Two classifications of standard materials are available from the MCC. Approved Reference Materials (ARMs) are intended as standard reference and calibration materials [similar to the SRMs of the US National Bureau of Standards (NBS)], for field calibration of MCC standard test methods. Each ARM is characterized by MCC and other laboratories such as NBS to a high level of accuracy and precision. Approved Testing Materials (ATMs) are used as common testing materials, representing specific formulations of typical waste forms. Most ATMs are radioactive materials, for which characterization has been conducted on shielded analytical instruments at PNL. More than ten different ATMs (borosilicate glass and spent fuel) are in the MCC inventory. These materials are available without charged, in reasonable amounts, to DOE programs. Other users pay pro-rated production costs. The materials normally are supplied in the form in which they were produced, e.g., glass as-cast bars. In some cases the MCC can supply special specimen forms, e.g., crushed powders or shaped monoliths

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

    International Nuclear Information System (INIS)

    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. 241Pu and 241Am). 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. 241Am/241Pu. 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 241Am/241Pu, 238Pu/234U, 239Pu/235U, 240Pu/236U, and possibly 242Pu/238U. 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 (238Pu, 239Pu, 240Pu, 241Pu, 242Pu) and daughter (234U, 235U, 236U, 238U and

  7. 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...

  8. Future needs and requirements for AMS 14C standards and reference materials

    International Nuclear Information System (INIS)

    14C measurement uses a number of standards and reference materials with different properties. Historically the absolute calibration of 14C measurement was tied to 1890 wood, through the 'primary' standard of NBS-OxI (produced by the National Bureau of Standards, now NIST - National Institute of Standards and technology) subsequently replaced by NBS-OxII. These are both internationally calibrated and certified materials, whose 14C activities are known absolutely. A second tier of materials, often called secondary standards or reference materials, and including internationally recognised materials such as ANU-sucrose (now also IAEA-C6), Chinese - sucrose and the IAEA C1-C6 series, augmented by additional oxalic acid samples are also used routinely. The activity of these materials has been estimated from large numbers of measurements made by many laboratories. Recently, further natural materials from the Third and Fourth International Radiocarbon Inter-comparisons (TIRI and FIRI) have been added to this list. The activities of these standards and reference materials span both the applied 14C age range and the chemical composition range of typical samples, but this is not achieved uniformly and there is a continuing need for reference materials for laboratory quality control and measurement-traceability purposes. In this paper, we review the development of 14C standards and reference materials and consider the future requirements for such materials within the 14C AMS community

  9. Reference material manufacture and certification for the AVNG

    International Nuclear Information System (INIS)

    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.

  10. 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.

  11. Development of a Northern Continental Air Standard Reference Material.

    Science.gov (United States)

    Rhoderick, George C; Kitzis, Duane R; Kelley, Michael E; Miller, Walter R; Hall, Bradley D; Dlugokencky, Edward J; Tans, Pieter P; Possolo, Antonio; Carney, Jennifer

    2016-03-15

    The National Institute of Standards and Technology (NIST) recently began to develop standard mixtures of greenhouse gases as part of a broad program mandated by the 2009 United States Congress to support research in climate change. To this end, NIST developed suites of gravimetrically assigned primary standard mixtures (PSMs) comprising carbon dioxide (CO2), methane (CH4), and nitrous oxide (N2O) in a dry-natural air balance at ambient mole fraction levels. In parallel, the National Oceanic and Atmospheric Administration (NOAA) in Boulder, Colorado, charged 30 aluminum gas cylinders with northern hemisphere air at Niwot Ridge, Colorado. These mixtures, which constitute NIST Standard Reference Material (SRM) 1720 Northern Continental Air, were certified by NIST for ambient mole fractions of CO2, CH4, and N2O relative to NIST PSMs. NOAA-assigned values are also provided as information in support of the World Meteorological Organization (WMO) Global Atmosphere Watch (GAW) Program for CO2, CH4, and N2O, since NOAA serves as the WMO Central Calibration Laboratory (CCL) for CO2, CH4, and N2O. Relative expanded uncertainties at the 95% confidence interval are first of its kind for a gaseous SRM developed by NIST. PMID:26890890

  12. 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.

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

    International Nuclear Information System (INIS)

    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. Certification of the uranium hexafluoride reference materials for isotopic composition

    OpenAIRE

    MIALLE SÉBASTIEN; Richter, Stephan; HENNESSY Carmel; TRUYENS Jan; Jakobsson, Ulf; Aregbe, Yetunde

    2014-01-01

    The IRMM-019 to IRMM-029 series of uranium hexafluoride materials is certified for the isotopic composition. After conversion into uranyl nitrate solution, certification and homogeneity measurements were performed by Thermal Ionization Mass Spectrometry. Analyses were performed by Modified Total Evaporation and for some materials the major isotope amount ratio n(235U)/n(238U) was measured using a n(233U)/n(236U) double spike. Measurements were confirmed by UF6 Gas Source Mass Spectrometry. Ma...

  15. Multi-elemental nuclear analysis of soil reference material

    International Nuclear Information System (INIS)

    Full text: In the last years, in the LEER (Laboratorio de Espectroscopia e Espectrometria das Radiacoes) at IPEN, several certified reference materials using neutron activation aiming to optimize its uses in different areas. Based on it, several works have been done using INAA as well as NAA with Au as flux monitor, i. e., a variant of k0 - NAA, or combination of both techniques using the different experimental facilities at IPEN: the IEA-R1 and MB-01 Nuclear Reactors and Neutron Irradiator. The intention of this research was to check the viability of using parametric NAA in the IEA-R1 nuclear reactor for performing soil characterization. The performance of this procedure was compared to results obtained in the same reference material using the k0-standardization method using the TRIGA MARK - IPR-R1 nuclear reactor from CDTN/CNEN, Belo Horizonte. The concentration of the elements in the soil reference material (IAEA/SOIL-7) was obtained using the parametric and at k0- standardization methods of neutron activation analyses. For parametric analyses the Cd Ratio Technique was used for the measurement of thermal neutron flux distribution, in the IEA-R1 nuclear reactor at IPEN/CNEN and the concentration was obtained by using an in-house software, which correlated the measured parameters, i. e., neutron flux, net area and efficiency of the selected gamma ray with the constants physics involved (the decay constant; the atomic masses, the Avogadro number, the cross section for the selected capture reaction, the isotopic fraction and the intensity of the gamma ray). For k0-standardization measurements a set of monitors (Al-(0.1%)-Au discs and Zr foils) were used for neutron flux determination in the TRIGA MARK I IPR-R1 nuclear reactor at CDTN/CNEN, and the concentration was obtained applying the commercial KayWin software package. The performance of these procedures is compared and the advantages and disadvantages of each method and sources of errors are discussed. (author)

  16. Characterization of Standard Reference Material 2941, uranyl-ion-doped glass, spectral correction standard for fluorescence

    International Nuclear Information System (INIS)

    Standard Reference Material (SRM) 2941 is a cuvette-shaped, uranyl-ion-doped glass, recommended for use for relative spectral correction of emission and day-to-day performance validation of fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum have been explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy, temperature coefficient of fluorescence intensity, and fluorescence lifetimes. The expanded uncertainties in the certified spectrum are about 4% around the peak maximum at 526 nm, using an excitation wavelength of 427 nm. The SRM also exhibits a strong resistance to photodegradation, with no measurable decrease in fluorescence intensity even after 8 h of laser irradiation

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

    International Nuclear Information System (INIS)

    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 90Sr, 137Cs and 239Pu + 240Pu. 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: 40K, 90Sr, 129I, 137Cs, 155Eu, 210Pb, 210Po, 212Pb, 214Bi, 226Ra, 228Ra, 228Th, 230Th, 232Th, 234U, 235U, 237Np, 238U, 238Pu, 239Pu + 240Pu, and 241Am. 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-dried shellfish flesh matrix has been

  18. Reference material for natural radionuclides in glass designed for underground experiments

    International Nuclear Information System (INIS)

    A reference material designed for the determination of natural radionuclides in solid samples (glass pellets) is described and the results of certification are presented. The material has been certified for 7 natural radionuclides (40K, 226Ra, 228Ra, 228Th, 232Th, 235U and 238U). An information value is given for 210Pb. Radon (222Rn) emanation experiments showed results comparable within participating laboratories, however, the number of data and precision was too low to carry out a certification process. The reference material may be used for quality management of analytical laboratories engaged in the high-sensitive analysis of radionuclides in the construction materials of detectors placed in ultra low background underground laboratories. (author)

  19. Reference material for natural radionuclides in glass designed for underground experiments

    CERN Document Server

    Povinec, P P; Busto, J; Cerna, C; Degering, D; Hamajima, Y; Holy, K; Hult, M; Jeskovsky, M; Koehler, M; Kovacik, A; Laubenstein, M; Loaiza, P; Mamedov, F; Marquet, C; Mott, J; Mullerova, M; Perrot, F; Piquemal, F; Reyss, J -L; Saakyan, R; Simgen, H; Soule, B; Stanicek, J; Sykora, I; Stekl, I

    2015-01-01

    A reference material designed for the determination of natural radionuclides in solid samples (glass pellets) is described and the results of certification are presented. The material has been certified for 7 natural radionuclides (40K, 226Ra, 228Ra, 228Th, 232Th, 235U and 238U). An information value is given for 210Pb. Radon (222Rn) emanation experiments showed results comparable within participating laboratories, however, the number of data and precision was too low to carry out a certification process. The reference material may be used for quality management of analytical laboratories engaged in the high-sensitive analysis of radionuclides in the construction materials of detectors placed in ultra low background underground laboratories.

  20. Characterization of Perchlorate in a New Frozen Human Urine Standard Reference Material

    Science.gov (United States)

    Yu, Lee L.; Jarrett, Jeffery M.; Davis, W. Clay; Kilpatrick, Eric L.; Oflaz, Rabia; Turk, Gregory C.; Leber, Dennis D.; Valentin, Liza; Morel-Espinosa, Maria; Blount, Benjamin C.

    2015-01-01

    Perchlorate, an inorganic anion, has recently been recognized as an environmental contaminant by the U.S. Environmental Protection Agency (EPA). Urine is the preferred matrix for assessment of human exposure to perchlorate. Although the measurement technique for perchlorate in urine was developed in 2005, the calibration and quality assurance aspects of the metrology infrastructure for perchlorate are still lacking in that there is no certified reference material (CRM) traceable to the International System of Units (SI). To meet the quality assurance needs in biomonitoring measurements of perchlorate and the related anions that affect thyroid health, the National Institute of Standards and Technology (NIST) in collaboration with the Centers for Disease Control and Prevention (CDC) developed Standard Reference Material (SRM) 3668 Mercury, Perchlorate, and Iodide in Frozen Human Urine. SRM 3668 consists of perchlorate, nitrate, thiocyanate, iodine, and mercury in urine at two levels that represent the 50th and 95th percentiles, respectively, of the concentrations (with some adjustments) in the U.S. population. It is the first CRM being certified for perchlorate. Measurements leading to the certification of perchlorate were made collaboratively at NIST and CDC using three methods based on liquid or ion chromatography tandem mass spectrometry (LC-MS/MS or IC-MS/MS). Potential sources of bias were analyzed and results were compared for the three methods. Perchlorate in SRM 3668 Level I urine was certified to be 2.70 μg L−1 ± 0.21 μg L−1, and for SRM 3668 Level II urine, the certified value is 13.47 μg L−1 ± 0.96 μg L−1. PMID:22850897

  1. 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)

    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)

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

    International Nuclear Information System (INIS)

    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)

  3. 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)

  4. Report on the intercomparison run and certified reference material IAEA-381. Radionuclides in Irish sea water

    International Nuclear Information System (INIS)

    The accurate and precise determinations of radionuclide concentrations in marine samples are important aspects of marine radioactivity assessments and the use of radionuclides in studies of oceanographic processes. To address the problem of data quality, the IAEA Marine Environment Laboratory (MEL) in Monaco has conducted intercomparison exercises on radionuclides in marine samples for many years as part of its contribution to the IAEA's programme of Analytical Quality Control Services (AQCS). For this intercomparison exercise, the Federal Maritime and Hydrographic Agency, Hamburg, Germany (BSH) collected sea water from the Irish Sea in 1993. IAEA-MEL distributed sample aliquots during 1995-1996 for intercomparison of anthropogenic and natural radionuclides. About 80 laboratories world-wide were approached with a questionnaire for participation. Of these, only 43 accepted the invitation because of financial constraints (the participating laboratories were asked to pay transportation expenses). As the sample was collected in the Irish Sea, elevated levels of anthropogenic radionuclides were expected due to discharges from the Sellafield reprocessing plant. Participants were informed that the expected activities for anthropogenic radionuclides would be in the ranges: 90Sr: 50-500 Bq/kg, 137Cs: 100-1000 Bq/kg, 239+240Pu: 1-50Bq/kg, 241Am: 1-50Bq/kg. This report describes the results obtained from 28 laboratories on anthropogenic and natural radionuclide determinations in sea water

  5. Anorganic fluorescence reference materials for decay time of fluorescence emission

    Science.gov (United States)

    Engel, A.; Ottermann, C.; Klahn, J.; Korb, T.; Resch-Genger, U.; Hoffmann, K.; Kynast, U.; Rupertus, V.

    2008-02-01

    Fluorescence techniques are known for their high sensitivity and are widely used as analytical tools, detection methods and imaging applications for product and process control, material sciences, environmental and bio-technical analysis, molecular genetics, cell biology, medical diagnostics, and drug screening. According to DIN/ISO 17025 certified standards are used for steady state fluorescence diagnostics, a method having the drawback of giving relative values for fluorescence intensities only. Therefore reference materials for a quantitative characterization have to be related directly to the materials under investigation. In order to evaluate these figures it is necessary to calculate absolute numbers such as absorption/excitation cross sections and quantum yield. This has been done for different types of dopands in different materials such as glass, glass ceramics, crystals or nano crystalline material embedded in polymer matrices. Samples doped with several fluophores of different emission wavelengths and decay times are required for fluorescent multiplexing applications. Decay times shorter than 100 ns are of special interest. In addition, a proper knowledge is necessary of quantum efficiency in highly scattering media. Recently, quantum efficiency in YAG:Ce glass ceramics has been successfully investigated. Glass and glass ceramics doped with threefold charged rare earth elements are available. However, these samples have the disadvantage of emission decay times much longer than 1 microsecond, due to the excitation and emission of their optical forbidden electronic transitions. Therefore first attempts have been made to produce decay-time standards based on organic and inorganic fluophores. Stable LUMOGEN RED pigments and YAG:Ce phosphors are diluted simultaneously in silicone matrices using a wide range of concentrations between 0.0001 and 2 wt%. Organic LUMOGEN RED has decay times in the lower nanosecond range with a slight dependency on concentration

  6. An outline of reference materials for analysis techniques in China

    International Nuclear Information System (INIS)

    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. Preparation of natural standard reference material (SRM) for El-lajjun oil shale/Jordan

    International Nuclear Information System (INIS)

    The standard reference materials (SR Ms) represent a key tool for the quality co trol of chemical of analysis and the demand on these materials is constantly increasing word wide. A standard reference material of oil shale (SJL-1) collected from El-lajjun area in Jordan was prepared and certified to be used for quality control of ana lyes and calibration particulary for the oil shale characterization and testing laboratories. The work was a part of the Arab collaborative projects initiated by Arab Atomic Energy Agency (AAEA) during the period from 2007 to 2009.The paper describes the certification procedure and the inter-laboratory comparison study results, which was carried out through participation of twelve national and international laboroatories applying eleven different analytical techniques used to determine the analytes concentraction. Details of the production, homogeneity and stability of SJL-1 standard refernce material were reviewed as well as the results of certification. The Certificate of Analysis for SJL-1 provides assigned certified values for almnuium oxide, phosphorus pentoxide, calcium oxide, titanium dioxide magnesium oxide, potassium oxide, ferric oxide, sodium oxide, manganese oxide, sulfur, uranium, vanadium, chromium, zinc, niclel, copper, and strontium Refernce values are provided for Loss on Ignition (LOI),silicon oxide, cadmium, molybdenum, cobalt, lead, barium and arsenic. Finally, range values are assigned for other thirty-seven constituents of oil shale. (authors).

  8. Production of artifact methylmercury during the analysis of certified reference sediments: Use of ionic exchange in the sample treatment step to minimise the problem

    International Nuclear Information System (INIS)

    Production of artifact methylmercury (MeHg+) during the analysis of two certified reference sediments, CRM-580 and IAEA-405, was investigated. Leaching of the analyte from the solid sample was achieved by ultrasound assisted acidic extraction. The aqueous leachate was either ethylated (NaBEt4) or phenylated (NaBPh4) using acetic/acetate or citric/citrate to buffer the solution. Preconcentration of the volatile compounds was carried out by extraction with an organic solvent (n-hexane) or solid phase microextraction (SPME). MeHg+ was finally separated and detected by gas chromatography with atomic emission or mass spectrometry detection (GC-MIP-AED or GC-MS). In all the cases the concentrations obtained for MeHg+ in the CRM-580 were significantly higher than the certified value. For the IAEA-405, however, the MeHg+ concentration found was always statistically indistinguishable from the certified value. Experiments were also conducted with synthetic samples, such as aqueous mixtures of MeHg+ and inorganic mercury (Hg2+) or silica-gel spiked with both compounds. The methylation rates found (defined as the percentage of Hg2+ present in the sample which methylates to give artifact MeHg+) ranged from not observable (in certain synthetic aqueous mixtures) to 0.57% (analysis of CRM-580 under certain conditions). As the amount of Hg2+ available in the sample seems to be the main factor controlling the magnitude of the artifact, several experiments were conducted using an ionic exchange resin (Dowex M-41) in order to minimise the concentration of this chemical in the reaction medium. First, a hydrochloric leachate of the sample was passed through a microcolumn packed with the exchanger. Second, the resin was mixed with the sample prior to extraction with HCl. In both cases, the predominant Hg2+ species, HgCl42-, was adsorbed on the resin, whereas MeHg+, mainly as MeHgCl, remained in solution. Following the second option, a new method to analyse MeHg+ in conflictive matrices

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

    International Nuclear Information System (INIS)

    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

  10. Preparation and certification of the Polish reference material Virginia Tobacco Leaves (CTA-VTL-2) for inorganic trace analysis including microanalysis

    International Nuclear Information System (INIS)

    A new Polish certified reference material Virginia Tobacco Leaves (CTA-VTL-2) for inorganic trace analysis including microanalysis has been prepared. Certification of the candidate reference material was based on the world-wide interlaboratory comparison in which 60 laboratories from 18 countries, participated using various analytical methods and techniques. Data evaluation performed by means of the new multifunctional software package -SSQC. Recommended values were assigned for 33 and 'information' values for 10 elements, respectively. The validity of 'certified' values was confirmed for several elements using 'very accurate' methods developed in this Laboratory. (author)

  11. Preparation and certification of the Polish reference material Virginia Tobacco Leaves (CTA-VTL-2) for inorganic trace analysis including microanalysis

    Energy Technology Data Exchange (ETDEWEB)

    Dybczynski, R.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z.

    1997-12-31

    A new Polish certified reference material Virginia Tobacco Leaves (CTA-VTL-2) for inorganic trace analysis including microanalysis has been prepared. Certification of the candidate reference material was based on the world-wide interlaboratory comparison in which 60 laboratories from 18 countries, participated using various analytical methods and techniques. Data evaluation performed by means of the new multifunctional software package -SSQC. Recommended values were assigned for 33 and `information` values for 10 elements, respectively. The validity of `certified` values was confirmed for several elements using `very accurate` methods developed in this Laboratory. (author). 47 refs, 28 figs, 12 tabs.

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

    International Nuclear Information System (INIS)

    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)

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

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Edson G.; Vasconcellos, Marina B.A., E-mail: emoreira@ipen.b, E-mail: mbvascon@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro do Reator de Pesquisas; Santos, Rafaela G. dos; Martinelli, Jose R., E-mail: jroberto@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencias e Tecnologia de Materiais

    2011-07-01

    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 {mu} = 94.6 {+-} 0.8 {mu}m. (author)

  14. 40 CFR 90.7 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be inspected at U.S. EPA Air and Radiation... 19103. Document number and name 40 CFR part 90 reference ASTM D86-93: Standard Test Method for...., Warrendale, PA 15096-0001. Document number and name 40 CFR part 90 reference SAE J1930 September...

  15. Development of Reference Materials for Thermal-Diffusivity Measurements by the Flash Method

    Science.gov (United States)

    Akoshima, M.; Abe, H.; Baba, T.

    2015-12-01

    The thermal conductivity of solid materials used for thermal simulations and thermal designs can be obtained as the product of thermal diffusivity, specific heat capacity, and bulk density in many cases. The thermal diffusivity is usually measured by the flash method, and the specific heat capacity is usually measured by differential scanning calorimetry. In order to obtain reliable thermal conductivities for strict thermal design, it is necessary to measure the thermal diffusivity using the flash method, a well-validated apparatus. Reference materials are an effective means for validation of most practical measurement apparatus. For the flash method, isotropic graphite was selected as a candidate reference material. A batch of isotropic graphite samples was prepared and characterized in detail in order to be a certified reference material for thermal-diffusivity measurement. The detailed characterization ensures the traceability of the measurement results to the international system of units (SI). A convenient reference material for thermal conductivity was also obtained by using the known thermal-diffusivity measurements, specific heat capacity, and density of the material.

  16. Determination of trace elements in NIES environmental reference materials by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Concentrations of trace elements in environmental reference materials prepared by the National Institute for Environmental Studies of Japan (NIES) were determined by instrumental neutron activation analysis (INAA). Mussel, Human Hair, Tea Leaves and Sargasso reference material samples (ca. 150∼1200 mg) were irradiated by thermal neutron without cadmium filter and epithermal neutron with cadmium filter at Musashi Institute of Technology Research Reactor (MITRR). The activated samples were measured by three methods; conventional γ-ray spectrometry using a coaxial Ge detector, anticoincidence counting spectrometry and coincidence counting spectrometry. The γ-ray spectrometric system (GAMA system) was developed by the authors. As a result, they could determined about 30 - 50 elements by the combination of these irradiation and counting methods. The analyzed values were in good agreement with NIES certified values

  17. Prompt gamma activation analysis of boron in reference materials using diffracted polychromatic neutron beam

    International Nuclear Information System (INIS)

    Boron concentrations were analyzed for standard reference materials by prompt gamma activation analysis (PGAA). The measurements were performed at the SNU-KAERI PGAA facility installed at Hanaro, the research reactor of Korea Atomic Energy Research Institute (KAERI). The facility uses a diffracted polychromatic beam with a neutron flux of 7.9 x 107 n/cm2 s. Elemental sensitivity for boron was calibrated from the prompt gamma-ray spectra of boric acid samples containing 2-45 μg boron. The sensitivity of 2131 cps/mg-B was obtained from the linearity of the boron peak count rate versus the boron mass. The detection limit for boron was estimated to be 67 ng from an empty sample bag spectrum for a counting time of 10,000 s. The measured boron concentrations for standard reference materials showed good consistency with the certified or information values

  18. Multielement analysis of environmental reference materials by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Concentrations of trace elements in environmental reference materials prepared by the National Institute for Environmental Studies, Japan (NIES) and by the National Institute of Standards and Technology, USA (NIST) were determined by instrumental neutron activation analysis (INAA). NIES CRM No. 5 Human Hair, No. 6 Mussel, No. 7 Tea Leaves, No. 8 Vehicle Exhaust Particulates, No. 9 Sargasso and No. 10 Rice Flour-unpolished samples (ca. 150 - 1200 mg) and NIST SRM 1632a Bituminous Coal, SRM 1635 Sub-bituminous Coal and SRM 1633a Coal Fly Ash samples (ca. 10 - 150 mg) were irradiated at the Musashi Institute of Technology Research Reactor (MITRR). Concentrations of 28 - 52 elements in these NIES and NIST environmental reference materials were determined by two irradiation methods and four γ-ray counting methods. The determined values were in good agreement with the NIES and NIST certified values. (author)

  19. Prompt gamma activation analysis of boron in reference materials using diffracted polychromatic neutron beam

    Science.gov (United States)

    Byun, S. H.; Sun, G. M.; Choi, H. D.

    2004-01-01

    Boron concentrations were analyzed for standard reference materials by prompt gamma activation analysis (PGAA). The measurements were performed at the SNU-KAERI PGAA facility installed at Hanaro, the research reactor of Korea Atomic Energy Research Institute (KAERI). The facility uses a diffracted polychromatic beam with a neutron flux of 7.9 × 10 7 n/cm 2 s. Elemental sensitivity for boron was calibrated from the prompt gamma-ray spectra of boric acid samples containing 2-45 μg boron. The sensitivity of 2131 cps/mg-B was obtained from the linearity of the boron peak count rate versus the boron mass. The detection limit for boron was estimated to be 67 ng from an empty sample bag spectrum for a counting time of 10,000 s. The measured boron concentrations for standard reference materials showed good consistency with the certified or information values.

  20. Caracterização detalhada de material de referência certificado de carvão brasileiro

    OpenAIRE

    Vera L. V. Fallavena; Cristiane S. de Abreu; Taísi D. Inácio; Marçal Pires; Carla M. N. Azevedo; Iolanda D. Fernandes; Lizete S. Ferret; M. Rosa Martinez Tarazona

    2013-01-01

    The use and characterization of the first Certified Reference Material (CRM) of Brazilian coal for analytical quality control are presented. All results were determined within the limits of repeatability and reproducibility allowed under the standards. Notable among the characterization parameters was the mineral matter content (45.39%) obtained by an alternative procedure showing a low relative error (-2.1%) compared to the standard technique (low ashing temperature). The possible expanded a...

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

    International Nuclear Information System (INIS)

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

    International Nuclear Information System (INIS)

    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 1013 n/cm2 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

  3. Reproducibility of polycarbonate reference material in toxicity evaluation

    Science.gov (United States)

    Hilado, C. J.; Huttlinger, P. A.

    1981-01-01

    A specific lot of bisphenol A polycarbonate has been used for almost four years as the reference material for the NASA-USF-PSC toxicity screening test method. The reproducibility of the test results over this period of time indicate that certain plastics may be more suitable reference materials than the more traditional cellulosic materials.

  4. Recent production of candidate reference materials at IRMM

    Energy Technology Data Exchange (ETDEWEB)

    Kramer, G.N.; Pauwels, J.; Le Guern, L.; Schimmel, H.; Trapmann, S. [Commission of the European Communities, Geel (Belgium). Joint Research Centre

    2001-06-01

    In the execution of its mission to promote a common European measurement system in support of EU policies, IRMM's Reference Materials Unit is currently involved in preparation of proficiency-testing samples and candidate reference materials. Recent work related to bovine spongiform encephalopathy in cows, genetically modified organisms, and a variety of environmental materials is described. (orig.)

  5. 40 CFR 89.6 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... 19428-2959. Document number and name 40 CFR part 89 reference ASTM D86-97: “Standard Test Method for... 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be inspected at US EPA, OAR, 1200 Pennsylvania Ave... D287-92: “Standard Test Method for API Gravity of Crude Petroleum and Petroleum Products”...

  6. 40 CFR 1065.1010 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... 2001), Standard Test Method for Air Cleaning Performance of a High-Efficiency Particulate Air Filter... Specification for Automotive Spark-Ignition Engine Fuel 1065.701 ASTM D5186-03, Standard Test Method for... Federal Register approved the incorporation by reference as prescribed in 5 U.S.C. 552(a) and 1 CFR...

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

    International Nuclear Information System (INIS)

    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, HE, and of a minimum sample mass M5% 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)

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

    International Nuclear Information System (INIS)

    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)

  9. Corrosion reference for geothermal downhole materials selection

    Energy Technology Data Exchange (ETDEWEB)

    Ellis, P.F. II, Smith, C.C.; Keeney, R.C.; Kirk, D.K.; Conover, M.F.

    1983-03-01

    Geothermal downhole conditions that may affect the performance and reliability of selected materials and components used in the drilling, completion, logging, and production of geothermal wells are reviewed. The results of specific research and development efforts aimed at improvement of materials and components for downhole contact with the hostile physicochemical conditions of the geothermal reservoir are discussed. Materials and components covered are tubular goods, stainless steels and non-ferrous metals for high-temperature downhole service, cements for high-temperature geothermal wells, high-temperature elastomers, drilling and completion tools, logging tools, and downhole pumps. (MHR)

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

    International Nuclear Information System (INIS)

    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)

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

    International Nuclear Information System (INIS)

    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.

  12. 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)

    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)

  13. The advantages of using standardized review procedures in certifying type B radioactive material packages

    International Nuclear Information System (INIS)

    This paper presents the advantages of adopting well-documented standardized review practices for reviewing Type B package designs. The US experience using standardized review plans and guidance has shown them to be a valuable tool in achieving more consistent and efficient package reviews, in training and qualifying technical reviewers, and in enhancing public and industry understanding of the package certification process. In addition, the standardized review practices, as living documents, have proven to be an effective method of incorporating new technical advances into the review process, and have provided a vehicle to make that knowledge widely available to fellow reviewers, the public and industry. Canada implemented a new internal review process in early 2003 to standardize the review of applications for certification of Type B Packages. Based on the similarity of these approaches, the United States and Canada have started discussions on a A North American System for the unilateral approval of Type B (U) packages. This initiative is looking into how each country is currently reviewing transportation package applications to see if agreement can be reached on accepting Type B certifications on a reciprocal basis, i.e., without additional review. Based on the experience in Canada and the United States, the authors believe that the use of standardized review processes, coupled with the knowledge and experience resident in IAEA's Transportation Advisory Material (TS-G-1.1) and series of TECDOCS, could also be used to develop a standard internationally accepted review process that could enhance the acceptance of unilateral approvals for Type B packages

  14. Implementation of Certified EHR, Patient Portal, and "Direct" Messaging Technology in a Radiology Environment Enhances Communication of Radiology Results to Both Referring Physicians and Patients.

    Science.gov (United States)

    Reicher, Joshua Jay; Reicher, Murray Aaron

    2016-06-01

    Since 2009, the Federal government distributed over $29 billion to providers who were adopting compliant electronic health record (EHR) technology. With a focus on radiology, we explore how EHR technology impacts interoperability with referring clinicians' EHRs and patient engagement. We also discuss the high-level details of contributing supporting frameworks, specifically Direct messaging and health information service provider (HISP) technology. We characterized Direct messaging, a secure e-mail-like protocol built to allow exchange of encrypted health information online, and the new supporting HISP infrastructure. Statistics related to both the testing and active use of this framework were obtained from DirectTrust.org, an organization whose framework supports Direct messaging use by healthcare organizations. To evaluate patient engagement, we obtained usage data from a radiology-centric patient portal between 2014 and 2015, which in some cases included access to radiology reports. Statistics from 2013 to 2015 showed a rise in issued secure Direct addresses from 8724 to 752,496; a rise in the number of participating healthcare organizations from 667 to 39,751; and a rise in the secure messages sent from 122,842 to 27,316,438. Regarding patient engagement, an average of 234,679 patients per month were provided portal access, with 86,400 patients per month given access to radiology reports. Availability of radiology reports online was strongly associated with increased system usage, with a likelihood ratio of 2.63. The use of certified EHR technology and Direct messaging in the practice of radiology allows for the communication of patient information and radiology results with referring clinicians and increases patient use of patient portal technology, supporting bidirectional radiologist-patient communication. PMID:26588906

  15. Preparation and characterization of a Perna perna (Linnaeus, 1758) mussel reference material; Preparo e caracterizacao de um material de referencia de mexilhao Perna perna (Linnaeus, 1758)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Edson Goncalves

    2010-07-01

    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{sup -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)

  16. Standard and reference materials for marine science, revised edition, 1993

    OpenAIRE

    IOC for UNESCO

    1993-01-01

    This is 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 o...

  17. [Review of normal spectral emissivity standard reference materials].

    Science.gov (United States)

    Yu, Kun; Liu, Yu-Fang; Zhao, Yue-Jin

    2012-11-01

    In order to improve the accuracy of spectral emissivity measurement, standard reference materials of spectral emissivity as the dissemination of quantity in spectral emissivity measurement are used for the calibration of spectral emissivity measurement apparatus. In the present paper, firstly the standard reference materials data proposed by the American National Institute of Standards and Technology are introduced, and some underlying standard reference materials suggested by some metering departments in Europe are analyzed in detail For the standard reference material Armco iron and SiC proposed by some researchers, the advantages and disadvantages were explored. Finally, the characteristics of standard reference materials are summarized, and the future development of spectral emissivity measurement standard is prospected. PMID:23387148

  18. Phosphated minerals to be used as radioactive reference materials; Minerais fosfatados para serem utilizados como materiais de referencia radioativos

    Energy Technology Data Exchange (ETDEWEB)

    Braganca, M.J.C.S.; Tauhata, L. [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil). Lab. Nacional de Metrologia das Radiacoes Ionizantes (LNMRI); Clain, A.F. [Universidade Severino Sombra, Vassouras, RJ (Brazil); Moreira, I. [Pontificia Univ. Catolica do Rio de Janeiro (PUC/Rio), RJ (Brazil). Dept. de Quimica

    2003-07-01

    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.

  19. A new reference material for radionuclides in the mussel sample from the Mediterranean Sea (IAEA-437)

    International Nuclear Information System (INIS)

    A new Reference Material (RM) for radionuclides in mussel (Mytilus galloprovincialis) from the Mediterranean Sea (IAEA-437) is described and the results of the certification process are presented. Four radionuclides (40K, 234U, 238U, and 239+240Pu) have been certified, and information values on massic activities with 95% confidence intervals are given for nine radionuclides (137Cs, 210Pb(210Po), 226Ra, 228Ra, 228Th, 230Th, 232Th, 235U, and 241Am). Results for less frequently reported radionuclides (90Sr, 129I, 238Pu, 239Pu, and 240Pu) are also reported. The RM can be used for quality assurance/quality control of the analysis of radionuclides in mussel samples, for the development and validation of analytical methods and for training purposes. The material is available in 200 g units. (author)

  20. Caracterização detalhada de material de referência certificado de carvão brasileiro

    Directory of Open Access Journals (Sweden)

    Vera L. V. Fallavena

    2013-01-01

    Full Text Available The use and characterization of the first Certified Reference Material (CRM of Brazilian coal for analytical quality control are presented. All results were determined within the limits of repeatability and reproducibility allowed under the standards. Notable among the characterization parameters was the mineral matter content (45.39% obtained by an alternative procedure showing a low relative error (-2.1% compared to the standard technique (low ashing temperature. The possible expanded application of this CRM application in national laboratories, beyond the certificated and reference parameters, has advantages such as lower cost and easy availability, but round robin tests must be performed.

  1. Quantification of the predominant monomeric catechins in baking chocolate standard reference material by LC/APCI-MS.

    Science.gov (United States)

    Nelson, Bryant C; Sharpless, Katherine E

    2003-01-29

    Catechins are polyphenolic plant compounds (flavonoids) that may offer significant health benefits to humans. These benefits stem largely from their anticarcinogenic, antioxidant, and antimutagenic properties. Recent epidemiological studies suggest that the consumption of flavonoid-containing foods is associated with reduced risk of cardiovascular disease. Chocolate is a natural cocoa bean-based product that reportedly contains high levels of monomeric, oligomeric, and polymeric catechins. We have applied solid-liquid extraction and liquid chromatography coupled with atmospheric pressure chemical ionization-mass spectrometry to the identification and determination of the predominant monomeric catechins, (+)-catechin and (-)-epicatechin, in a baking chocolate Standard Reference Material (NIST Standard Reference Material 2384). (+)-Catechin and (-)-epicatechin are detected and quantified in chocolate extracts on the basis of selected-ion monitoring of their protonated [M + H](+) molecular ions. Tryptophan methyl ester is used as an internal standard. The developed method has the capacity to accurately quantify as little as 0.1 microg/mL (0.01 mg of catechin/g of chocolate) of either catechin in chocolate extracts, and the method has additionally been used to certify (+)-catechin and (-)-epicatechin levels in the baking chocolate Standard Reference Material. This is the first reported use of liquid chromatography/mass spectrometry for the quantitative determination of monomeric catechins in chocolate and the only report certifying monomeric catechin levels in a food-based Standard Reference Material. PMID:12537419

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

    International Nuclear Information System (INIS)

    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)

  3. Preparation of reference material for the measurement of natural radioactivity

    International Nuclear Information System (INIS)

    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.

  4. Study of reference material for NMR core analysis

    International Nuclear Information System (INIS)

    Reference Materials of NMR core experimental analysis have been studied systematically in this paper. According to the national standard criterion, a set of NMR reference materials have been made successfully. These reference materials include fluid pattern-D2O and H2O, divergence of glass grain muster, and the solid ceramics. They have been applied to the core analysis in Daqing, Xinjiang, Dagang Oilfield, etc. The results show, fluid pattern, divergence of glass grain muster as well as ceramics reference materials have different calibration results of core NMR porosity as a result of their different relaxation mechanisms. Fluid pattern is suitable for NMR porosity calibration in Berea sandstone as well as terrestrial sediment sand with little shale content and well sorted. Ceramics reference material is applied to shaly sand with average sorted. Both fluid pattern and solid ceramics material are not suitable for calibration in sandstone sample with high clay content, complex lithology with rich paramagnetic materials. It is suggested that the representative natural core sample should be selected as regional reference material to calibrate NMR porosity of complex lithology, or internal magnetic field gradient in complex rock grain/fluid system should be studied in order to get corrected NMR porosity. (authors)

  5. Standard guide for preparation of working reference materials for use in analysis of nuclear fuel cycle materials

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2001-01-01

    1.1 This guide covers the preparation and characterization of working reference materials (WRM) that are produced by a laboratory for its own use in the analysis of nuclear materials. Guidance is provided for establishing traceability of WRMs to certified reference materials by a defined characterization process. The guidance provided is generic; it is not specific for a given material. 1.2 The information provided by this guide is found in the following sections: Section Planning 6 Preparation 7 Packaging and Storage 8 Characterization 9 Statistical Analysis 10 Documentation 11 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  6. The IAEA's analytical quality control services (AQCS) programme on intercomparison runs and references materials

    International Nuclear Information System (INIS)

    For more than 30 years the IAEA has been operating a programme of Analytical Quality Control Services (AQCS) concerned mainly with intercomparison and reference materials (RMs) for radionuclides, trace elements and pesticide residues. Through this programme the IAEA has established itself as a worldwide centre for analytical quality assurance which assists its Member States to maintain and improve the quality of analytical data obtained in their laboratories. The large number of participants in IAEA AQCS intercomparison runs and extensive use of IAEA AQCS RMs in laboratories around the world testify to the importance of this programme. However, demands on the level of confidence for certified values are continuously increasing. They are clearly stated in the recently published ISO Guide 34 'Quality System Guidelines for the Production of Reference Materials'. The main aim in the paper is to describe the present procedures of the IAEA AQCS concerning the production of RMs, with special reference to materials of environmental interest, and to compare them with is the latest requirements mentioned above. (author)

  7. The development of the first set of Brazilian reference materials for the petroleum sector; O desenvolvimento dos primeiros materiais de referencia nacionais para o setor de petroleo

    Energy Technology Data Exchange (ETDEWEB)

    Zucchini, Ricardo R. [Instituto de Pesquisas Tecnologicas (IPT), Sao Paulo, SP (Brazil). Agrupamento de Materiais de Referencia

    2004-07-01

    The petroleum sector uses a number of standardized tests to characterize raw materials and products. The development of in-company programs for assurance of measurement quality, the increasing need to demonstrate proficiency by means of certification schemes or by widely accepted metrological practices, have been promoting a more intensive use of certified reference materials, in calibration as well as in validation of measurement methods and also in order to show the qualification of the laboratories. In this paper it is presented the preparation, performed by IPT's Reference Materials Group, of the first set of reference materials specially developed considering the needs of the petroleum community. Briefly, are presented the identification of the demands from the users, selection of matrices, homogeneity tests and stability studies, and the certification of the new reference materials, which are four diesel fuel oils with certified sulfur contents and one material with flash point certified by TAG and Pensky-Martens methods. It is presented a summary of the certification process, performed by means of a combined effort of several professionals that are now working at laboratories of research institutions, refineries and other industries, universities, fuel monitoring facilities and in National Petroleum Agency. (author)

  8. olive leaves as standard reference material for elemental analysis

    International Nuclear Information System (INIS)

    there is no local standard reference materials which can express the local elemental matrix of plants, therefore, olive leaves is selected to be a standard reference material, young olive leaves was collected from atomic energy authority farm ( inshas area). the sample was prepared by washing,drying grinding and divided into bottles and distributed to different laboratories for analysis . this sample is intended to be used as a reference material for the measurement of major, minor and trace elements in botanical materials, agricultural food products and materials of similar matrix. it can also be used as a quality control material for the assessment of a laboratory's analytical work, for the validation of analytical methods and for quality assurance within a laboratory

  9. Determination of boron in ceramic reference materials by prompt gamma activation analysis using focused neutron guided beam of JRR-3M

    International Nuclear Information System (INIS)

    Prompt gamma activation analysis using a focused thermal neutron guided beam at JAEA JRR-3M was applied to the determination of B in ceramic certified reference materials (BAM CRM S-003 Silicon Carbide Powder and NMIJ CRM 8004-a Silicon Nitride Powder). Cl and Si were used as internal standards to obtain linear calibration curves of B. The analytical result of B in BAM CRM S-003 was in good agreement with the certified value. The relative expanded measurement uncertainties (k = 2) were 4.8% for BAM CRM S-003 and 4.9% for NMIJ CRM 8004-a. (author)

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

    International Nuclear Information System (INIS)

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

  11. The development and evaluation of reference materials for food microbiology.

    NARCIS (Netherlands)

    in 't Veld, P.H.

    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 (SM&T). The RMs a

  12. Uranium Isotopic Ratio Measurements of U3O8 Reference Materials by Atom Probe Tomography

    Energy Technology Data Exchange (ETDEWEB)

    Fahey, Albert J.; Perea, Daniel E.; Bartrand, Jonah AG; Arey, Bruce W.; Thevuthasan, Suntharampillai

    2016-01-01

    We report results of measurements of isotopic ratios obtained with atom probe tomography on U3O8 reference materials certified for their isotopic abundances of uranium. The results show good agreement with the certified values. High backgrounds due to tails from adjacent peaks complicate the measurement of the integrated peak areas as well as the fact that only oxides of uranium appear in the spectrum, the most intense of which is doubly charged. In addition, lack of knowledge of other instrumental parameters, such as the dead time, may bias the results. Isotopic ratio measurements can be performed at the nanometer-scale with the expectation of sensible results. The abundance sensitivity and mass resolving power of the mass spectrometer are not sufficient to compete with magnetic-sector instruments but are not far from measurements made by ToF-SIMS of other isotopic systems. The agreement of the major isotope ratios is more than sufficient to distinguish most anthropogenic compositions from natural.

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

    International Nuclear Information System (INIS)

    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 dm3 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 oC. Short-term stability was examined by the determination of concentrations of the selected elements in the bottle stored in the CO2 incubator at 37 oC. 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 values

  14. Preparation and certification of the Polish reference material `Oriental Tobacco Leaves` (CTA-OTL-1) for inorganic trace analysis

    Energy Technology Data Exchange (ETDEWEB)

    Dybczynski, R.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z. [Institute of Nuclear Chemistry and Technology, Warsaw (Poland)

    1996-12-31

    A new Polish certified reference material `Oriental Tobacco Leaves` (CTA-OTL-1) for inorganic trace analysis was prepared. Fresh tobacco leaves of variety `Oriental` were dried, ground and sieved. All precautions were taken to avoid contamination of material with metals. The next step was homogenization. Preliminary homogeneity checking consisted in determining of Ca, Fe and K content by X-ray fluorescence. Final homogeneity testing was performed by neutron activation analysis determining Co, Cr, Fe and Rb. To assure long-term stability, the whole lot of material was sterilized by electron beam radiation. Certification of the candidate reference material was done on the basis of world-wide interlaboratory comparisons exercise in which 61 laboratories, using various analytical methods participated. (author). 30 refs, 12 tabs, 21 figs.

  15. Preparation and certification of the Polish reference material 'Oriental Tobacco Leaves' (CTA-OTL-1) for inorganic trace analysis

    International Nuclear Information System (INIS)

    A new Polish certified reference material 'Oriental Tobacco Leaves' (CTA-OTL-1) for inorganic trace analysis was prepared. Fresh tobacco leaves of variety 'Oriental' were dried, ground and sieved. All precautions were taken to avoid contamination of material with metals. The next step was homogenization. Preliminary homogeneity checking consisted in determining of Ca, Fe and K content by X-ray fluorescence. Final homogeneity testing was performed by neutron activation analysis determining Co, Cr, Fe and Rb. To assure long-term stability, the whole lot of material was sterilized by electron beam radiation. Certification of the candidate reference material was done on the basis of world-wide interlaboratory comparisons exercise in which 61 laboratories, using various analytical methods participated. (author). 30 refs, 12 tabs, 21 figs

  16. Evaluation of a reference material for glycated haemoglobin

    NARCIS (Netherlands)

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

    1996-01-01

    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

  17. [Preparation and certification of mussel reference material for organochlorine pesticides and polychlorinated biphenyls using isotope dilution-high resolution mass spectrometry].

    Science.gov (United States)

    Lu, Xianbo; Chen, Jiping; Wang, Shuqiu; Zou, Lili; Tian, Yuzeng; Ni, Yuwen; Su, Fan

    2012-09-01

    A method for the preparation and certification of the reference material of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in mussel tissue is described. The mussel tissue from Dalian Bay was frozen-dried, comminuted, sieved, homogenized, packaged, and sterilized by 60Co radiation sterilization in turn. The certified values for 18 OCPs and 16 PCBs were determined by high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) using isotope dilution and internal standard quantitation techniques. The certified values were validated and given based on seven accredited laboratories, and these values are traceable to the SI (international system of units) through gravimetrically prepared standards of established purity and measurement intercomparisons. The certified values of PCBs and OCPs in mussel span 4 orders of magnitude with a relative uncertainty of about 10%. This material is a natural biological material with confirmed good homogeneity and stability, and it was approved as the grade "primary reference material" (GBW10069) in June 2012 in China. This reference material provided necessary quality control products for our country to implement the Stockholm Treaty on the monitoring of persistent organic pollutants (POPs). The material is intended to be used for the method validation and quality control in the determination of OCPs and PCBs in biota samples. PMID:23285973

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

    International Nuclear Information System (INIS)

    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)

  19. The preparation and certification of ten uranium reference materials

    International Nuclear Information System (INIS)

    This report describes the procedures involved in the preparation, analysis and certification of ten 'UREM' uranium-bearing materials for use as international reference materials. Recommended values for total U3O8 are assigned to all of the ten materials. Twenty-two laboratories from seven countries contributed a total of approximately 300 analytical results for each material. The analytical methods used were X-ray-fluorescence spectrometry, colorimetry, fluorimetry, neutron-activation analysis, and emission spectroscopy using an inductively coupled plasma source. Approximately 300 kg of each reference material was prepared, primarily for use by the South African uranium industry. However, a limited amount of each material is available for overseas laboratories

  20. The characterization of uranium and plutonium reference materials by the (100-X) route; basic principle and applications

    International Nuclear Information System (INIS)

    Uranium and plutonium reference materials are produced to calibrate reagents used in titrimetric methods or to check instrumental techniques like electrochemical methods. For this purpose, the most commonly prepared reference materials are high-purity uranium metal pieces and uranium dioxide pellets, respectively plutonium metal pieces and plutonium dioxide powders. Two different routes can be followed to certify the element content: a direct or an indirect route. With the direct route the main element is assayed using appropriate redox titration methods. The overall uncertainty on the main element is limited by both the precision of the titration methods used and the uncertainty of the reference materials. The indirect route is applicable only for high purity base material. It requires the measurement of the sum of impurities (X) in the material and the substraction of this sum from hundred per cent (100-X). Since the (100-X) route requires the measurement of a large number of elements, a variety of analytical methods has to be used, and a contribution by different specialized laboratories is requested. The uncertainty of the total of impurities is calculated from the respective uncertainties of the determination of each specific element. If the total of impurities is sufficiently small and even if it is determined with a rather large uncertainty, the (100-X) route leads nevertheless to a low uncertainty on the main element content. The application of the (100-X) route is illustrated for the case of uranium dioxide pellets certified as an European Community Nuclear Reference Material. The (100-X) route is recommended as a very accurate one for high purity material characterization and certification purposes

  1. 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

  2. Reference materials characterized for impurities in uranium matrices. An overview and re-evaluation of the NBL CRM 124 series

    International Nuclear Information System (INIS)

    The characterized concentrations of 24 impurity elements in New Brunswick Laboratory (NBL) Certified Reference Material (CRM) 124 were reevaluated. A provisional certificate of analysis was issued in September 1983 based upon the 'as prepared' values (gravimetric mixing). The provisional certificate does not state uncertainties for the characterized values, or estimate the degree of homogeneity. Since release of the provisional certificate of analysis various laboratories have reported analytical results for CRM 124. Based upon the reported data a re-evaluation of the characterized values with an estimate of their uncertainties was performed in this work. An assessment of the degree of homogeneity was included. The overall difference between the re-evaluated values for the 24 impurity elements and the 'as prepared' values from the provisional certificate of analysis is negligible compared to the uncertainties. Therefore, NBL will establish the 'as prepared' values as the certified values and use the derived uncertainties from this work for the uncertainties of the certified values. The traceability of the 'as prepared' values was established by the gravimetric mixing procedure employed during the preparation of the CRM. NBL further recommends a minimum sample size of 1 g of the CRM material to ensure homogeneity. Samples should be dried by heating up to 110 deg C for one hour before use. (author)

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

    International Nuclear Information System (INIS)

    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

  4. Certification of the reference material of water content in water saturated 1-octanol by Karl Fischer coulometry, Karl Fischer volumetry and quantitative nuclear magnetic resonance.

    Science.gov (United States)

    Wang, Haifeng; Ma, Kang; Zhang, Wei; Li, Jia; Sun, Guohua; Li, Hongmei

    2012-10-15

    Certified reference materials (CRMs) of water content are widely used in the calibration and validation of Karl Fischer coulometry and volumetry. In this study, the water content of the water saturated 1-octanol (WSO) CRM was certified by Karl Fischer coulometry, volumetry and quantitative nuclear magnetic resonance (Q NMR). The water content recovery by coulometry was 99.76% with a diaphragm-less electrode and Coulomat AG anolyte. The relative bias between the coulometry and volumetry results was 0.06%. In Q NMR, the water content of WSO is traceable to the International System (SI) of units through the purity of internal standard. The relative bias of water content in WSO between Q NMR and volumetry was 0.50%. The consistency of results for these three independent methods improves the accuracy of the certification of the RM. The certified water content of the WSO CRM was 4.76% with an expanded uncertainty of 0.09%. PMID:23442697

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

    International Nuclear Information System (INIS)

    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 204Pb/205Pb, 111Cd/114Cd and 66Zn/67Zn were determined in an atomic emission spectrometer with a plasma source with the following characteristics: plasma ionization

  6. Recent applications of nuclear analytical methods to the certification of elemental content in NIST standard reference materials

    International Nuclear Information System (INIS)

    Well-characterized, certified reference materials (CRMs) play an essential role in assuring the quality of analytical measurements. NIST has been producing CRMs, currently called NIST Standard Reference Materials (SRMs), to validate analytical measurements for nearly one hundred years. The predominant mode of certifying inorganic constituents in complex-matrix SRMs is through the use of two critically evaluated, independent analytical techniques at NIST. These techniques should have no significant sources of error in common. The use of nuclear analytical methods in combination with one of the chemically based analytical method at NIST eliminates the possibility of any significant, common error source. The inherent characteristics of the various forms of nuclear analytical methods make them extremely valuable for SRM certification. Instrumental NAA is nondestructive, which eliminates the possibility of any dissolution problems, and often provides homogeneity information. Radiochemical NAA typically provides nearly blank-free determinations of some highly important, but difficult elements at very low levels. Prompt-gamma NAA complements INAA, and provides independent determinations of some key elements. In addition, all significant uncertainty components can be evaluated for these techniques, and we believe these methods can meet all the requirements of a primary method of measurement as defined by ISO and the CCQM. NIST has certified several SRMs using INAA and RNAA as primary methods. In addition, NIST has compared measurements by INAA and PGAA with other primary methods as part of the CCQM intercomparisons of national metrology institutes. Some significant SRMs recently certified for inorganic constituents with contributions from the nuclear analytical methods include: Toxic Substances in Urine (SRM 2670a), Lake Superior Fish Tissue (SRM 1946), Air Particulate on Filter Media (SRM 2783), Inorganics in Marine Sediment (SRM 2702), Sediment for Solid Sampling (Small

  7. The development and evaluation of reference materials for food microbiology.

    OpenAIRE

    in 't Veld, P.H.

    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 (SM&T). The RMs are the result of efforts, which was started many years ago, to develop standardised samples that could be used in collaborative studies and in particular for the evaluation of methods for the detec...

  8. Particle size studies in the preparation of AQCS reference materials

    International Nuclear Information System (INIS)

    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)

  9. Preparation of reference materials for frit chemical analysis

    Energy Technology Data Exchange (ETDEWEB)

    Gazulla, M.F.; Gomez, M.P.; Barba, A.; Orduna, M. [Inst. de Tecnologia Ceramica, Univ. Jaume I., Castellon (Spain)

    2002-08-01

    A study was undertaken on how to prepare frit reference materials in which the following elements are analysed: Si, Al, Fe, Ca, Mg, N, K, Ti, Zr, Ba, Pb, Zn, Hf, P, B and Li. The following analytical techniques were used: X-ray fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrophotometry (AAS) and titrimetry. Boron and lithium were analysed by ICP-OES, sodium and lithium by AAS, and boron by titrimetry, while the remaining frit elements and sodium were analysed by XRF. The results found by the different methods were compared and each method was validated by means of reference materials. A procedure was established for preparing frit reference materials for calibrating and validating working methods on an industrial scale. (orig.)

  10. On criteria for examining analysis quality with standard reference material

    International Nuclear Information System (INIS)

    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

  11. Determination of arsenic in food and dietary supplement standard reference materials by neutron activation analysis

    International Nuclear Information System (INIS)

    Arsenic was measured in food and dietary supplement standard reference materials by neutron activation analysis for the purpose of assigning certified or reference As mass fractions and to assess material homogeneity. Instrumental neutron activation analysis was used to value assign As in candidate SRM 3532 Calcium Dietary Supplement and candidate SRM 3262 Hypericum perforatum (St. John's Wort) Aerial Parts down to about 100 μg/kg. Values were also determined for two additional candidate St. John's Wort SRMs with As mass fractions 24Na and 82Br limited the reproducibility of the method below 100 μg/kg. For measurement of lower As mass fractions, a radiochemical neutron activation analysis method with extraction of As3+ into diethyl-dithiocarbamate in chloroform and detection limits down to 0.1 μg/kg. As was used to value-assign As mass fractions for SRM 3280 Multivitamin/Multielement Tablets and for candidate SRM 3233 Fortified Breakfast Cereal, and at <10 μg/kg in candidate SRM 1845a Whole Egg Powder. (author)

  12. Determination of copper, molybdenum and selenium in biological reference materials by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    In a contribution to the elemental characterization of 10 new reference materials, Bovine Muscle Powder (136), Corn Starch (162), Hard Red Spring Wheat Flour (165), Soft Winter Wheat Flour (166), Whole Milk Powder (183), Wheat Gluten (184), Corn Bran (186). Durum Wheat Flour (187), Whole Egg Powder (188) and Microcrystalline Cellulose (189), the total concentrations of Cu, Mo and Se were determined by the application of an analytical method based on isotope dilution inductively coupled plasma mass spectrometry. Cu and Mo contents were quantified by measurement of 65Cu/63Cu and 97Mo/100Mo isotopic ratios following spiking with 65Cu and 97Mo and digestion with nitric acid. Selenium was separated as hydrogen selenide from the matrix using sodium borohydride after spiking with 82Se and acid digestion-dry ashing and quantified by measurement of the 82Se/78Se isotopic ratio. Comparison of these results with those from a variety of other methods and assessment of the procedures using certified reference materials indicated that the determinations of Cu, Mo and Se were performed without analytical bias. (orig.)

  13. Reference materials for microanalytical nuclear techniques. Final report of a co-ordinated research project 1994-1999

    International Nuclear Information System (INIS)

    A significant problem in the use of solid- and small-sample techniques is a general lack in suitable certified reference materials (CRM). Essentially, no CRM are certified for the small sample sizes typically used. Direct utilization of most existing CRM in solid sampling analysis procedures, typically 1 mg sample size, is often difficult or even impossible because trace components may not be sufficiently homogeneously distributed in the sample or their homogeneous distribution has not been tested. To explore the production, characterization and use of CRM for determinations with sample sizes much smaller than currently used, the Coordinated Research Program focused on selection of biological and environmental materials suitable for microanalytical techniques, definition of specifications for suitable CRM, evaluation of existing CRM for use with microanalytical techniques, evaluation of requirements for sample pre-treatment, evaluation of analytical techniques and research on development of techniques to be used in characterizing the homogeneity and chemical composition of small samples, and application of analytical techniques to the characterization of candidate reference materials for use with microanalytical techniques

  14. The updated IAEA database of natural matrix reference materials

    International Nuclear Information System (INIS)

    The International Atomic Energy Agency (IAEA) maintains a database of biological and environmental reference materials of natural origin (human and animal tissues, foods, plants, soils, sediments, etc.) for trace elements, radionuclides, stable isotopes, organic contaminants and other related measurands. The purpose is to help analysts to select reference materials for quality assurance purposes that match as closely as possible (i.e., with respect to matrix type and concentrations of the measurands of interest) the real samples that are to be analyzed. Former versions of this database were prepared in co-operation with the United Nations Environment Programme (UNEP), and provided as hardcopies free of charge. The latest version was from 1995. More recently the database bas been updated by the IAEA so that it now contains more than 22,500 values (mass fraction or concentration) for 660 different measurands and 1,705 reference materials developed by 56 producers from 22 countries. An overview of the structure and content of the database and of the two ways it may be browsed is given. Emphasis is given to reference materials that are intended to verifying analysis for radioanalytical measurements. The database is soon accessible on-line, cost-free, via the internet. (author)

  15. Effects of Extraction Solvents on the Extraction Efficiencies of Polychlorinated Dibenzo-p-dioxins and Dibenzofurans, and Polychlorinated Biphenyls in Reference Materials

    OpenAIRE

    KIGUCHI, Osamu; Kobayashi, Takashi; SAITOH, Katsumi

    2006-01-01

    This study investigated the extraction efficiency of a couple of different extraction solvents for Certified Reference Materials of soil and sediment that include Polychlorinated Dibenzo-p-dioxins and Dibenzofurans and Coplanar Polychlorinated Biphenyls using Soxhlet and Pressurized Liquid extraction (PLE). n-Hexane, toluene, acetone, acetone/n-hexane and acetone/toluene (1:1, v/v) as solvents were examined. Unsatisfactory results for Soxhlet extraction were obtained using n-hexane alone. For...

  16. Multi-Element Determination of Trace Elements in Natural Water Reference Materials by ICP-SFMS after Tm Addition and Iron Co-precipitation

    OpenAIRE

    Bayon, Germain; Birot, Dominique; Bollinger, Claire; Barrat, Jean Alix

    2011-01-01

    We report on an improved method for determining trace element abundances in seawater and other natural waters. The analytical procedure involves co-precipitation on iron hydroxides after addition of a Tm spike, and measurement by inductively coupled plasma-sector field mass spectrometry (ICP-SFMS). The validity of the method was assessed through a series of co-precipitation experiments, using ultra-diluted solutions of a certified rock reference material (BIR-1). Results obtained for four nat...

  17. Are they the same? Retrofitting 1 g sample data to certified 10 g sample characterization

    International Nuclear Information System (INIS)

    The National Institute of Standards and Technology Standard Reference Material 4357 (ocean sediment) was certified for anthropogenic radionuclides at ≥10 g sample size. However, the Aldermaston Weapons Establishment used a 1 g sample size that resulted in a highly skewed 239Pu + 240Pu alpha spectrometry measurement distribution that was outside the certified tolerance range for 10 g samples. This study evaluates the equivalence of 1 g sample results and those from 10 g samples used for certification. By re-batching the AWE 1 g results into simulated 10 g results, it was found that the AWE results were consistent with the certified plutonium activity for SRM 4357. (author)

  18. 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

  19. 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

  20. Gyttja, a low-level, high-organic reference material

    International Nuclear Information System (INIS)

    Gyttja, the bottom sediment from Perch Lake at Chalk River Nuclear Laboratories, was collected to prepare a low-level, high-organic standard radioactivity reference material. In the natural state it contained about 92% water and when dried the residue was about 50% organic material. The surface layer of this sediment contains small quantities of 60Co,90Sr,137Cs and 239Pu. The material was collected from depth using a sludge pump and the radioactivity content adjusted with addition of surface-layer material. It was then dewatered by centrifuge and freeze-dried. The overall exercise was a demonstration of co-operation between the National Bureau of Standards, Washington, D.C., Atomic Energy of Canada Limited, the Ontario Department of Labour, the Environmental Protection Service of Environment Canada, the Department of Agriculture, the Atomic Energy Control Board and two commercial firms, Rush Engineering and Freeze-Dried Foods, Incorporated. (author)

  1. Elemental Characterization of Olive Leaves as a Standard Reference Material

    International Nuclear Information System (INIS)

    Olive leaves standard reference material was produced by a co-operation programme between the Arab Atomic Energy Agency and Central Laboratory for Elemental and Isotopic Analysis in Atomic Energy Authority, Egypt. An intercomparison study was carried out, with 18 independent sets of results being reported from 9 analytical laboratories, The statistical evaluation of the collected data resulted in recommended values for 6 elements and information values for 8 elements

  2. Development of a Thin Film Magnetic Moment Reference Material.

    Science.gov (United States)

    Pappas, D P; Halloran, S T; Owings, R R; da Silva, F C S

    2008-01-01

    In this paper we present the development of a magnetic moment reference material for low moment magnetic samples. We first conducted an inter-laboratory comparison to determine the most useful sample dimensions and magnetic properties for common instruments such as vibrating sample magnetometers (VSM), SQUIDs, and alternating gradient field magnetometers. The samples were fabricated and then measured using a vibrating sample magnetometer. Their magnetic moments were calibrated by tracing back to the NIST YIG sphere, SRM 2853. PMID:27096108

  3. Homogeneity study of candidate reference material in fish matrix

    International Nuclear Information System (INIS)

    A material is perfectly homogeneous with respect to a given characteristic, or composition, if there is no difference between the values obtained from one part to another. Homogeneity is usually evaluated using analysis of variance (ANOVA). However, the requirement that populations of data to be processed must have a normal distribution and equal variances greatly limits the use of this statistical tool. A more suitable test for assessing the homogeneity of RMs, known as sufficient homogeneity, was proposed by Fearn and Thompson. In this work, we evaluate the performance of the two statistical treatments for assessing homogeneity of methylmercury (MeHg) in candidate reference material of fish tissue

  4. New Filler Material for Reference Free Part Encapsulation Fixture

    Institute of Scientific and Technical Information of China (English)

    LI Bei-zhi; YANG Jian-guo; ZHOU Hu

    2002-01-01

    Reference free part encapsulation (RFPE) is a nontraditional universal fixturing technique. In this paper,new filler material-a lower melting point alloy for RFPE technique is introduced. Based on experiment, the shrinlkage and expansion rate, the effect of filler on workpiece drift and the effect of filler thickness on cutting distortion are studied. The alloy has a good mechanical and physical performance and the need of RFPE fixturing can be perfectly satisfied. The result shows that if the formula and process parameters of filler material are properly selected, it can obviously improve the quality of the workpiece, enhance the machining efficiency and reduce the manufacturing cost.

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

    International Nuclear Information System (INIS)

    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

  6. Development and characterisation of a new line width reference material

    Science.gov (United States)

    Dai, Gaoliang; Zhu, Fan; Heidelmann, Markus; Fritz, Georg; Bayer, Thomas; Kalt, Samuel; Fluegge, Jens

    2015-11-01

    A new critical dimension (CD, often synonymously used for line width) reference material with improved vertical parallel sidewalls (IVPSs) has been developed and characterised. The sample has a size of 6 mm  ×  6 mm, consisting of 4 groups of 5  ×  5 feature patterns. Each feature pattern has a group of five reference line features with a nominal CD of 50 nm, 70 nm, 90 nm, 110 nm and 130 nm, respectively. Each feature pattern includes a pair of triangular alignment marks, applicable for precisely identifying the target measurement position, e.g. for comparison or calibration between different tools. The geometry of line features has been investigated thoroughly using a high-resolution transmission electron microscope and a CD atomic force microscope (CD-AFM). Their results indicate the high quality of the line features: the top corner radius of  strategy for the non-destructive calibration of the developed sample is introduced, which enables the application of the reference material in practice.

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

    International Nuclear Information System (INIS)

    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 UO2 spread throughout a graphite matrix. The 235U content ranges from 0 to 100 g. The manual also describes the far-field assay procedure used with low-resolution detectors

  8. Preparation and quality control of materials used in the reference buffer material

    Energy Technology Data Exchange (ETDEWEB)

    Dixon, D.A.; Hnatiw, D.S.J.; Kohle, C.L.

    1992-09-15

    This document summarizes the methodologies developed for preparing the reference buffer material (RBM) for use in laboratory-scale and field-scale experiments. Two commercially available concrete mixers have been successfully used to repeatedly produce homogeneous bulk buffer and backfill materials. The components, blending procedures, quality control sampling requirements, and mixing checklists used in the production of the reference buffer material are presented. Use of these directions will ensure that consistent batching of sealing materials is achieved and operator-induced variability is minimized.

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

    International Nuclear Information System (INIS)

    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)

  10. Recent developments in food-matrix Reference Materials at NIST.

    Science.gov (United States)

    Sharpless, K E; Colbert, J C; Greenberg, R R; Schantz, M M; Welch, M J

    2001-06-01

    Since 1996, the National Institute of Standards and Technology (NIST) has developed several food-matrix Standard Reference Materials (SRMs) characterized for nutrient concentrations. These include SRM 1544 Fatty Acids and Cholesterol in a Frozen Diet Composite, SRM 1546 Meat Homogenate, SRM 1548a Typical Diet, SRM 1566b Oyster Tissue, SRM 1846 Infant Formula, and SRM 2383 Baby Food Composite. Three additional materials--SRM 1946 Lake Superior Fish Tissue, SRM 2384 Baking Chocolate, and SRM 2385 Spinach--are in preparation. NIST also recently assigned values for proximate (fat, protein, etc.), individual fatty acid, and total dietary fiber concentrations in a number of existing SRMs and reference materials (RMs) that previously had values assigned for their elemental composition. NIST has used several modes for assignment of analyte concentrations in the food-matrix RMs, including the use of data provided by collaborating laboratories, alone and in combination with NIST data. The use of data provided by collaborating food industry and contract laboratories for the analysis of food-matrix RMs has enabled NIST to provide assigned values for many analytes that NIST does not have the resources or analytical expertise to measure. PMID:11451251

  11. Elemental Characterization of Single-Wall Carbon Nanotube Certified Reference Material by Neutron and Prompt gamma Activation Analysis

    Czech Academy of Sciences Publication Activity Database

    Kučera, Jan; Bennett, J. W.; Oflaz, R.; Paul, R. L.; De Nadai Fernandes, E. A.; Kubešová, Marie; Bacchi, M. A.; Stopic, A. J.; Sturgeon, R. E.; Grinberg, P.

    2015-01-01

    Roč. 87, č. 7 (2015), s. 3699-3705. ISSN 0003-2700 R&D Projects: GA ČR(CZ) GBP108/12/G108; GA MŠk LM2011019 Institutional support: RVO:61389005 Keywords : Neutron Activation Analyses * nanotechnology * Carbon nanotubes * Chemical activation * Single-walled carbon nanotubes (SWCN) Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

  12. Determination of trace elements in reference material Mussel by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Concentration of trace elements in an environmental reference material Mussel prepared by National Institute for Environmental Studies (NIES) has been determined by instrumental neutron activation analysis. The Mussel samples (ca. 50--250 mg) were irradiated for 2 min (pneumatic transfer) at a thermal neutron flux of 1.5 x 1012 n cm-2s-1 and then for 5h(central thimble) at thermal neutron flux of 3.2 x 1012 n cm-2s-1 in Musashi Institute of Technology Research Reactor (MITRR). The gamma-ray measurements of 2 min irradiation samples were performed for 5 min intervals after 1 min cooling and for 4--27 min after 12--80 min cooling using a Ge (Li) detector coupled to a 4096 channel multichannel analyzer. The gamma-ray spectra from 5h irradiation samples were obtained by measuring samples for 3--14h after 4--8d cooling period and for 14--45h after 15--50d cooling. Peak-fitting procedure by a minicomputer system (GAMA system) was applied to analyze gamma-ray spectra. In this work 38 elements (Na,Mg,Al,S,Cl,K,Ca,Sc,V,Cr,Mn,Fe,Co,Ni,Zn,As,Se,Br,Rb,Sr,Mo,Ag,Cd,Sn,Sb,I,Cs,Ba,La,Ce,Sm,Eu,Tb,Hf,Ta,Au,Th,U) were quantitatively determined. Special cares were taken for obtaining accurate concentrations of aluminum and magnesium by correcting contributions by interefering nuclear reactions such as 31P(n,α)28Al and 27Al(n,p)27Mg. Duplicate analyses showed a reasonable reproduciblity for the analytical data of major and trace elements, suggesting that the Mussel is homogeneous enough to be used as a certified reference material. (author)

  13. Collaborative analysis for certification of zirconium and zirconium base alloy reference materials JAERI-Z11 to Z16

    International Nuclear Information System (INIS)

    The second Sub-Committee on Zircaloy Analysis was organized in April 1978, under the Committee on Analytical Chemistry on Nuclear Fuels and Reactor Materials, JAERI, for the renewal of zirconium and zirconium base alloy certified reference materials (CRMs). The Sub-Committee carried out collaborative analysis among 13 participating laboratories for the certification of the CRMs, JAERI-Z11 to Z18, after development, improvement and evaluation of analytical methods during the period of May 1978 to June 1982. As the result of the collaborative analysis, the certified value was given for 18 elements (Sn, Fe, Ni, Cr, B, Cd, U, Cu, Co, Mn, Pb, Al, Ti, Si, Mo, W, Hf, C) in the CRMs. The first part of this report includes general discussion, the second part principles of certification, the third part development and verification of analytical methods, and the fourth part evaluation of analytical results on 17 elements. Preparation of Z11 to Z18, and certification for carbon in JAERI-Z17 and Z18 were reported separately in JAERI-M 83-241 and M 83-035, respectively. (author)

  14. Multielement analysis of human hair reference material by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    A Human Hair (NIES No. 5) as an environmental reference material prepared by the National Institute for Environmental Studies of Japan (NIES) was analyzed by an instrumental neutron activation method. The human hair samples (ca. 200∼500 mg) were irradiated for 2 min or 5 h at Musashi Institute of Technology Research Reactor. The activated samples were measured by four gamma-ray spectrometories, namely a spectrometry using a coaxial Ge detector, anticoincidence and coincidence counting spectrometries using a coaxial Ge detector, and a well-type NaI (Tl) detector, and a low energy photon spectrometry (LEPS) using a planer Ge detector, to determine as many trace elements as possible with high sensitivity. Concentrations of 43 elements (Na, Mg, Al, Si, S, Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Ag, Cd, Sn, Sb, I, Cs, Ba, La, Ce, Nd, Sm, Eu, Tb, Yb, Hf, Ta, Au, Hg, Th, U) were determined by these measurements. The analyzed values of many elements except Sr were in good agreement with NIES certified values determined by nine different analytical methods. (author)

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

    International Nuclear Information System (INIS)

    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 31 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)

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

    International Nuclear Information System (INIS)

    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

  17. Development and characterisation of a new line width reference material

    International Nuclear Information System (INIS)

    A new critical dimension (CD, often synonymously used for line width) reference material with improved vertical parallel sidewalls (IVPSs) has been developed and characterised. The sample has a size of 6 mm  ×  6 mm, consisting of 4 groups of 5  ×  5 feature patterns. Each feature pattern has a group of five reference line features with a nominal CD of 50 nm, 70 nm, 90 nm, 110 nm and 130 nm, respectively. Each feature pattern includes a pair of triangular alignment marks, applicable for precisely identifying the target measurement position, e.g. for comparison or calibration between different tools. The geometry of line features has been investigated thoroughly using a high-resolution transmission electron microscope and a CD atomic force microscope (CD-AFM). Their results indicate the high quality of the line features: the top corner radius of  <7 nm, vertical sidewall (slope mostly within 90°  ±  0.5°) and very small line width variation (LWR down to 0.36 nm). The application of the developed sample for calibrating the scaling factor and effective tip geometry of the CD-AFM are demonstrated. The scaling factor of the CD-AFM is calibrated to be 0.9988, coinciding well with the theoretical value 1 as the tool was calibrated to a traceable metrological atomic force microscope. The effective width of a CDR120-EBD tip is calibrated as 128.32 nm. Finally, a strategy for the non-destructive calibration of the developed sample is introduced, which enables the application of the reference material in practice. (paper)

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

    International Nuclear Information System (INIS)

    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)

  19. Certified Schools - SEVIS

    Data.gov (United States)

    Department of Homeland Security — Certified schools must provide specific information regarding the school, the nature and requirements of the educational program, location and contact information,...

  20. Use of reference materials for validating analytical methods. Applied to the determination of As, Co, Na, Hg, Se and Fe using neutron activation analysis

    International Nuclear Information System (INIS)

    The main purpose of an analytical laboratory is to provide reliable information on the nature and composition of the materials submitted for analysis. This purpose can only be attained if analytical methodologies that have the attributes of accuracy, precision, specificity and sensitivity, among others, are used. The process by which these attributes are evaluated is called validation of the analytical method. The Chilean Nuclear Energy Commission's Neutron Activation Analysis Laboratory is applying a quality guarantee program to ensure the quality of its analytical results, which aims, as well, to attain accreditation for some of its measurements. Validation of the analytical methodologies used is an essential part of applying this program. There are many forms of validation, from comparison with reference techniques to participation in inter-comparison rounds. Certified reference materials were used in this work in order to validate the application of neutron activation analysis in determining As, Co, Na, Hg, Se and Fe in shellfish samples. The use of reference materials was chosen because it is a simple option that easily detects sources of systematic errors. Neutron activation analysis is an instrumental analytical method that does not need chemical treatment and that is based on processes which take place in the nuclei of atoms, making the matrix effects unimportant and different biological reference materials can be used. The following certified reference materials were used for validating the method used: BCR human hair 397, NRCC dogfish muscle DORM-2, NRCC -dogfish liver DOLT-2, NIST - oyster tissue 1566, NIES - mussel 6 and BCR - tuna fish 464. The reference materials were analyzed using the procedure developed for the shellfish samples and the above-mentioned elements were determined. With the results obtained, the parameters of accuracy, precision, detection limit, quantification limit and uncertainty associated with the method were determined for each

  1. Polish reference material: soya bean flour (INCT-SBF-4) for inorganic trace analysis - preparation and certification

    International Nuclear Information System (INIS)

    Preparation, examination and certification of the new matrix reference material of biological origin: Soya Bean Flour (INCT-SBF-4) is described. The material was prepared from soya bean grown in India, not genetically modified. After milling, the material was sieved through the 150 mm nylon sieves and stored in a polyethylene (PE) bag. Approximately 50 kg of sieved soya bean flour was collected. Examination by optical microscopy revealed that Martin's diameter of over 90% of particles was below 50 mm. The whole lot of soya bean flour was then homogenized by mixing for 20 hours in a 110 dm3 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-SBF-4 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 oC. Short-term stability was examined by the determination of concentrations of the selected elements in the bottle stored in the CO2 incubator at 37 oC. The material was certified on the basis of a worldwide interlaboratory comparison, in which 92 laboratories from 19 countries participated providing 1107 laboratory averages (4873 individual determinations) for 58 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 results for a few elements were 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

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

    International Nuclear Information System (INIS)

    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)

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

    International Nuclear Information System (INIS)

    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 241Am relative to weapons grade Pu, waste that is dominantly 241Am, as well as wastes containing various proportions of depleted uranium. The CEP WRMs consist of a special mixture of PuO2/AmO2 (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

  4. 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.

  5. Traceability and quality requirements for reference materials. The context for trace element speciation

    International Nuclear Information System (INIS)

    of methylmercury (IAEA-085 and IAEA- 086, Human Hair, IAEA-140/TM, Fucus and IAEA-142, Mussel Homogenate), RMs for trace element speciation represent a new type of RMs for the IAEA. RMs for trace element speciation belong to the group of matrix RMs. The simplest and possibly best definition of a matrix RM is that it is a 'natural' substance more representative of laboratory samples that has been chemically characterised for one or more elements, constituents, etc. with quantified uncertainty. 'Natural' materials are more complex, chemically, compositionally and structurally, than primary reference standards, which are often pure substances. On the other hand, the chemical characterisation of 'natural' materials usually has a greater level of uncertainty and is less straightforward in terms of traceability. It is also true to say that the majority of matrix RMs, available, including the RMs produced by the IAEA, have been certified through laboratory intercomparison or measurement programmes

  6. 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

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

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira Junior, Olivio Pereira de

    2006-07-01

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

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

    International Nuclear Information System (INIS)

    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

  9. Production of highly-enriched 134Ba for a reference material for isotope dilution mass spectrometry measurements

    International Nuclear Information System (INIS)

    Isotope dilution mass spectrometry (IDMS) is an analytical technique capable of providing accurate and precise quantitation of trace isotope abundance and assay providing measurement uncertainties below 1 %. To achieve these low uncertainties, the IDMS method ideally utilizes chemically pure 'spike' solutions that consist of a single highly enriched isotope that is well-characterized relating to the abundance of companion isotopes and concentration in solution. To address a current demand for accurate 137Cs/137Ba ratio measurements for 'age' determination of radioactive 137Cs sources, Idaho National Laboratory (INL) is producing enriched 134Ba isotopes that are tobe used for IDMS spikes to accurately determine 137Ba accumulation from the decay of 137Cs. The final objective of this work it to provide a homogenous set of reference materials that the National Institute of Standards and Technology can certify as standard reference materials used for IDMS. The process that was developed at INL for the separation and isolation of Ba isotopes, chemical purification of the isotopes in solution, and the encapsulation of the materials will be described. (author)

  10. Certified Subterm Criterion and Certified Usable Rules

    OpenAIRE

    Sternagel, Christian; Thiemann, René

    2010-01-01

    In this paper we present our formalization of two important termination techniques for term rewrite systems: the subterm criterion and the reduction pair processor in combination with usable rules. For both techniques we developed executable check functions in the theorem prover Isabelle/HOL which can certify the correct application of these techniques in some given termination proof. As there are several variants of usable rules we designed our check function in such a way ...

  11. k{sub 0}-NAA quality assessment in an Algerian laboratory by analysis of SMELS and four IAEA reference materials using Es-Salam research reactor

    Energy Technology Data Exchange (ETDEWEB)

    Hamidatou, L.A., E-mail: lylia.h@hotmail.fr [Nuclear Reseach Center of Birine, P.O. Box 180 Ain Oussera, 17200 Djelfa (Algeria); Dekar, S.; Boukari, S. [Department of physics, Ferhat Abbes University, 19000 Setif (Algeria)

    2012-08-01

    Different types of synthetic multi-element standard material (SMELS) and four IAEA reference materials, 140, Sl-1, Soil-7 and Lichen-336 were analyzed for validation and QC/QA of the k{sub 0}-standardised Neutron Activation Analysis (k{sub 0}-NAA). The samples of SMELS and RMs were irradiated at Es-Salam research reactor and measured on an absolutely calibrated HPGe detector with 35% relative efficiency connected to a Canberra Genie 2k inspector. Concentrations of 33 elements such as As, Au, Ba, Br, Ca, Ce, Co, Cr, Cs, Eu, Fe, Hf, In, K, La, Mn, Mo, Na, Nd, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, Tm, U, Yb, Zn, and Zr were determined in SMELS and RMs. The analytical results agreed well with the assigned values of SMELS and certified values of RMs. In the case of RMs, concentrations of a few elements, whose certified values are not available, could be determined. The comparison between experimental values and assigned/certified data for SMELS and RMs was made by means of the results from Relative Bias, Z-score and U-score. The relatives bias of the elements determined in SMELS with respect to the assigned values were all within{+-}4.6%. For RMs with respect to certified values were within{+-}10% except for few elements for which RB varied from -28.6% to +12.8%. The Z-score values at 95% confidence level for most of the elements in both the materials were within {+-}1. The U-scores for most of the elements were lower than 1.

  12. k0-NAA quality assessment in an Algerian laboratory by analysis of SMELS and four IAEA reference materials using Es-Salam research reactor

    Science.gov (United States)

    Hamidatou, L. A.; Dekar, S.; Boukari, S.

    2012-08-01

    Different types of synthetic multi-element standard material (SMELS) and four IAEA reference materials, 140, Sl-1, Soil-7 and Lichen-336 were analyzed for validation and QC/QA of the k0-standardised Neutron Activation Analysis (k0-NAA). The samples of SMELS and RMs were irradiated at Es-Salam research reactor and measured on an absolutely calibrated HPGe detector with 35% relative efficiency connected to a Canberra Genie 2k inspector. Concentrations of 33 elements such as As, Au, Ba, Br, Ca, Ce, Co, Cr, Cs, Eu, Fe, Hf, In, K, La, Mn, Mo, Na, Nd, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, Tm, U, Yb, Zn, and Zr were determined in SMELS and RMs. The analytical results agreed well with the assigned values of SMELS and certified values of RMs. In the case of RMs, concentrations of a few elements, whose certified values are not available, could be determined. The comparison between experimental values and assigned/certified data for SMELS and RMs was made by means of the results from Relative Bias, Z-score and U-score. The relatives bias of the elements determined in SMELS with respect to the assigned values were all within±4.6%. For RMs with respect to certified values were within±10% except for few elements for which RB varied from -28.6% to +12.8%. The Z-score values at 95% confidence level for most of the elements in both the materials were within ±1. The U-scores for most of the elements were lower than 1.

  13. k0-NAA quality assessment in an Algerian laboratory by analysis of SMELS and four IAEA reference materials using Es-Salam research reactor

    International Nuclear Information System (INIS)

    Different types of synthetic multi-element standard material (SMELS) and four IAEA reference materials, 140, Sl-1, Soil-7 and Lichen-336 were analyzed for validation and QC/QA of the k0-standardised Neutron Activation Analysis (k0-NAA). The samples of SMELS and RMs were irradiated at Es-Salam research reactor and measured on an absolutely calibrated HPGe detector with 35% relative efficiency connected to a Canberra Genie 2k inspector. Concentrations of 33 elements such as As, Au, Ba, Br, Ca, Ce, Co, Cr, Cs, Eu, Fe, Hf, In, K, La, Mn, Mo, Na, Nd, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, Tm, U, Yb, Zn, and Zr were determined in SMELS and RMs. The analytical results agreed well with the assigned values of SMELS and certified values of RMs. In the case of RMs, concentrations of a few elements, whose certified values are not available, could be determined. The comparison between experimental values and assigned/certified data for SMELS and RMs was made by means of the results from Relative Bias, Z-score and U-score. The relatives bias of the elements determined in SMELS with respect to the assigned values were all within±4.6%. For RMs with respect to certified values were within±10% except for few elements for which RB varied from −28.6% to +12.8%. The Z-score values at 95% confidence level for most of the elements in both the materials were within ±1. The U-scores for most of the elements were lower than 1.

  14. Metallurgical and chemical characterization of copper alloy reference materials within laser ablation inductively coupled plasma mass spectrometry: Method development for minimally-invasive analysis of ancient bronze objects

    Energy Technology Data Exchange (ETDEWEB)

    Walaszek, Damian, E-mail: damian.walaszek@empa.ch [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); University of Warsaw, Faculty of Chemistry, Pasteura 1, 02-093 Warsaw (Poland); Senn, Marianne [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Faller, Markus [Laboratory for Jointing Technology and Corrosion, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Philippe, Laetitia [Laboratory for Mechanics of Materials and Nanostructures, Swiss Federal Laboratories for Materials Science and Technology, Feuerwerkstrasse 39, CH-3602 Thun (Switzerland); Wagner, Barbara; Bulska, Ewa [University of Warsaw, Faculty of Chemistry, Pasteura 1, 02-093 Warsaw (Poland); Ulrich, Andrea [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland)

    2013-01-01

    The chemical composition of ancient metal objects provides important information for manufacturing studies and authenticity verification of ancient copper or bronze artifacts. Non- or minimal-destructive analytical methods are preferred to mitigate visible damage. Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) enables the determination of major elements as well as impurities down to lower ppm-levels, however, accuracy and precision of analysis strongly depend on the homogeneity of reference materials used for calibration. Moreover, appropriate analytical procedures are required e.g. in terms of ablation strategies (scan mode, spot size, etc.). This study reviews available copper alloy (certified) reference materials — (C)RMs from different sources and contributes new metallurgical data on homogeneity and spatial elemental distribution. Investigations of the standards were performed by optical and scanning electron microscopy with X-ray spectrometry (SEM-EDX) for the following copper alloy and bronze (certified) reference materials: NIST 454, BAM 374, BAM 211, BAM 227, BAM 374, BAM 378, BAS 50.01-2, BAS 50.03-4, and BAS 50.04-4. Additionally, the influence of inhomogeneities on different ablation and calibration strategies is evaluated to define an optimum analytical strategy in terms of line scan versus single spot ablation, variation of spot size, selection of the most appropriate RMs or minimum number of calibration reference materials. - Highlights: ► New metallographic data for copper alloy reference materials are provided. ► Influence of RMs homogeneity on quality of LA-ICPMS analysis was evaluated. ► Ablation and calibration strategies were critically discussed. ► An LA-ICPMS method is proposed for analyzing most typical ancient copper alloys.

  15. Metallurgical and chemical characterization of copper alloy reference materials within laser ablation inductively coupled plasma mass spectrometry: Method development for minimally-invasive analysis of ancient bronze objects

    International Nuclear Information System (INIS)

    The chemical composition of ancient metal objects provides important information for manufacturing studies and authenticity verification of ancient copper or bronze artifacts. Non- or minimal-destructive analytical methods are preferred to mitigate visible damage. Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) enables the determination of major elements as well as impurities down to lower ppm-levels, however, accuracy and precision of analysis strongly depend on the homogeneity of reference materials used for calibration. Moreover, appropriate analytical procedures are required e.g. in terms of ablation strategies (scan mode, spot size, etc.). This study reviews available copper alloy (certified) reference materials — (C)RMs from different sources and contributes new metallurgical data on homogeneity and spatial elemental distribution. Investigations of the standards were performed by optical and scanning electron microscopy with X-ray spectrometry (SEM-EDX) for the following copper alloy and bronze (certified) reference materials: NIST 454, BAM 374, BAM 211, BAM 227, BAM 374, BAM 378, BAS 50.01-2, BAS 50.03-4, and BAS 50.04-4. Additionally, the influence of inhomogeneities on different ablation and calibration strategies is evaluated to define an optimum analytical strategy in terms of line scan versus single spot ablation, variation of spot size, selection of the most appropriate RMs or minimum number of calibration reference materials. - Highlights: ► New metallographic data for copper alloy reference materials are provided. ► Influence of RMs homogeneity on quality of LA-ICPMS analysis was evaluated. ► Ablation and calibration strategies were critically discussed. ► An LA-ICPMS method is proposed for analyzing most typical ancient copper alloys

  16. 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.

  17. Utilization of Research Reactors in Standard Reference Material Certification

    Energy Technology Data Exchange (ETDEWEB)

    Capannesi, G.; Rosada, A. [UTFISST-CATNUC, ENEA, R.C.-Casaccia, via Anguillarese 301, 00060 Rome (Italy); Avino, P. [DIPIA, INAIL (ex-ISPESL), via Urbana 167, 00184 Rome (Italy)

    2011-07-01

    The certification issue of Standard Reference Materials is one of the most complex analytical problems and runs over different research fields. International organization, e.g. NIST, BCR etc., organize continuously systematic intercomparison campaigns among worldwide laboratories using different analytical techniques. Samples are irradiated in nuclear research reactors and analyzed by Instrumental Neutron Activation Analysis, a technique strongly involved in this field for its significant analytical properties. This paper shows a study on Zircaloy-4. The importance of accurate measurements of minor constituents, i.d. Cr, Fe, Hf and Sn, regards its characteristics of corrosion resistance and mechanical properties. The samples were irradiated in the rotating rack of the TRIGA Mark II reactor of the R.C.-Casaccia (ENEA). The gamma spectrometry measurements were performed after 30 and 90 days of decay by means of HPGe detector. The results obtained by interlaboratory intercomparison can highlight an excellent precision for Cr, Hf and Sn, and a good precision for Fe. The reliability of the technique is confirmed by Hf determination, since the INAA is one of the few analytical techniques measuring and delivering accurate and homogeneous data. (author)

  18. FDA Certified Mammography Facilities

    Science.gov (United States)

    ... Products Radiation-Emitting Products Home Radiation-Emitting Products Mammography Quality Standards Act and Program Consumer Information (MQSA) ... it Email Print This list of FDA Certified Mammography Facilities is updated weekly. If you click on ...

  19. ENERGY STAR Certified Boilers

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 3.0 ENERGY STAR Program Requirements for Boilers that are effective as of October 1,...

  20. ENERGY STAR Certified Dehumidifiers

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 3.0 ENERGY STAR Program Requirements for Dehumidifiers that are effective as of October...

  1. ENERGY STAR Certified Computers

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 6.1 ENERGY STAR Program Requirements for Computers that are effective as of June 2,...

  2. ENERGY STAR Certified Displays

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 6.0 ENERGY STAR Program Requirements for Displays that are effective as of June 1, 2013....

  3. 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)

    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

  4. Development of a multi-VOC reference material for quality assurance in materials emission testing.

    Science.gov (United States)

    Nohr, Michael; Horn, Wolfgang; Jann, Oliver; Richter, Matthias; Lorenz, Wilhelm

    2015-04-01

    Emission test chamber measurement is necessary to proof building materials as sources of volatile organic compounds (VOCs). The results of such measurements are used to evaluate materials and label them according to their potential to emit harmful substances, polluting indoor air. If only labelled materials were installed indoors, this would improve indoor air quality and prevent negative impacts on human health. Because of the complex testing procedure, reference materials for the quality assurance are mandatory. Currently, there is a lack of such materials because most building products show a broad variation of emissions even within one batch. A previous study indicates lacquers, mixed with volatile organic pollutants, as reproducible emission source for a wide range of substances. In the present study, the curing of the lacquer-VOC mixture inside micro-chambers was optimised. Therefore, the humidity and the chamber flow were varied. Typical indoor air pollutants with a wide range of volatilities, for example, styrene, n-hexadecane, dimethyl and dibutyl phthalate were selected. It turned out that, under optimised curing parameters inside the micro-chamber, their emission can be reproduced with variations of less than 10 %. With this, a next important step towards a reference material for emission testing was achieved. PMID:25543146

  5. 40 CFR 600.011-93 - Reference materials.

    Science.gov (United States)

    2010-07-01

    ... 5 U.S.C. 552(a) and 1 CFR part 51. Copies may be inspected at the U.S. Environmental Protection.... Document number and name 40 CFR part 600 reference ASTM E 29-67 (Reapproved 1973) Standard Recommended... the U.S. and Canada), or at http://www.sae.org. Document No. and name 40 CFR part 600 reference...

  6. 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…

  7. Selective arsenic speciation analysis of human urine reference materials using gradient elution ion-exchange HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, K.

    2004-01-01

    identical with the reference values given for total arsenic. The obtained values for arsenobetaine and dimethylarsinic acid were identical with the values certified for the NIES No. 18 urine CRM. The speciation data presented here may be valuable for the quality assurance of analytical method development...

  8. [Reference ranges of 9 plasmatic proteins in Tunisian population based on the new IFCC reference material CRM 470].

    Science.gov (United States)

    Znazen, Raja; Ben Ayed, Mourad; Gargouri, Jalel; Bel Hadj Hmida, Youssef; Kassis, Mondher; Damak, Jamel; Masmoudi, Hatem

    2003-04-01

    The interpretation of biological exam results requires the knowledge of physiological variation factors and reference values for every parameter. Following the preparation and the diffusion by the International Federation of Clinical Chemistry (IFCC) of a new reference material for the dosage of plasmatic proteins (CRM470) and in order to take part in the international effort of standardization of these dosages, we established reference ranges in the tunisian population for 9 plasmatic proteins: the Immunoglobulines G, A and M, complement factors C3 and C4, albumin, transferrin, haptoglobin and the a 1-glycoprotéin acid. Our sample of 211 healthy blood donors aged between 18 and 63 years. Reference limits 0.95 that we obtained are located within variation of most reference values lately found in the literature. PMID:12848010

  9. Determination of As, Cd, Pb and Se in DORM-1 dogfish muscle reference material using alkaline solubilization and electrothermal atomic absorption spectrometry with Ir+Rh as permanent modifiers or Pd+Mg in solution

    International Nuclear Information System (INIS)

    In this work, tetramethylammonium hydroxide (TMAH) was used to solubilize the DORM-1 dogfish muscle certified reference material as a model substance for the determination of As, Cd, Pb and Se by electrothermal atomic absorption spectrometry (ET AAS). The sample was mixed with a small amount of TMAH and heated to 60 deg. C for 10 min in a water bath. After dissolution, As and Se were determined using palladium and magnesium nitrates as a chemical modifier added in solution. For Cd and Pb, best results were obtained with a mixture of 250 μg of each of iridium and rhodium as permanent modifiers. In both cases, the calibration was performed with aqueous solutions in 0.2% v/v HNO3. The temperature program for each analyte was optimized using pyrolysis and atomization curves established with the fish reference material. The detection limits in dry samples and the characteristic mass values were: Cd 0.005 μg g-1 and 0.9 pg; Pb 0.04 μg g-1 and 7.6 pg; As 0.4 μg g-1 and 13 pg and Se 0.6 μg g-1 and 20 pg, respectively. Results from the determination of these elements in the DORM-1 certified fish reference material were within the 95% confidence interval of the certified values

  10. INAA study of Hg, Se, As, and Br irradiation losses from l-cysteine treated and untreated reference materials

    International Nuclear Information System (INIS)

    U. S. Food and Drug Administration in-house reference material (RM) Cocoa Powder and National Institute of Standards and Technology Standard RMs (SRMs) 1515 apple leaves, 1547 peach leaves, 1571 orchard leaves, 1566a oyster tissue, and 1568a rice flour were co-irradiated together with polyethylene blanks and analyzed for Hg and Se by anticoincidence instrumental neutron activation analysis. The three botanical SRM portions showed a combined Hg recovery of 70 % while the other portions showed a combined Hg recovery of 169 %, indicating that volatile Hg was lost from botanical SRMs and absorbed by the other irradiated portions. Total Hg recovery for all portions was 82 %. Se results showed no evidence of cross-contamination and all results agreed with certified and known values. National Research Council of Canada Certified RMs DOLT-3 dogfish liver, TORT-2 lobster hepatopancreas, and DORM-3 fish protein were separately analyzed either with no treatment or after treatment with l-cysteine solutions followed by drying over magnesium perchlorate. Each set of portions was co-irradiated with polyethylene and treated filter blanks. Analysis of all components of each treated portion irradiation package showed that essentially all Hg was retained within the package. Treated DOLT-3 portions (inorganic Hg content 53 %) showed a tenfold improvement with 99 % Hg retention. Hg retention for DORM-3 (7 % inorganic Hg) was 85 % (a twofold improvement) while retention for TORT-2 (44 % inorganic Hg), was 94 %, similar to that for untreated portions (96 %). Small irradiation losses (≤0.5 %) of volatile species of Se, As, and Br were observed. (author)

  11. Acquisition of improved reference values for cesium, iodine, strontium, thorium, and uranium in selected NIST reference materials.

    Science.gov (United States)

    Parr, R M; Kawamura, H; Iyengar, G V

    1999-01-01

    As part of a study on the ingestion and organ content of some trace elements of importance in radiological protection, additional work has been undertaken to acquire improved reference values for cesium, iodine, strontium, thorium, and uranium in four selected reference materials provided by the US National Institute of Standards and Technology. The materials are SRM-1548 Total Diet, SRM-1548a Typical Diet, SRM-1486 Bone Meal, and RM-8414 Bovine Muscle. A coordinated study was undertaken with the help of seven selected laboratories in five countries. Instrumental and radiochemical neutron activation analysis and inductively coupled plasma-mass spectrometry were the analytical main techniques used. PMID:10676473

  12. The preparation of biological reference materials for QUASIMEME

    OpenAIRE

    Kotterman, M.J.J.

    2011-01-01

    Biological materials, consisting of three different batches of mussels; from Den Helder harbour (POPs, TBT), Irish mussels (metals) and Wadden Sea mussels, fortified with highly contaminated mussels from Belgium (POPs), and of one batch of turbot liver (metals) have been prepared for use in QUASIMEME interlaboratory studies for metal and organic contaminant analyses. The homogeneity of the prepared material was tested for metals or POPs, depending on the intended use of the material, and indi...

  13. 9 CFR 77.1 - Material incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ... been approved for incorporation by reference into the Code of Federal Regulations by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. (a) The procedures... 1141, USDA South Building, 14th Street and Independence Avenue, SW., Washington, DC; or (3) May...

  14. 10 CFR 431.443 - Materials incorporated by reference.

    Science.gov (United States)

    2010-01-01

    ... this section for incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Any... Polyphase Induction Motors and Generators, approved February 9, 2004, IBR approved for § 431.444. (2) IEEE... Single-Phase Induction Motors, approved December 6, 2001, IBR approved for § 431.444....

  15. Reference materials and their role in quality assurance in environmental monitoring

    International Nuclear Information System (INIS)

    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)

  16. REIMEP-22 U age dating - Determination of the production date of a uranium certified test sample Inter-laboratory comparison, Report to participants

    OpenAIRE

    VENCHIARUTTI CELIA; VARGA ZSOLT; Richter, Stephan; Nicholl, Adrian; KRAJKO JUDIT; JAKOPIC Rozle; Mayer, Klaus; AREGBE Yetunde

    2015-01-01

    The REIMEP-22 inter-laboratory comparison (ILC) "U Age Dating - Determination of the production date of a uranium certified test sample" was organised by JRC-IRMM as support to the Nuclear Forensics International Technical Working Group (ITWG) This ILC was organised prior to the release of the candidate certified reference material IRMM-1000, produced in cooperation with JRC-ITU. The aim of REIMEP-22 was to determine the production date of the uranium certified test sample (i.e. the last chem...

  17. Household Hazardous Materials and Their Labels: A Reference for Teachers.

    Science.gov (United States)

    Dean, Lillian F.

    Household hazardous materials are products or wastes which are toxic, corrosive, reactive, and/or ignitable. Although common products such as pesticides, oils, gasoline, solvents, cleaners, and polishes are hazardous, students and adults are not always aware of potential dangers. This sourcebook contains definitions and examples of household…

  18. 16O thin film reference materials for nuclear reaction analysis

    International Nuclear Information System (INIS)

    Full text: Thin film Ta2O5 samples were distributed to CRP participants for use in the round-robin exercise. This appendix describes how these samples were prepared and characterized. Preparation was made using anodic oxidation of tantalum using an electrolyte solution of 4% ammonium citrate prepared with water of natural 16O isotopic composition. A constant anodising current of 4 mA/cm2 was maintained until the desired electrolysis v voltage was reached, then stopped immediately. The areal density of 16O in these thin Ta2O5 films was determined by NRA using the method described elsewhere and comparing the data with that from a primary anodic Ta2O5 standard kindly made available to us by Dr C. Ortega of GPS, Paris. The 16O(d,p1)14N reaction at 850 keV was used with the protons detected with a 300 mm2 silicon detector located at an angle of 150 deg. A 12 μm MylarTM foil covered the detector. Detector count rates were kept sufficiently low so that deadtime corrections are negligible. There are various sources of uncertainty which when compounded, produce the final uncertainty in the 16O areal density of the thin film samples. The major sources of uncertainty are: 1. The primary reference standard is estimated to have an absolute value that is within ± 3% of the true value. 2. There is a small low energy tail on the p1 peak in the NRA spectrum, most likely due to oxygen dissolved in the bulk tantalum. The counts in this tailing are less than 2% of the gross counts recorded in the spectrum peak, and similar in magnitude from sample to sample. We assign a systematic error of 0.5% to the background correction for all samples. There is negligible change in the total sample uncertainty when this systematic error is added in quadrature to the uncertainty of the primary reference standard. 3. The reproducibility of peak areas from several measurements was better than 1%. This indicates that sample homogeneity and current integration were both sufficiently good that their

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

    International Nuclear Information System (INIS)

    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

  20. 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.

  1. 238U/235U determinations of some commonly used reference materials and U-bearing accessory minerals (Invited)

    Science.gov (United States)

    Condon, D.; Noble, S.; McLean, N.; Bowring, S. A.

    2009-12-01

    We have determined 238U/235U ratios for a suite of commonly used natural (CRM 112a, SRM 950a, HU-1) and synthetic (IRMM 184 and CRM U500) uranium reference materials in addition to several U-bearing accessory phases (zircon and monazite) by thermal ionisation mass-spectrometry (TIMS) using the IRMM 3636 233U-236U double spike to accurately correct for mass fractionation. The 238U/235U values for the natural uranium reference materials differ, by up to 0.1%, from the widely used ‘consensus’ value (137.88) with all having 238U/235U values less than 137.88. Similarly, initial 238U/235U data from zircon and monazite yield 238U/235U values that are lower than the ‘consensus’ value. The data obtained from U-bearing minerals is used to assess how the uncertainty in the 238U/235U ratio contributes to the systematic discordance observed in 238U/206Pb and 235U/207Pb dates (Mattinson, 2000; Schoene et al., 2006) which has traditionally been wholly attributed to error in the U decay constants. The 238U/235U determinations made on the synthetic reference materials yield results that are considerably more precise and accurate than the certified values (0.02% vs. 0.1% for CRM U500). The calibration of isotopic tracers used for U-daughter geochronology that are partially based upon these reference materials, and the resultant age determinations, will benefit from increased accuracy and precision. Mattinson, J.M., 2000. Revising the “gold standard”—the uranium decay constants of Jaffey et al., 1971. Eos Trans. AGU, Spring Meet. Suppl., Abstract V61A-02. Schoene B., Crowley J.L., Condon D.C., Schmitz M.D., Bowring S.A., 2006, Reassessing the uranium decay constants for geochronology using ID-TIMS U-Pb data. Geochimica et Cosmochimica Acta 70: 426-445

  2. DGNB certified Healthcare Centres

    DEFF Research Database (Denmark)

    Brunsgaard, Camilla; Larsen, Tine Steen

    2015-01-01

    sustainability and wants a certification. This research investigates the decision‐making and design process (DMaDP) behind four DGNB certified Healthcare Centres (HCC) in Northern Jutland in Denmark. In general, knowledge about the DMaDP is important. However it is important to know what part DGNB plays in an...... the architect, the construction engineer, the plumbing engineer etc. which overlap professional field just like other disciplines. Secondly, the general conception is that DGNB brings in limited new things into the project, but it gives a common notion of sustainability which usually can be discussed...... Healthcare Centres, which was certified as office buildings, however more traditional office buildings might differ en experience with DGNB....

  3. DGNB certified Healthcare Centres

    DEFF Research Database (Denmark)

    Brunsgaard, Camilla; Larsen, Tine Steen

    2015-01-01

    In recent years, research and the building industry greatly focused on lowering and optimising the energy use of buildings during operation. It has resulted in several pilot projects which illustrate how it can be achieved. At the same time voluntary sustainability certification schemes (BEAM, LEED...... already highly complex design processes; does it become even more complex? What can we learn from these projects about future DMaDP in DGNB certified projects?The research project is setup as a case study design, where the HCC act as four cases. We analyse the DMaDP behind the four HCC using qualitative...... interviews of key actors in each design team. Each interview is analysed individually and summarised in a report. Finally the four cases are analysed in a comparative study which draw a picture of what kind of DMaDP the DGNB certified HCC have had. At time of writing the analysis of the interviews are in...

  4. Standard reference materials: srm 768: temperature reference standard for use below 0. 5 k

    Energy Technology Data Exchange (ETDEWEB)

    Stolen, R.J. Jr; Dove, R.B.

    1979-04-01

    Cryogenic temperature scales are now available (viz., the newly created EPT-76) which are quite accurate and which extend deep into the cryogenic region (as low as 0.5 K). It is the region below 0.5 K where no formal scale exists which is of concern here. By developing a compact device which provides five reference temperatures from 0.015 K to 0.21 K, the authors hope to provide a lingua franca by which experimental results of different laboratories involving the parameter temperature may be meaningfully compared. Such a device, designated SRM 768, is now available and consists of a self-contained assembly of coils and five samples which can be used to provide in situ temperature calibration. Simple room temperature electronics readily permit the observation of the five narrow and highly reproducible superconducting phase transitions. These phase transitions have been assigned temperature values by means of fundamental thermometers used at the National Bureau of Standards. Provided that care is exercised in reducing the magnetic field acting upon the device, the user can confidently expect to achieve a temperature reproducibility and traceability to the NBS temperature scale of plus or minus 0.3 mK.

  5. Certified Rule Labeling

    OpenAIRE

    Nagele, Julian; Zankl, Harald

    2015-01-01

    The rule labeling heuristic aims to establish confluence of (left-)linear term rewrite systems via decreasing diagrams. We present a formalization of a confluence criterion based on the interplay of relative termination and the rule labeling in the theorem prover Isabelle. Moreover, we report on the integration of this result into the certifier CeTA, facilitating the checking of confluence certificates based on decreasing diagrams for the first time. The power of the method is illustrated by ...

  6. Investigation on homogeneity within micro-areas of IAEA urban dust reference materials by SPM technique

    International Nuclear Information System (INIS)

    In order to develop new reference materials for microanalytical nuclear techniques, a scanning proton microprobe (SPM) was used to determine homogeneity level within 100 μm x 200 μm micro-areas of the IAEA Urban Dust Reference Materials. The experimental methods are described and the results discussed

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

    International Nuclear Information System (INIS)

    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 241Am 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 241Am and 137Cs. 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)

  8. Development of reference materials for SNF NDA systems

    International Nuclear Information System (INIS)

    The Department of Energy has over 200 different fuel types which will be placed in a geologic repository for ultimate disposal. At the present time, DOE EM is responsible for assuring safe existing conditions, achieving interim storage, and preparing for final disposition. Each task is governed by regulations which dictate a certain degree of knowledge regarding the contents and condition of the fuel. This knowledge and other associated characteristics are referred to as data needs. It is the stance of DOE EM, that personnel and economic resources are not available to obtain the necessary data to characterize such individual fuel type for final disposal documentation purposes. In addition, it is beyond the need of DOE to do so. This report describes the effort to classify the 200+ fuel types into a subset of fuel types for the purpose of non-destructive analysis (NDA) measurement system development and demonstration testing in support of the DOE National Spent Nuclear Fuel (NSNFP) Program. The fuel types have been grouped into 37 groups based on fuel composition, fuel form, assembly size, enrichment, and other characteristics which affect NDA measurements (e.g., neutron poisons)

  9. Development of reference materials for SNF NDA systems

    Energy Technology Data Exchange (ETDEWEB)

    Klann, R. T.

    2000-02-29

    The Department of Energy has over 200 different fuel types which will be placed in a geologic repository for ultimate disposal. At the present time, DOE EM is responsible for assuring safe existing conditions, achieving interim storage, and preparing for final disposition. Each task is governed by regulations which dictate a certain degree of knowledge regarding the contents and condition of the fuel. This knowledge and other associated characteristics are referred to as data needs. It is the stance of DOE EM, that personnel and economic resources are not available to obtain the necessary data to characterize such individual fuel type for final disposal documentation purposes. In addition, it is beyond the need of DOE to do so. This report describes the effort to classify the 200+ fuel types into a subset of fuel types for the purpose of non-destructive analysis (NDA) measurement system development and demonstration testing in support of the DOE National Spent Nuclear Fuel (NSNFP) Program. The fuel types have been grouped into 37 groups based on fuel composition, fuel form, assembly size, enrichment, and other characteristics which affect NDA measurements (e.g., neutron poisons).

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

    International Nuclear Information System (INIS)

    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

  11. Critical Evaluation of an Intercalibration Project Focused on the Definition of New Multi-Element Soil Reference Materials (AMS-MO1 and AMS-ML1

    Directory of Open Access Journals (Sweden)

    Livia Vittori Antisari

    2014-12-01

    Full Text Available Soils are complex matrices and their geochemical investigation necessarily needs reliable Certified Reference Materials (CRMs, i.e. standards, to support analytical precision and accuracy. In particular, the definition of soil multi-element CRMs is particularly complex and involves an inter-laboratory program that employs numerous analytical techniques. In this study, we present the results of the inter-calibration experiment focused on the certification of two new soil standards named AMS-ML1 and AMS-MO1. The two soils developed on sandstone and serpentinite parent materials, respectively. The experiment involved numerous laboratories and focused on the evaluation of soil physicochemical parameters and geochemical analyses of major and trace elements by X-ray fluorescence (XRF and Inductive Coupled Plasma techniques (ICP-OES and ICP-MS. The data was statistically elaborated. Three levels of repeatability and accuracy in function of the different analytical methods and instrumentation equipment was observed. The statistical evaluation of the results obtained by ICP-OES on Aqua Regia extracts (i.e., Lilliefors test for normally, Grubbs test for outliers, Cochran test for outliers in variances and ANOVA allowed to computed some certified values for the two proposed soil standards. This preliminary study will represent the first step of a more thorough intercalibration ring-test involving a higher number of laboratories, in order to propose the investigated matrices as CRMs.

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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

  14. Simultaneous determination of inorganic mercury, methylmercury, and total mercury concentrations in cryogenic fresh-frozen and freeze-dried biological reference materials

    Energy Technology Data Exchange (ETDEWEB)

    Point, David; Davis, W.C.; Christopher, Steven J.; Becker, Paul R. [National Institute of Standards and Technology, Analytical Chemistry Division, Hollings Marine Laboratory, Charleston, SC (United States); Garcia Alonso, J.I. [University of Oviedo, Department of Physical and Analytical Chemistry, Faculty of Chemistry, Oviedo (Spain); Monperrus, Mathilde; Donard, Olivier F.X. [Equipe de Chimie Analytique Bio-Inorganique et Environnement - UMR 5254, Institut Pluridisciplinaire de Recherche sur l' Environnement et les Materiaux, Pau (France); Wise, Stephen A. [National Institute of Standards and Technology, Analytical Chemistry Division, Gaithersburg, MD (United States)

    2007-10-15

    Two speciated isotope dilution (SID) approaches consisting of a single-spike (SS) method and a double-spike (DS) method including a reaction/transformation model for the correction of inadvertent transformations affecting mercury species were compared in terms of accuracy, method performance, and robustness for the simultaneous determination of methylmercury (MeHg), inorganic mercury (iHg), and total mercury (HgT) concentrations in five biological Standard Reference Materials (SRMs). The SRMs consisted of oyster and mussel tissue materials displaying different mercury species concentration levels and different textural/matrix properties including freeze-dried (FD) materials (SRMs 1566b, 2976, and 2977) and cryogenically prepared and stored fresh-frozen (FF) materials (SRMs 1974a, 1974b). Each sample was spiked with {sup 201}iHg (Oak Ridge National Laboratory, ORNL) and Me{sup 202}Hg (Institute for Reference Materials and Measurements. IRMM-670) solutions and analyzed using alkaline microwave digestion, ethylation, and gas chromatography inductively coupled plasma mass spectrometry (GC/ICP-MS). The results obtained by the SS-SID method suggested that FF and FD materials are not always commutable for the simultaneous determination of iHg, MeHg, and HgT, due to potential transformation reactions resulting probably from the methodology and/or from the textural/matrix properties of the materials. These transformations can occasionally significantly affect mercury species concentration results obtained by SS-SID, depending on the species investigated and the materials considered. The results obtained by the DS-SID method indicated that the two classes of materials were commutable. The simultaneous and corrected concentrations of iHg, MeHg, and HgT obtained by this technique were not found to be statistically different form the certified and reference concentration together with their expanded uncertainty budgets for the five SRMs investigated, exemplifying the robustness

  15. Reference materials for nondestructive assay of special nuclear material. Volume 2. Thin metal foils of highly enriched uranium

    International Nuclear Information System (INIS)

    This report describes the fabrication of reference materials for use in gamma-ray-based nondestructive assay of small high-density uranium samples. The sample containers are small Petri dishes. The reference materials consist of thin circular discs of highly enriched uranium metal foil. The 235U content ranges from 0.2 to 10 g. The report also describes the assay procedure used with low-resolution detectors

  16. Embrapa's experience in the production and development of agriculture reference materials

    Science.gov (United States)

    Nogueira, A. R. A.; Souza, G. B.; Bossu, C. M.; Bianchi, S. R.; Verhalen, T. R.; Silva, P. T.; Peixoto, A. A. J.; Silva, C. S.

    2016-07-01

    The main challenge of Embrapa is to develop a model of genuine Brazilian tropical agriculture and livestock. To get this task, the quality of laboratories results is mandatory, increasing the demand for reference materials. Projects were proposed to produce reference materials to support the national agriculture laboratories and consolidate a network able to perform reliable and reproducible analytical testing laboratory within the internationally standards required. Reference materials were produced and available to interested laboratories and collaborative tests were conducted to obtain consensus values. The results and statistical evaluations were performed with the use of software developed by Embrapa Pecuaria Sudeste.

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

    International Nuclear Information System (INIS)

    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)

  18. 78 FR 58567 - Criteria to Certify Coal Mine Rescue Teams

    Science.gov (United States)

    2013-09-24

    ... Safety and Health Administration Criteria to Certify Coal Mine Rescue Teams AGENCY: Mine Safety and... mine rescue team training. MSHA prescribes training materials through the issuance of instruction guides. Existing standards for coal mine rescue teams include criteria for mine operators to certify...

  19. Micro-homogeneity of candidate reference materials: Results from an intercomparison study for the Analytical Quality Control Services (AQCS) of the IAEA

    International Nuclear Information System (INIS)

    The IAEA Analytical Quality Control Services (AQCS) has made available two single cell algae materials IAEA-392 and IAEA-393 as well as an urban dust IAEA-396 to study their use for analytical sample sizes in the milligram range and below. Micro-analytical techniques such as PIXE and μ-PIXE, solid sampling AAS, scanning electron microprobe X-ray analysis and INAA were applied to the determination of trace elements on the basis of μg to mg amounts of the selected materials. The comparability of the mean values as well as the reproducibility of successive measurements is being evaluated in order to compare relative homogeneity factors for many elements in the investigated materials. From the reported results it seems that the algae materials IAEA-392 and IAEA-393 are extremely homogeneous biological materials for a number of elements with an extraordinary sharp particle size distribution below 10 μm. A similar situation seems to hold for the urban dust material IAEA-396 which had been air-jet milled to a particle size distribution around 4 μm. The introduction of these materials as CRMs with very small amounts needed to determine the certified concentrations will help to meet the needs of micro-analytical techniques for natural matrix reference materials. (author)

  20. Development of an orange juice in-house reference material and its application to guarantee the quality of vitamin C determination in fruits, juices and fruit pulps.

    Science.gov (United States)

    Valente, A; Sanches-Silva, A; Albuquerque, T G; Costa, H S

    2014-07-01

    Reference materials are useful for the quality control of analytical procedures and to evaluate the performance of laboratories. There are few and expensive certified reference materials commercially available for vitamin C or ascorbic acid analysis in food matrices. In this study, the preparation and the suitability assessment of an orange juice in-house reference material (RM) for vitamin C analysis in fruits, juices and in fruit pulps is described. This RM was used for the development and full validation of an HPLC method. The results showed excellent linearity (r(2)=0.9995), good accuracy (96.6-97.3%) and precision, as relative standard deviation, ranged from 0.70% to 3.67%. The in-house RM was homogenous and stable at storage conditions (-80°C) during 12 months. According to our results, this in-house RM is an excellent tool to use in quality control and method verification purposes for vitamin C analysis of fruits, juices and fruit pulps matrices. Furthermore, a stabilization solution with perchloric and metaphosphoric acids was developed which prevents degradation of ascorbic acid for a period of 12 months at -80°C. PMID:24518317

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

    International Nuclear Information System (INIS)

    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, δ-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)

  2. Use of neutron activation analysis and LC-ICP-MS in the development of candidate reference materials for As species determination

    International Nuclear Information System (INIS)

    Arsenic (As) is widely found in marine organisms, mainly as organic arsenical compounds. With the introduction of regulations for As species in foodstuffs and for environmental control, it has become more important to quantify the amount of arsenic species present. To address this concern new reference materials (RMs) for validation and quality assurance of As speciation measurements are being developed, including a tuna fish tissue and a robalo liver tissue. Instrumental neutron activation analysis (INAA) is used in this work as a proven analytical tool for As determinations and for validating the As mass fraction determined by liquid chromatography coupled to inductively coupled mass spectrometry (LC-ICP-MS) in extracts of the candidate RMs and other fish samples including certified RMs. Various methods for the extraction of water-soluble As species were evaluated. The best results were acquired after methanol/acetone/water extraction yielding in 93 % extractable As in the tuna RM. This procedure was used for the LC-ICP-MS studies. The results demonstrate that INAA can account for 100 % of the distribution of As species in analytical processes. It complements LC-ICP-MS for the validation of the characterization of As species in the development of RMs for such species. Excellent agreement of measured results in certified RMs with the reported values confirms the validity of the applied procedures. (author)

  3. SI-traceable measurement of methylmercury in tuna by species-specific isotope dilution with a 202Hg isotopically enriched methylmercury reference material

    International Nuclear Information System (INIS)

    The Comite Consultatif pour la Quantite de Matiere, CCQM, from the International Committee for Weights and Measures, has the tasks to co-ordinate the activities of national metrology laboratories in establishing traceability of measurements to the SI and to stimulate understanding of the concept of uncertainty and assignment of uncertainty statements to measurements. CCQM working groups develop and execute international comparisons to establish the technical basis for the mutual recognition of measurement capabilities. In 2003, IRMM, the metrology institute of the European Commission, launched CCQM pilot study 39 on the measurement of As, Se, Pb, Hg and CH3Hg in tuna. The aims were to strengthen the comparability of measurements EU member states are obliged to make under EC regulation 466/2001 (monitoring of contaminants in food) on the total element contents, and to evaluate the comparability of CH3Hg measurement with new measurement techniques. At the CCQM level, it is necessary to produce measurements for all analytes through processes with established traceability to the SI and with uncertainty statements. The IRMM contribution to CCQM-P39 for the determination of the tuna's CH3Hg amount content was based on species specific isotope dilution mass spectrometry applied as a primary method of measurement. IRMM-670, a newly developed 202Hg enriched CH3Hg isotopic reference material, was blended to the tuna sample, from which Hg species were extracted and derivatised to non-polar forms. Gas chromatography inductively coupled plasma mass spectrometry, GC-ICP-MS, was used for Hg species separation and detection of the n(200Hg)/n(202Hg) ratio in the CH3Hg of the blended material. The SI-traceable CH3Hg amount content was then obtained through comparison using an IDMS equation with the IRMM-670 reference CH3Hg amount content (including the isotopic compositions of natural Hg recommended by IUPAC, and certified for CH3Hg in IRMM-670). IRMM-639, a natural-like Hg

  4. Chemical quality control of plutonium fuels: potassium plutonium sulphate as a reference material

    International Nuclear Information System (INIS)

    Potassium plutonium sulphate, K4Pu(SO4)4 prepared in our division has been proposed as a reference material for plutonium. The suitability of the material as a reference standard in the quality assurance of plutonium fuels has been demonstrated by its regular use in our laboratory over the past six months. Results of the analysis of the standard by potentiometric and biamperometric methods were in close agreement with the theoretical plutonium content. (author)

  5. Biological reference materials in routine analysis: Results from the German Food Contamination Monitoring Programme

    Energy Technology Data Exchange (ETDEWEB)

    Schauenburg, H.; Weigert, P. (Bundesgesundheitsamt, Berlin (Germany, F.R.))

    1990-10-01

    Within the research project 'German Food Contamination Monitoring Programme', selected foodstuffs have to be examined by the official food control laboratories. Contents of pesticides and heavy metals have to be determined by means of routine analysis. Biological reference materials are used in collaborative studies and in parallel investigations for analytical quality assurance. Using lead as an example, results obtained for three reference materials are discussed. (orig.).

  6. Quantitative analysis of trace elements in environmental powders with laser ablation inductively coupled mass spectrometry using non-sample-corresponding reference materials for signal evaluation

    Science.gov (United States)

    Bauer, Gerald; Limbeck, Andreas

    2015-11-01

    Laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) is an attractive alternative to traditional procedures for the analysis of environmental samples (i.e., conventional liquid measurement after sample digestion). However, for accurate quantification, certified reference materials (CRM) are necessary which match the composition of the sample and include all elements of interest at the required concentration levels. The limited availability of appropriate CRMs hampers therefore substantial application. In this work, an LA-ICP-MS procedure allowing for accurate determination of trace element contents in powdered environmental samples is presented. For LA-ICP-MS analysis, the samples are mixed with an internal standard (silver oxide) and a binder (sodium tetra borate) and subsequently pressed to pellets. Quantification is accomplished using a calibration function determined using CRMs with varying matrix composition and analyte content, pre-treated and measured in the same way as the samples. With this approach, matrix-induced ablation differences resulting from varying physical/chemical properties of the individual CRMs could be compensated. Furthermore, ICP-related matrix-effects could be minimized using collision/reaction cell technology. Applicability of the procedure has been demonstrated by assessment of Cd, Cu, Ni, and Zn in four different environmental CRMs (NIST SRM1648a (urban particulate matter), NIST SRM2709 (San Joaquin Soil), BCR144 (sewage sludge), and BCR723 (road dust)). Signal evaluation was performed by alternative use of three CRMs for calculation of the calibration function whereas the remaining fourth CRM acted as unknown sample, resulting in a good agreement between measured and certified values for all elements and reference materials.

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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: 60Co≤4.6%, 134Cs≤4.7%, 137Cs≤5.0%, total β≤0.6% and 3H≤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

  10. Certificate of Analysis, Standard Reference Material® 1849, Infant/Adult Nutritional Formula

    Science.gov (United States)

    Standard Reference material (SRM) 1849 is intended primarily for validation of methods for determining proximates, fatty acids, vitamins, elements and nucleotides in infant and adult nutritional formulas and similar materials. This SRM can also be used for quality assurance when assigning values to ...

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

    International Nuclear Information System (INIS)

    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

  12. List of reference materials for non-destructive assay of U, Th and Pu isotopes

    International Nuclear Information System (INIS)

    A list of reference materials for non-destructive assay has been compiled within six countries of the EEC, the Commission and the IAEA with the assistance of the members of the Esarda working group on NDA. The reference materials have been tabulated according to the type of fuel cycle (HEU, LEU, Pu) and type of fuel. For each material the following data are given: the chemical composition, the nominal value or the range in quantity of the element, the U235 enrichment or isotopic composition, the physical form and number of pieces

  13. The use of BIM reference models for multi-material structural design

    OpenAIRE

    Djedović, Sanel

    2014-01-01

    Master thesis deals with multi-material structural design that is based on reference architectural model. We performed process and product analysis that is relevant for multi-material structural design and proposed and demonstrated its use for three construction materials (concrete, steel and wood) In the frames of process analysis we used IDEFØ methodology to describe AS-IS structural design. A detailed description of process models of existing design procedures for building permit and pr...

  14. Using ICP-qMS to trace the uptake of nanoscale titanium dioxide by microalgae-potential disadvantages of vegetable reference material.

    Science.gov (United States)

    Potouridis, Theodoros; Völker, Johannes; Alsenz, Heiko; Oetken, Matthias; Püttmann, Wilhelm

    2014-04-01

    As nanoscale materials have gained in economic importance over recent years, concerns about accumulation in the environment and, consequently, analysis of nanoparticles in biological material have increasingly become the focus of scientific research. A nanomaterial used in a wide range of food, consumer and household products is titanium dioxide (nTiO2). Monitoring of nTiO2 via determination of elemental titanium (Ti) can be very challenging because of a variety of possible interferences. This work describes problems during the development of a quantification method for titanium dioxide (TiO2) using inductively coupled plasma-quadrupole mass spectrometry (ICP-qMS). To evaluate the analytical method, certified vegetable reference material NCS DC 73349 was used. Interestingly, measurements of NCS DC 73349 seemed to result in acceptable recovery values-however, this was without considering interferences or conceivable differences in the natural isotopic abundance of the certified titanium calibration solution and NCS DC 73349. Actually, recoveries were lower than initially assumed. The potential interferences causing augmented recovery could be attributed to the presence of the elements sulfur (S) and phosphorus (P), which were able to form oxide ions and nitrogen-interfering species. The effect of such interfering cluster ions could be prevented by dry ashing as a sample preparation step, to evaporate S and P, before digestion with aqua regia in a high-pressure asher (HPA). Final practicability of the analysis method was proved by monitoring the uptake of nTiO2 by the microalgae Scenedesmus acutus in an environmental exposure study. PMID:24604322

  15. 40 CFR 161.175 - Certified limits.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Certified limits. 161.175 Section 161... Certified limits. The applicant must propose certified limits for the ingredients in the product. Certified limits become legally binding limits upon approval of the application. Certified limits will apply to...

  16. IFCC primary reference procedures for the measurement of catalytic activity concentrations of enzymes at 37 degrees C. International Federation of Clinical Chemistry and Laboratory Medicine. Part 7. Certification of four reference materials for the determination of enzymatic activity of gamma-glutamyltransferase, lactate dehydrogenase, alanine aminotransferase and creatine kinase accord.

    Science.gov (United States)

    Siekmann, Lothar; Bonora, Roberto; Burtis, Carl A; Ceriotti, Ferruccio; Clerc-Renaud, Pascale; Férard, Georges; Ferrero, Carlo A; Forest, Jean-Claude; Franck, Paul F H; Gella, F-Javier; Hoelzel, Wieland; Jørgensen, Poul Jørgen; Kanno, Takashi; Kessner, Art; Klauke, Rainer; Kristiansen, Nina; Lessinger, Jean-Marc; Linsinger, Thomas P J; Misaki, Hideo; Mueller, Mathias M; Panteghini, Mauro; Pauwels, Jean; Schiele, Françoise; Schimmel, Heinz G; Vialle, Arlette; Weidemann, Gerhard; Schumann, Gerhard

    2002-07-01

    This paper is the seventh in a series dealing with reference procedures for the measurement of catalytic activity concentrations of enzymes at 37 degrees C and the certification of reference preparations. Other parts deal with: Part 1. The Concept of Reference Procedures for the Measurement of Catalytic Activity Concentrations of Enzymes; Part 2. Reference Procedure for the Measurement of Catalytic Concentration of Creatine Kinase; Part 3. Reference Procedure for the Measurement of Catalytic Concentration of Lactate Dehydrogenase; Part 4. Reference Procedure for the Measurement of Catalytic Concentration of Alanine Aminotransferase; Part 5. Reference Procedure for the Measurement of Catalytic Concentration of Aspartate Aminotransferase; Part 6. Reference Procedure for the Measurement of Catalytic Concentration of Gamma-Glutamyltransferase. A document describing the determination of preliminary reference values is also in preparation. The certification of the catalytic activity concentrations as determined by the recently elaborated IFCC primary reference methods at 37 degrees C of four enzyme preparations, namely IRMM/IFCC 452 (gamma-glutamyltransferase), IRMM/IFCC 453 (lactate dehydrogenase 1), IRMM/IFCC 454 (alanine aminotransferase) and IRMM/IFCC 455 (creatine kinase) is described. Homogeneity data were derived from previous results. Stability was assessed using recently obtained data as well as data from previous stability studies. The collaborative study for value assignment was performed under a strict quality control scheme to ensure traceability to the primary reference method. Uncertainty of the materials was assessed in compliance with the Guide to the Expression of Uncertainty in Measurement. The certified values obtained at 37 degrees C are 1.90 microkat/l +/- 0.04 microkat/l (114.1 U/l +/- 2.4 U/l), for gamma-glutamyltransferase, 8.37 microkat/l +/- 0.12 microkat/l (502 U/l +/- 7 U/l), for lactate dehydrogenase 1, 3.09 microkat/l +/- 0.07 microkat

  17. Tailored graphitized soot as reference material for EC/OC measurement validation

    Directory of Open Access Journals (Sweden)

    O. Popovicheva

    2011-05-01

    Full Text Available The lack of standard reference materials for calibrating, troubleshooting and intercomparing techniques that measure the composition of black carbon, commonly referred to as soot, has been a major obstacle that hinders improved understanding of how climate and health is impacted by this ubiquitous component of the atmosphere. A different approach is offered here as a means of constructing precisely controlled material with fractions of organic carbon (OC on the surface of elemental carbon (EC whose structure reflects that of the combustion produced particles found in the atmosphere. The proposed soot reference material (SRM uses EC as a basis substrate for surface coatings of organic compounds that are representative of the main classes of organics identified in the coverage of soot produced by fossil fuel burning. A number of methods are used to demonstrate the quality and stability of the reference EC and SRM. Comparison of the nominal fraction of OC deposited on the EC substrate with the fraction measured with thermal/optical analysis (TOA shows excellent agreement. Application of this type of reference material for evaluating the different methods of carbon analysis may help resolve differences that currently exist between comparable measurement techniques when trying to separate OC and EC from ambient samples.

  18. Instrumental neutron activation analysis for the certification of biological reference materials

    International Nuclear Information System (INIS)

    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

  19. 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.

  20. Certification of total arsenic in blood and urine standard reference materials by radiochemical neutron activation analysis and inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Radiochemical neutron activation analysis (RNAA) was used to measure arsenic at four levels in standard reference material (SRM) 955c Toxic Elements in Caprine Blood and at two levels in SRM 2668 Toxic Elements in Frozen Human Urine for the purpose of providing mass concentration values for certification. Samples were freeze-dried prior to analysis followed by neutron irradiation for 3 h at a fluence rate of 1 × 1014 cm-2 s-1. After sample dissolution in perchloric and nitric acids, arsenic was separated from the matrix either by retention on hydrated manganese dioxide (urine) or by extraction into zinc diethyldithiocarbamate in chloroform (blood). 76As was quantified by gamma-ray spectroscopy. Differences in chemical yield and counting geometry between samples and standards were monitored by measuring the count rate of a 77As tracer added before sample dissolution. RNAA results were combined with inductively coupled plasma-mass spectrometry values from National Institute of Standards and Technology and collaborating laboratories to provide certified values of 10.81 ± 0.54 and 213.1 ± 0.73 μg/L for SRM 2668 Levels I and II, and certified values of 21.66 ± 0.73, 52.7 ± 1.1, and 78.8 ± 4.9 μg/L for SRM 955c Levels II-IV, respectively. Because of discrepancies between values obtained by different methods for SRM 955c Level I, an information value of <5 μg/L was assigned for this material. (author)

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

    International Nuclear Information System (INIS)

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

  2. A new 202Hg isotopically enriched methylmercury spike material with SI-traceable reference values for isotope dilution measurements in biological and environmental samples

    International Nuclear Information System (INIS)

    HgO enriched in 202Hg was used for the preparation of a solution of 202Hg enriched CH3Hg. The CH3HgCl was synthesised by reaction with a Grignard reagent and a subsequent comproportionation reaction between dimethylmercury, (CH3)2Hg, and HgCl2, that was optimised to give a high yield of the product, pure from other Hg species and by-products of the synthesis reaction. To prepare the CH3HgCl for use as an IDMS spike, it was dissolved in 2 % ethanol. The spike was thereby maintained in a relatively reactive form without solution preservatives that might alter its chemical behaviour compared to incipient CH3Hg in a sample. Aliquots were sealed in quartz ampoules and a 1-year stability study was undertaken by storing a series of ampoules under different temperature conditions to all be measured on the same occasion (an isochronous study) and by retaining a portion of the solution in a closeable bottle under recommended storage conditions, with measurements at 3-month intervals. The Hg amount content in the form of CH3Hg was obtained by subtraction of the inorganic Hg amount content (determined by gas chromatography inductively coupled plasma mass spectrometry, GC-ICP-MS) from the total Hg amount content (determined by blending with IRMM-639, a natural Hg isotopic certified reference material, ICRM, and isotope dilution mass spectrometry of the digested material). Only CH3Hg and inorganic Hg were detectable in the reference material with inorganic Hg in 3Hg was identical to that of IRMM-640, an inorganic Hg ICRM prepared from the same 202Hg enriched HgO, within enlarged uncertainty statements. These processes allowed the SI-traceable certification of both the amount content of CH3Hg and its isotopic composition, accompanied by combined uncertainty statements estimated according to ISO/GUM. The final uncertainty on the Hg amount content in the form of CH3Hg (3.5 % relative, k=2) included a contribution covering for potential changes over 2 years of shelf-life. No

  3. 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. PMID:27216677

  4. Testing of IAEA standard reference materials by Research and Development Institute, Czechoslovak Uranium Industry

    International Nuclear Information System (INIS)

    The Institute have partaken of attestations for a number of years. It has thus obtained a number of reference materials and could completely test the accuracy of the analytical methods used. The materials being tested included uranium and thorium ores, milk, whey, sea sediments and algae. The methods used included X-ray fluorescence analysis, high resolution gamma spectrometry, atomic absorption spectrometry, radiometric methods. Uranium was determined by spectrophotometry using Arsenazo III. (M.D.). 2 tabs., 17 refs

  5. Material Deprivation, Economic Stress and Reference Groups in Europe: An Analysis of EU-SILC2009

    OpenAIRE

    Whelan, Christopher T.; Bertrand Maître

    2012-01-01

    In this paper we take advantage of the recent availability of data from the special module on material deprivation in the 2009 European Union Statistics on Income and Living Conditions (EU-SILC) to develop a more comprehensive understanding of the relationship between material deprivation and economic stress, the mediating role played by cross-national differences in levels of income and income inequality and the implications for competing perspectives on the nature of reference groups in Eur...

  6. ENERGY STAR Certified Pool Pumps

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 1.0 ENERGY STAR Program Requirements for Pool Pumps that are effective as of February...

  7. ENERGY STAR Certified Imaging Equipment

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 2.0 ENERGY STAR Program Requirements for Imaging Equipment that are effective as of...

  8. ENERGY STAR Certified Audio Video

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 3.0 ENERGY STAR Program Requirements for Audio Video Equipment that are effective as of...

  9. ENERGY STAR Certified Ventilating Fans

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 4.0 ENERGY STAR Program Requirements for Ventilating Fans that are effective as of...

  10. ENERGY STAR Certified Water Heaters

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 3.0 ENERGY STAR Program Requirements for Water Heaters that are effective April 16,...

  11. ENERGY STAR Certified Roof Products

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 2.3 ENERGY STAR Program Requirements for Roof Products that are effective as of July 1,...

  12. ENERGY STAR Certified Water Coolers

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 2.0 ENERGY STAR Program Requirements for Water Coolers that are effective as of February...

  13. ENERGY STAR Certified Vending Machines

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 3.0 ENERGY STAR Program Requirements for Refrigerated Beverage Vending Machines that are...

  14. ENERGY STAR Certified Commercial Fryers

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 2.0 ENERGY STAR Program Requirements for Commercial Fryers that are effective as of...

  15. ENERGY STAR Certified Ceiling Fans

    Data.gov (United States)

    U.S. Environmental Protection Agency — Certified models meet all ENERGY STAR requirements as listed in the Version 3.0 ENERGY STAR Program Requirements for Ceiling Fans that are effective as of April 1,...

  16. Survey of inorganic arsenic in marine animals and marine certified reference materials by anion exchange high-performance liquid chromatography-inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Sloth, Jens Jørgen; Larsen, Erik Huusfeldt; Julshamn, Kåre

    2005-01-01

    A method for the determination of inorganic arsenic in seafood samples using high-performance liquid chromatography-inductively coupled plasma mass spectrometry is described. The principle of the method relied on microwave-assisted alkaline dissolution of the sample, which at the same time oxidized...... arsenite [As(Ill)] to arsenate [As(V)], whereby inorganic arsenic could be determined as the single species As(V). Anion exchange chromatography using isocratic elution with aqueous ammonium carbonate as the mobile phase was used for the separation of As(V) from other coextracted organoarsenic compounds...

  17. Human urine certified reference material CZ 6010: creatinine and toluene metabolites (hippuric acid and o-cresol) and a benzene metabolite (phenol)

    Czech Academy of Sciences Publication Activity Database

    Šperlingová, I.; Dabrowská, L.; Stránský, V.; Kučera, Jan; Tichý, M.

    2007-01-01

    Roč. 387, č. 7 (2007), s. 2419-2424. ISSN 1618-2642 Institutional research plan: CEZ:AV0Z10480505 Keywords : toluene metabolites * benzene metabolite * human urine Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 2.867, year: 2007

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

    International Nuclear Information System (INIS)

    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

  19. Certifying controls and systems software

    OpenAIRE

    Feron, Eric; Roozbehani, Mardavij

    2007-01-01

    Software system certification presents itself with many challenges, including the necessity to certify the system at the level of functional requirements, code and binary levels, the need to chase down run-time errors, and the need for proving timing properties of the eventual, compiled system. This paper illustrates possible approaches for certifying code that arises from control systems requirements as far as stability properties are concerned. The relative simplicity of the certification p...

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

    International Nuclear Information System (INIS)

    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 2H, 13C, 15N and 18O. Results were submitted by forty participants in twenty countries. 2 refs, 13 figs, 18 tabs

  1. Future needs and requirements for AMS C-14 standards and reference materials

    NARCIS (Netherlands)

    Scott, EM; Boaretto, E; Bryant, C; Cook, GT; Gulliksen, S; Harkness, DD; Heinemeier, J; McGee, E; Naysmith, P; Possnert, G; van der Plicht, H; van Strydonck, M; Cook, Gordon T.

    2004-01-01

    C-14 measurement uses a number of standards and reference materials with different properties. Historically the absolute calibration of C-14 measurement was tied to 1890 wood, through the 'primary' standard of NBS-OxI (produced by the National Bureau of Standards, now NIST - National Institute of St

  2. The preparation of a reference material of South African zirconium concentrate from Richards Bay

    International Nuclear Information System (INIS)

    This report describes the preparation of a South African zirconium concentrate as an inernational reference material. The procedure for the selection of preferred values is outlined. Eleven laboratories contributed to the analytical programme, and 7 elements have been asssigned preferred values

  3. 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…

  4. 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

  5. DIRECT CALIBRATION OF GC/MS SYSTEMS USING SRM (STANDARD REFERENCE MATERIAL) GAS CYLINDERS

    Science.gov (United States)

    A cryogenic trapping system has been developed for use in calibrating GC/MS systems for the analysis of volatile organic compounds. This system provides for direct Standard Reference Material (SRM) traceability on data generated on gaseous samples. The cryogenic trap is a coil of...

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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 2500C 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

  8. Validation of reference materials for uranium radiochronometry in the frame of nuclear forensic investigations

    International Nuclear Information System (INIS)

    The results of a joint effort by expert nuclear forensic laboratories in the area of age dating of uranium, i.e. the elapsed time since the last chemical purification of the material are presented and discussed. Completely separated uranium materials of known production date were distributed among the laboratories, and the samples were dated according to routine laboratory procedures by the measurement of the 230Th/234U ratio. The measurement results were in good agreement with the known production date showing that the concept for preparing uranium age dating reference material based on complete separation is valid. Detailed knowledge of the laboratory procedures used for uranium age dating allows the identification of possible improvements in the current protocols and the development of improved practice in the future. The availability of age dating reference materials as well as the evolvement of the age dating best-practice protocol will increase the relevance and applicability of age dating as part of the tool-kit available for nuclear forensic investigations. - Highlights: • A methodology for preparing uranium age dating reference material was validated. • Detailed laboratory procedures for uranium age dating are summarized. • The difficulties and further developments of uranium age dating are demonstrated

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

    International Nuclear Information System (INIS)

    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

  10. Determination of operationally defined fractions of aluminium in reference materials and acid attacked environmental samples

    International Nuclear Information System (INIS)

    The aim of the presented work is to evaluate the selectivity of the operationally defined procedures for the aluminium fractionation in the reference materials and the environmental samples affected by the mining activity. The combination of the sequential optimized BCR (European Commission Community Bureau of Reference) three-step, the single (H2O, CaCl2, Na2S2O4, NH4F (NH4)2C2O4, HCl, NTA, EDTA, DTPA) and the solid phase chelating ion-exchange extraction procedures was performed for the aluminium fractionation in the samples. The amount of the reactive Al determined by the solid phase extraction on the chelating resin Iontosorb Salicyl is the most important operationally defined fraction of aluminium from the aspect of its negative effects on the environment. The available Al concentrations obtained from the different operationally defined fractionation methods were compared. The flame atomic absorption spectrometry was used for the aluminium quantification. The X-ray diffraction analyse of the samples was performed for the mineral composition determination. The precision, the repeatability and the accuracy for the all steps of the optimized BCR sequential extraction procedure were checked on six reference materials (SRM 2710, RSS SO-2, RSS SO-4, CRM SA-B, SRM RTH 912, CRM 025-050). The precision and the repeatability were very good with the R.S.D. values 11%. The fraction specific accuracy was excellent. The new indicative fractional Al values in the used reference materials are published

  11. 40 CFR 158.350 - Certified limits.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Certified limits. 158.350 Section 158... REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.350 Certified limits. The applicant must propose certified limits for the ingredients in the product. Certified limits become legally binding limits upon...

  12. 12 CFR 327.2 - Certified statements.

    Science.gov (United States)

    2010-01-01

    ... known as the quarterly certified statement invoice. Each insured depository institution shall file and certify its quarterly certified statement invoice in the manner and form set forth in this section. (2) The quarterly certified statement invoice shall reflect the institution's risk assignment,...

  13. Present status and strategic plan for the stable isotope reference materials at the IAEA.

    Science.gov (United States)

    Assonov, Sergey; Groening, Manfred

    2016-04-01

    The presentation will give the overview of the stable isotope reference materials (SI-RMs) under distribution by the IAEA, its stable isotope laboratory and capacities related to material testing & production as well as future plans. Historically, most of the IAEA reference materials were produced and made available via collaborations with expert stable isotope laboratories worldwide. The IAEA plans include several directions as follows: • Maintaining the scale-defining SI-RMs at the highest level and introducing adequate replacements when needed; • Monitoring existing SI-RMs for any potential alteration(s) and of isotopic values assigned; • Identifying and then addressing the needs for new SI-RMs, with the priority to address the most critical applications (environmental and climate related applications, human health, food safety studies) and newly emerging analytical isotope techniques; • Performing all measurements aimed for characterisation of new SI-RMs and the corresponding uncertainty evaluation in accordance to the latest metrological concepts; • Promoting metrological approaches on traceability and uncertainty evaluation in every day practice of stable isotope measurements; • Expanding the IAEA capacities for SI-RMs by (i) planning a renewed laboratory at IAEA; (ii) enlarging collaboration with expert laboratories aimed to help IAEA in production and characterisation of new SI-RMs. These major directions will help to address the increasing demand for Stable Isotope Reference Materials.

  14. Microwave-assisted extraction and quantitative LC/ID-MS measurement of total choline and free carnitine in food standard reference materials.

    Science.gov (United States)

    Phillips, Melissa M; Sander, Lane C

    2012-01-01

    The Stakeholder Panel on Infant Formula and Adult Nutritionals of AOAC INTERNATIONAL has declared both choline and carnitine to be priority nutrients in infant formulas, and ongoing efforts exist to develop or improve Official Methods of Analysis for these nutrients. As a result, matrix-based certified reference materials are needed with assigned values for these compounds. In this work, traditional acid and enzymatic hydrolysis procedures were compared to microwave-assisted acid hydrolysis, and conditions optimized to provide complete sample hydrolysis and recovery of total choline from four food standard reference materials (SRMs): whole milk powder, whole egg powder, infant formula, and soy flour. The extracts were analyzed using LC on a mixed-mode column (simultaneous RP and ion exchange) with isotope dilution-MS detection to achieve simultaneous quantification of total choline and free carnitine. Total choline has been determined in these four food matrixes with excellent precision (0.65 to 2.60%) and accuracy, as confirmed by use of SRM 1849 Infant/Adult Nutritional Formula as a control material. Free carnitine has been determined in two of these food matrixes with excellent precision (0.69 to 2.19%) and accuracy, as confirmed by use of SRM 1849 Infant/Adult Nutritional Formula as a control material. Limitations in simultaneous determination of total choline and free carnitine resulted from extreme differences in concentration of the two components in egg powder and soy flour (at least three orders of magnitude). Samples required dilution to prevent poor LC peak shape, which caused decreased precision in the determination of low concentrations of free carnitine. Despite this limitation, the described method yields results comparable to current AOAC Official Method 999.14 Choline in Infant Formula, with a decrease of more than 2 h in sample preparation time. PMID:23175983

  15. Exploration of optical fibres as a carrier for new benzene and toluene matrix-free reference materials

    OpenAIRE

    Słomińska, Marta; Marć, Mariusz; Szczygelska-Tao, Jolanta; Konieczka, Piotr; Namieśnik, Jacek

    2015-01-01

    To meet high expectations concerning precision and accuracy of reference materials, preparation of matrix-free reference materials using thermal decomposition-gas chromatography-mass spectrometry (TD-GC-MS) was proposed in this study. In the paper, the results obtained in preparation of the new reference materials for benzene and toluene are presented, based on the thermal decomposition technique of compounds chemically bound to the surface of optical fibre segments. The results obtained at v...

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

    International Nuclear Information System (INIS)

    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

  17. 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)

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

    International Nuclear Information System (INIS)

    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)

  19. Evaluation of the Community's research programme ''Nuclear measurements and reference materials'' (1980-1985)

    International Nuclear Information System (INIS)

    A panel has evaluated the research programme ''Nuclear measurements and reference materials'' performed by JRC-Geel, CBNM (Central Bureau for Nuclear Measurements) during the period 1980-85. Furthermore the panel has considered more general topics such as major facilities, staff and collaboration between JRC-Geel, CBNM and other organizations. Finally, the panel has discussed the future direction of the programme. The panel expressed its satisfaction with the scientific and technical quality of the work and recommended that JRC-Geel, CBNM should continue to play an important role in Europe in the fields of nuclear measurements and nuclear reference materials. The panel also recommended that the underlying research be strengthened and that the nuclear experience and expertise of JRC-Geel, CBNM be utilized for non-nuclear applications

  20. Filling the AOAC triangle with food-matrix standard reference materials.

    Science.gov (United States)

    Sharpless, Katherine E; Greenberg, Robert R; Schantz, Michele M; Welch, Michael J; Wise, Stephen A; Ihnat, Milan

    2004-03-01

    Well-characterized reference materials are needed by laboratories in the food testing and nutrition communities to facilitate compliance with nutritional labeling laws, to provide traceability for food exports needed for acceptance in many foreign markets, and to improve the accuracy of nutrition information that is provided to assist consumers in making sound dietary choices. As a result of the enactment of the Nutrition Labeling and Education Act of 1990 and the Infant Formula Act of 1980, the National Institute of Standards and Technology (NIST) has developed a suite of food-matrix Standard Reference Materials (SRMs) characterized for nutrient concentrations. These include SRM 1544 Fatty Acids and Cholesterol in a Frozen Diet Composite, SRM 1546 Meat Homogenate, SRM 1548a Typical Diet, SRM 1566b Oyster Tissue, SRM 1846 Infant Formula, SRM 1946 Lake Superior Fish Tissue, SRM 2383 Baby Food Composite, SRM 2384 Baking Chocolate, SRM 2385 Spinach, and SRM 2387 Peanut Butter. Many of these materials were developed at the request of the food industry to populate a nine-sectored fat-protein-carbohydrate triangle developed by AOAC International. With the completion of SRM 2387, SRMs representing each sector of the triangle are now available. These food-matrix reference materials are intended primarily for validation of analytical methods for the measurement of proximates, fatty acids, vitamins, minerals, and so on in foods of similar composition. They may also be used as "primary control materials" in the value-assignment of in-house, secondary, control materials to confirm accuracy as well as to establish traceability to NIST. PMID:14689156

  1. Applications of nuclear analytical techniques for multielement determination in reference materials and archaeological artifacts

    International Nuclear Information System (INIS)

    The paper presents applications of four nuclear analytical techniques namely INAA, PGNAA, PIGE and PIXE to ancient potteries as well as soil or sediment reference materials (RMs) obtained from IAEA. The methods are non-destructive in nature and capable of determining multi-elements at major to trace concentration levels. Methods have been applied to three clay potteries and two IAEA RMs namely Soil-7 and SL-3. (author)

  2. Reference Material Development for Paralytic Shellfish Poisoning Toxins and Associated Analytical Applications

    OpenAIRE

    Burrell, Stephen

    2015-01-01

    Food poisoning incidences relating to marine biotoxins are a global phenomenon and have the potential to severely impact the aquaculture industry. As a result, and as a legislative requirement in the European Union (EU), many countries have implemented monitoring programmes for these compounds but their success relies on the availability of certain quality assurance tools, two of which are reference materials (RMs) and proficiency testing. The limited amounts of RMs, in particular matrix cert...

  3. The NIMROC reference materials: revised values for thorium, yttrium, lanthanum, and the rare-earth elements

    International Nuclear Information System (INIS)

    This report gives all the analytical results submitted by the contributing laboratories before July 1983 for thorium, yttrium, lanthanum, and the rare-earth elements in the six NIMROC reference materials (SARM 1 to 6), which were prepared in 1966 by the former National Institute for Metallurgy, now the Council for Mineral Technology (Mintek). The statistical evaluation of these results and the assignment of new or revised recommended or provisional values are described

  4. The homogeneous determination of some standard reference materials using NAA and micro-PIXE

    International Nuclear Information System (INIS)

    The combined application techniques of NAA (Instrumental Neutron Activation) and Micro-PIXE (Proton Induced X-ray Emission) were used to determine homogeneity for minimum sample sizes lower than 10 mg of standard reference materials, including Tobacco Leaves (Poland), Spruce Shoots (Germany), Urban Dust (IAEA-396A/M and 396A/S) and Single Cell Algae (IAEA-393A). The experimental methods were described and the results were shown for further evaluation. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Schauenburg, H.; Weigert, P. (Bundesgesundheitsamt, Berlin (Germany). Centre for Surveillance and Health Evaluation of Environmental Chemicals (ZEBS))

    1992-04-01

    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.).

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

    International Nuclear Information System (INIS)

    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

  7. Synthesis and trace metal characterization of potassium plutonium sulphate: working reference material for plutonium

    International Nuclear Information System (INIS)

    An attempt was made to prepare potassium plutonium sulphate, which is proposed to be the working reference material for analyzing plutonium based fuel samples and associated materials. X-ray diffraction was employed for phase characterization and the structure was found to be monoclinic in nature with a space group of P21/c. Trace metallic impurity analyses was carried out for the 26 elements e.g. Ag, Al, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, Li, Mg, Mn, Mo, Na, Ni, Pb, Si, Sn, Sr, W, Zn, Dy, Eu, Sm and Gd using ICP-AES as well as D.C.Arc AES. (author)

  8. Collection and characterization of a bulk PM2.5 air particulate matter material for use in reference materials.

    Science.gov (United States)

    Heller-Zeisler, S F; Ondov, J M; Zeisler, R

    1999-01-01

    A contemporary PM2.5 (particulate matter smaller than 2.5 microns aerodynamic diameter) aerosol material from an urban site has been collected for the production of a new standard reference material that will be made available for the development of new PM2.5 air quality standards. Air particulate matter corresponding to the PM2.5 fraction was collected at an established Environmental Protection Agency monitoring site in Baltimore, Maryland. The air-sampling system that has been constructed for this collection separates fine particles with a cyclone separator and deposits them onto an array of Teflon membrane filters. The fine air particulate material is removed by ultrasonication or by mechanical means and collected for further preparation of standards. The composition of the collected PM2.5 aerosol, as well as the composition of the deposited PM2.5 aerosol, are determined by instrumental nuclear activation analysis and other techniques. PMID:10676493

  9. Candidate BCR reference materials for arsenic and selenium determinations in human serum and urine

    International Nuclear Information System (INIS)

    The pilot production of candidate reference materials for the quality assurance and statistical control of methods to determine toxic trace elements in biological samples is described. In the initial phase the project concerns a lyophilized human blood material containing Cd and Pb, a lyophilized human urine material containing As, Cd, Co and Cr, and a liquid human serum material with Al, Se and Zn at three different levels, representative of environmental and occupational exposure. The homogeneity and stability of the pilot batches were investigated by determining Al and Zn in serum, As in urine, Cd and Pb in blood at the medium level. The pilot batches produced were deemed to be homogeneous with respect to all the trace elements tested, and there was no indication of thermal instability except that the arsenic levels decreased significantly with time at 200 deg., 370 deg. and 450 deg. C. Thirty-two laboratories from 12 different countries participated in an intercomparison round organized to test the suitability of the reference material and validate the methodological approaches for certification purposes. Focusing on the neutron activation results, the outcome of this first intercomparison exercise demonstrates that the comparability of the calibration standards needs improvement. Therefore, for the certification round stronger efforts will be undertaken to document the spiked concentrations and to reduce their uncertainties, and the laboratories will be required to meet defined quality criteria for the checking and documentation of traceability. (author)

  10. A reference material for establishing uncertainties in full-field displacement measurements

    International Nuclear Information System (INIS)

    A simple reference material for establishing the minimum measurement uncertainty of optical systems for measuring 3D surface displacement fields in deforming objects is described and its use demonstrated by employing 3D digital image correlation as an exemplar technique. The reference material consists of a stepped bar, whose dimensions can be scaled to suit the application, and that can be clamped rigidly at its thick end to create an idealized cantilever. The cantilever was excited at resonance to generate out-of-plane displacements and, in a separate experiment, loaded statically in-plane to provide in-plane displacement fields. The displacements were measured using 3D digital image correlation and compared to the predicted displacement fields derived from tip deflections obtained using a calibrated transducer that provided traceability to the national standard for length. The minimum measurement uncertainties were evaluated by comparing the measured and predicted displacement fields, taking account of the uncertainties in the input parameters for the predictions. It was found that the minimum measurement uncertainties were less than 3% for the Cartesian components of displacement present during static in-plane bending and less than 3 µm for out-of-plane displacements during dynamic loading. It was concluded that this reference material was more straightforward to use, more versatile and yielded comparable results relative to an earlier design. (paper)

  11. Evaluation of homogeneity of selected reference materials for selenium by cyclic neutron activation analysis

    International Nuclear Information System (INIS)

    The homogeneity of four reference materials was evaluated for Se by cyclic instrumental neutron activation analysis (CINAA). The relative standard deviation for Se measurements at ppb levels by CINAA was <12% for NIST Wheat Flour (SRM 1567) in 5-10 mg samples, while it was <11% for Chinese Hair (HH-CH-1), <13% for IAEA Animal Muscle (H-4) and 25% for IAEA Animal Blood (A-13) in 50 mg samples. The highest relative subsampling uncertainties were observed in the mass range of samples ≤50 mg for Chinese Hair, ≤100 mg for Wheat Flour and Animal Muscle and ≤300 mg for Animal Blood. The results of a one-way analysis of variance indicate that all reference materials above these mass ranges are adequately homogeneous with respect to Se distribution. Our data suggest that these materials, except Animal Blood, can be used as reference standards for Se in quality assurance programs well below the sample masses recommended by the issuing agencies. (author) 14 refs.; 2 figs.; 5 tabs

  12. TOGAF 9 certified study guide

    CERN Document Server

    Group, The Open

    2010-01-01

    The TOGAF 9 certification program is a knowledge-based certification program. It has two levels, leading to certification for TOGAF 9 Foundation and TOGAF 9 Certified, respectively. The purpose of certification to TOGAF 9 Certified is to provide validation that, in addition to the knowledge and comprehension of TOGAF 9 Foundation level, the Candidate is able to analyze and apply this knowledge. The learning objectives at this level therefore focus on application and analysis in addition to knowledge and comprehension.This Study Guide supports students in preparation for the TOGAF 9 Part 2 Exam

  13. Developing a reference material for diffusion-controlled formaldehyde emissions testing.

    Science.gov (United States)

    Liu, Zhe; Liu, Xiaoyu; Zhao, Xiaomin; Cox, Steven S; Little, John C

    2013-11-19

    Formaldehyde, a known human carcinogen and mucous membrane irritant, is emitted from a variety of building materials and indoor furnishings. The drive to improve building energy efficiency by decreasing ventilation rates increases the need to better understand emissions from indoor products and to identify and develop lower emitting materials. To help meet this need, formaldehyde emissions from indoor materials are typically measured using environmental chambers. However, chamber testing results are frequently inconsistent and provide little insight into the mechanisms governing emissions. This research addresses these problems by (1) developing a reference formaldehyde emissions source that can be used to validate chamber testing methods for characterization of dynamic sources of formaldehyde emissions and (2) demonstrating that emissions from finite formaldehyde sources can be predicted using a fundamental mass-transfer model. Formaldehyde mass-transfer mechanisms are elucidated, providing practical approaches for developing diffusion-controlled reference materials that mimic actual sources. The fundamental understanding of emissions mechanisms can be used to improve emissions testing and guide future risk reduction actions. PMID:24102115

  14. Determination of perfluorinated alkyl acid concentrations in biological standard reference materials.

    Science.gov (United States)

    Reiner, Jessica L; O'Connell, Steven G; Butt, Craig M; Mabury, Scott A; Small, Jeff M; De Silva, Amila O; Muir, Derek C G; Delinsky, Amy D; Strynar, Mark J; Lindstrom, Andrew B; Reagen, William K; Malinsky, Michelle; Schäfer, Sandra; Kwadijk, Christiaan J A F; Schantz, Michele M; Keller, Jennifer M

    2012-11-01

    Standard reference materials (SRMs) are homogeneous, well-characterized materials used to validate measurements and improve the quality of analytical data. The National Institute of Standards and Technology (NIST) has a wide range of SRMs that have mass fraction values assigned for legacy pollutants. These SRMs can also serve as test materials for method development, method validation, and measurement for contaminants of emerging concern. Because inter-laboratory comparison studies have revealed substantial variability of measurements of perfluoroalkyl acids (PFAAs), future analytical measurements will benefit from determination of consensus values for PFAAs in SRMs to provide a means to demonstrate method-specific performance. To that end, NIST, in collaboration with other groups, has been measuring concentrations of PFAAs in a variety of SRMs. Here we report levels of PFAAs and perfluorooctane sulfonamide (PFOSA) determined in four biological SRMs: fish tissue (SRM 1946 Lake Superior Fish Tissue, SRM 1947 Lake Michigan Fish Tissue), bovine liver (SRM 1577c), and mussel tissue (SRM 2974a). We also report concentrations for three in-house quality-control materials: beluga whale liver, pygmy sperm whale liver, and white-sided dolphin liver. Measurements in SRMs show an array of PFAAs, with perfluorooctane sulfonate (PFOS) being the most frequently detected. Reference and information values are reported for PFAAs measured in these biological SRMs. PMID:22476786

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

    International Nuclear Information System (INIS)

    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 109 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)

  16. Estudo de homogeneidade de lote de material silício metálico candidato a material de referência Homogeneity testing of a lot of silicon metal prepared as a reference material

    OpenAIRE

    Queenie Siu Hang Chui; Celia Omine Iamashita; João Marcos de Almeida Bispo

    2005-01-01

    From the perspective of the uncertainties in chemical measurements all uncertainty sources should be part of the uncertainty of the reference material. When the primary methods are not available, interlaboratorial comparisons are used as a means of certification. The material to be distributed to the laboratories should have its homogeneity confirmed. The uncertainty due to this factor will be added to the characterization uncertainty. This work presents a homogeneity study of a lot of silico...

  17. CEH Certified Ethical Hacker Study Guide

    CERN Document Server

    Graves, Kimberly

    2010-01-01

    Prepare for the new version of CEH certification with this advanced guide. Once you learn the thought processes of unethical hackers, you can figure out how to secure your computer systems to defend against them. That's the philosophy behind ethical hacking, and it's a growing field. Prepare for certification in this important area with this advanced study guide that covers all exam objectives for the challenging CEH Certified Ethical Hackers exam. The book provides full coverage of exam topics, real-world examples, and a CD with additional materials for extra review and practice.:; Covers eth

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

    International Nuclear Information System (INIS)

    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)

  19. 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.

  20. Value assignment of nutrient concentrations in standard reference material 2384 baking chocolate.

    Science.gov (United States)

    Sharpless, Katherine E; Brown Thomas, Jeanice; Nelson, Bryant C; Phinney, Curtis S; Sieber, John R; Wood, Laura J; Yen, James H; Howell, Daniel W

    2002-11-20

    Standard Reference Material (SRM) Baking Chocolate was recently issued, and the process used for value assignment of nutrient concentrations is reported herein. SRM 2384 is intended for use as a primary control material for assigning values to in-house control materials and for validation of analytical methods for the measurement of fatty acids, proximates, vitamins, and elements in chocolate and similar high-fat matrices. The Certificate of Analysis for SRM 2384 provides assigned values for concentrations of fatty acids, proximates, vitamins, elements, and total dietary fiber, for which product labeling is required by the Nutrition Labeling and Education Act of 1990, as well as for catechins, caffeine, theobromine, and theophylline. These assigned values were based on measurements by NIST and/or collaborating laboratories. PMID:12428961

  1. REIMEP-22 inter-laboratory comparison. ''U Age Dating - determination of the production date of a uranium certified test sample''

    International Nuclear Information System (INIS)

    The REIMEP-22 inter-laboratory comparison aimed at determining the production date of a uranium certified test sample (i.e. the last chemical separation date of the material). Participants in REIMEP-22 on ''U Age Dating - Determination of the production date of a uranium certified test sample'' received one low-enriched 20 mg uranium sample for mass spectrometry measurements and/or one 50 mg uranium sample for a-spectrometry measurements, with an undisclosed value for the production date. They were asked to report the isotope amount ratios n(230Th)/n(234U) for the 20 mg uranium sample and/or the activity ratios A(230Th)/A(234U) for the 50 mg uranium sample in addition to the calculated production date of the certified test samples with its uncertainty. Reporting of the 231Pa/235U ratio and the respective calculated production date was optional. Eleven laboratories reported results in REIMEP-22. Two of them reported results for both the 20 mg and 50 mg uranium certified test samples. The measurement capability of the participants was assessed against the independent REIMEP-22 reference value by means of z- and zeta-scores in compliance with ISO 13528:2005. Furthermore a performance assessment criterion for acceptable uncertainty was applied to evaluate the participants' results. In general, the REIMEP-22 participants' results were satisfactory. This confirms the analytical capabilities of laboratories to determine accurately the age of uranium materials with low amount of ingrown thorium (young certified test sample). The Joint Research Centre of the European Commission (EC-JRC) organised REIMEP-22 in parallel to the preparation and certification of a uranium reference material certified for the production date (IRMM-1000a and IRMM-1000b).

  2. REIMEP-22 inter-laboratory comparison. ''U Age Dating - determination of the production date of a uranium certified test sample''

    Energy Technology Data Exchange (ETDEWEB)

    Venchiarutti, Celia; Richter, Stephan; Jakopic, Rozle; Aregbe, Yetunde [European Commission, Joint Research Centre (JRC), Geel (Belgium). Institute for Reference Materials and Measurements (IRMM); Varga, Zsolt; Mayer, Klaus [European Commission, Joint Research Centre (JRC), Karlsruhe (Germany). Institute for Transuranium Elements (ITU)

    2015-07-01

    The REIMEP-22 inter-laboratory comparison aimed at determining the production date of a uranium certified test sample (i.e. the last chemical separation date of the material). Participants in REIMEP-22 on ''U Age Dating - Determination of the production date of a uranium certified test sample'' received one low-enriched 20 mg uranium sample for mass spectrometry measurements and/or one 50 mg uranium sample for a-spectrometry measurements, with an undisclosed value for the production date. They were asked to report the isotope amount ratios n({sup 230}Th)/n({sup 234}U) for the 20 mg uranium sample and/or the activity ratios A({sup 230}Th)/A({sup 234}U) for the 50 mg uranium sample in addition to the calculated production date of the certified test samples with its uncertainty. Reporting of the {sup 231}Pa/{sup 235}U ratio and the respective calculated production date was optional. Eleven laboratories reported results in REIMEP-22. Two of them reported results for both the 20 mg and 50 mg uranium certified test samples. The measurement capability of the participants was assessed against the independent REIMEP-22 reference value by means of z- and zeta-scores in compliance with ISO 13528:2005. Furthermore a performance assessment criterion for acceptable uncertainty was applied to evaluate the participants' results. In general, the REIMEP-22 participants' results were satisfactory. This confirms the analytical capabilities of laboratories to determine accurately the age of uranium materials with low amount of ingrown thorium (young certified test sample). The Joint Research Centre of the European Commission (EC-JRC) organised REIMEP-22 in parallel to the preparation and certification of a uranium reference material certified for the production date (IRMM-1000a and IRMM-1000b).

  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)

    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. Biological reference materials for quality control of elemental composition analytical data

    International Nuclear Information System (INIS)

    Twelve biological-matrix, agricultural/food reference materials, Corn Stalk (Zea Mays) (NIST RM 8412), Corn Kernel (Zea Mays) (NIST RM 8413), Bovine Muscle Powder (NIST RM 8414), Whole Egg Powder (NIST RM 8415), Microcrystalline Cellulose (NIST RM 8416), Wheat Gluten (NIST RM 8418), Corn Starch (NIST RM 8432), Corn Bran (NIST RM 8433), Whole Milk Powder (NIST RM 8435), Durum Wheat Flour (NIST RM 8436), Hard Red Spring Wheat Flour (NIST RM 8437) and Soft Winter Wheat Flour (NIST RM 8438) were developed. They were characterized with respect to elemental composition via two extensive international interlaboratory characterization campaigns providing 303 reference and informational concentration values for 34 elements (Al, As, B, Ba, Br, Ca, Cd, Cl, Co, Cr, Cs, Cu, F, Fe, Hg, I, K, Mg, Mn, Mo, N, Na, Ni, P, Pb, Rb, S, Sb, Se, Sr, Ti, V, W, Zn) of nutritional, toxicological, and environmental significance. These products are available to the analytical community, for quality control of elemental composition analytical data, from the Standard Reference Materials Program, National Institute of Standards and Technology, Gaithersburg, MD, USA. (author)

  5. The impact of rumination on memory for self-referent material.

    Science.gov (United States)

    Moulds, Michelle L; Kandris, Eva; Williams, Alishia D

    2007-11-01

    Previous findings have linked rumination to the enhanced retrieval of negative memories (Lyubormirsky, Caldwell, & Nolen-Hoeksema, 1998) and overgeneral autobiographical memories (Watkins & Teasdale, 2004) in depression. However, little is known of the impact of rumination on the encoding of information, and in particular, self-referent information. This study examined the impact of rumination on self-referent encoding in high (BDI-II>or=13) and low (BDI-IIreferent. However, consistent with our hypothesis, high-dysphoric participants who ruminated recalled more negative self-referent words, after controlling for the proportion of words endorsed as self-descriptive. The findings demonstrate that rumination results in enhanced memory for negative, self-related material, and raises the possibility that this may serve as another pathway via which the negative evaluations of the self observed clinically in depression are maintained. PMID:18033619

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

    International Nuclear Information System (INIS)

    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

  7. Reference waste forms and packing material for the Nevada Nuclear Waste Storage Investigations Project

    International Nuclear Information System (INIS)

    The Lawrence Livermore National Laboratory (LLNL), Livermore, Calif., has been given the task of designing and verifying the performance of waste packages for the Nevada Nuclear Waste Storage Investigations (NNWSI) Project. NNWSI is studying the suitability of the tuffaceous rocks at Yucca Mountain, Nevada Test Site, for the potential construction of a high-level nuclear waste repository. This report gives a summary description of the three waste forms for which LLNL is designing waste packages: spent fuel, either as intact assemblies or as consolidated fuel pins, reprocessed commercial high-level waste in the form of borosilicate glass, and reprocessed defense high-level waste from the Defense Waste Processing Facility in Aiken, S.C. Reference packing material for use with the alternative waste package design for spent fuel is also described. 14 references, 8 figures, 20 tables

  8. 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)

  9. 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.

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

    International Nuclear Information System (INIS)

    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)

  11. Noble metals as permanent chemical modifiers for the determination of mercury in environmental reference materials using solid sampling graphite furnace atomic absorption spectrometry and calibration against aqueous standards

    Science.gov (United States)

    da Silva, Alessandra Furtado; Welz, Bernhard; Curtius, Adilson J.

    2002-12-01

    Iridium, palladium, rhodium and ruthenium, thermally deposited on the platform, were investigated as permanent modifiers for the determination of mercury in ash, sludge, marine and river sediment reference materials, ground to a particle size of 50 μm, using solid sampling graphite furnace atomic absorption spectrometry. A total mass of 250 μg of each modifier was applied using 25 injections of 20 μl of modifier solution (500 mg l -1), and executing a temperature program for modifier conditioning after each injection. The performance of palladium was found to be most consistent, taking the characteristic mass as the major criterion, resulting in an excellent correlation between the measured integrated absorbance values and the certified mercury contents. Mercury was found to be lost in part from aqueous solutions during the drying stage in the presence of all the investigated permanent modifiers, as well as in the presence of the palladium and magnesium nitrates modifier added in solution. A loss-free determination of mercury in aqueous solutions could be reached only after the addition of potassium permanganate, which finally made possible the use of aqueous standards for the direct analysis of solid samples. A characteristic mass of 55-60 pg Hg was obtained for the solid samples, using Pd as a permanent modifier, and also in aqueous solutions after the addition of permanganate. The results obtained for mercury in ash, sludge and sediment reference materials, using direct solid sapling and calibration against aqueous standards, as well as the detection limit of 0.2 mg kg -1 were satisfactory for a routine procedure.

  12. Noble metals as permanent chemical modifiers for the determination of mercury in environmental reference materials using solid sampling graphite furnace atomic absorption spectrometry and calibration against aqueous standards

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Alessandra Furtado da; Welz, Bernhard; Curtius, Adilson J

    2002-12-02

    Iridium, palladium, rhodium and ruthenium, thermally deposited on the platform, were investigated as permanent modifiers for the determination of mercury in ash, sludge, marine and river sediment reference materials, ground to a particle size of 50 {mu}m, using solid sampling graphite furnace atomic absorption spectrometry. A total mass of 250 {mu}g of each modifier was applied using 25 injections of 20 {mu}l of modifier solution (500 mg l{sup -1}), and executing a temperature program for modifier conditioning after each injection. The performance of palladium was found to be most consistent, taking the characteristic mass as the major criterion, resulting in an excellent correlation between the measured integrated absorbance values and the certified mercury contents. Mercury was found to be lost in part from aqueous solutions during the drying stage in the presence of all the investigated permanent modifiers, as well as in the presence of the palladium and magnesium nitrates modifier added in solution. A loss-free determination of mercury in aqueous solutions could be reached only after the addition of potassium permanganate, which finally made possible the use of aqueous standards for the direct analysis of solid samples. A characteristic mass of 55-60 pg Hg was obtained for the solid samples, using Pd as a permanent modifier, and also in aqueous solutions after the addition of permanganate. The results obtained for mercury in ash, sludge and sediment reference materials, using direct solid sapling and calibration against aqueous standards, as well as the detection limit of 0.2 mg kg{sup -1} were satisfactory for a routine procedure.

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

    International Nuclear Information System (INIS)

    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 ZrO2, 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 ZrO2 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 ZrO2: 97.7334 ± 0.0016%, HfO2: 1.7329 ± 0.0024%, SiO2: 30.1224 ± 0.0053%, Al2O3: 0.0245 ± 0.0015%, TiO2: 0.0153 ± 0.0006%, Fe2O3: 0.0068 ± 0.0005%, CdO: 3.1798 ± 0.00006 ppm, and the LOI results was = 0.0217 ± 0.00022%. (author)

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

    International Nuclear Information System (INIS)

    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)

  15. Total Digestion Efficient Results For Thorium Isotopes For Standard Reference Material (SRM)

    International Nuclear Information System (INIS)

    Radiochemical separation procedures are required to determine thorium isotopes in the environmental samples which has been used in the Radiochemistry and Environment Laboratory (RAS). Therefore, to testify the results is more efficient and reliable, the leaching and totally dissolve acid have been used in the radiochemical separation procedures for ten standard material reference (SRM) samples. From the finding shows different results of U-score, which is a totally dissolved method is more reliable and efficient compared to leaching method. Both of the digested samples are counting using alpha spectrometry counting system for 72 hours. (author)

  16. Analysis of candidate micro-reference materials of lichen and algae by SRXRF and PIXE

    International Nuclear Information System (INIS)

    The two micro-analysis techniques, synchrotron radiation X-ray fluorescence and macro-proton induced X-ray emission (macro-PIXE), were used in a homogeneity test of two candidate reference materials (RMs), lichen IAEA-338 and algae IAEA-413 (International Atomic Energy Agency, IAEA), in the present work. The two candidate RMs had good homogeneity with the minimum sampling mass of 10 mg required for micro-analytical nuclear techniques. The elemental content in the RMs was also determined by macro-PIXE. The relative homogeneity factors HE of elements in the RMs were estimated on the base of our macro-PIXE results

  17. Development of a standard reference material for Cr(vi) in contaminated soil

    Science.gov (United States)

    Nagourney, S.J.; Wilson, S.A.; Buckley, B.; Kingston, H.M.S.; Yang, S.-Y.; Long, S.E.

    2008-01-01

    Over the last several decades, considerable contamination by hexavalent chromium has resulted from the land disposal of Chromite Ore Processing Residue (COPR). COPR contains a number of hexavalent chromium-bearing compounds that were produced in high temperature industrial processes. Concern over the carcinogenic potential of this chromium species, and its environmental mobility, has resulted in efforts to remediate these waste sites. To provide support to analytical measurements of hexavalent chromium, a candidate National Institute of Standards and Technology (NIST) Standard Reference Material?? (SRM 2701), having a hexavalent chromium content of approximately 500 mg kg -1, has been developed using material collected from a waste site in Hudson County, New Jersey, USA. The collection, processing, preparation and preliminary physico-chemical characterization of the material are discussed. A two-phase multi-laboratory testing study was carried out to provide data on material homogeneity and to assess the stability of the material over the duration of the study. The study was designed to incorporate several United States Environmental Protection Agency (USEPA) determinative methods for hexavalent chromium, including Method 6800 which is based on speciated isotope dilution mass spectrometry (SIDMS), an approach which can account for chromium species inter-conversion during the extraction and measurement sequence. This journal is ?? The Royal Society of Chemistry 2008.

  18. A GUPIX-based approach to interpreting the PIXE-plus-XRF spectra from the Mars Exploration rovers: II geochemical reference materials

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, J.L., E-mail: icampbel@uoguelph.c [Guelph-Waterloo Physics Institute, University of Guelph, Guelph, Ontario, N1G 2W1 (Canada); McDonald, A.M. [Department of Earth Sciences, Laurentian University, Sudbury, Ontario, P3E 2E6 (Canada); Perrett, G.M. [Guelph-Waterloo Physics Institute, University of Guelph, Guelph, Ontario, N1G 2W1 (Canada); Taylor, S.M. [Department of Atmospheric and Oceanic Sciences, McGill University, Montreal, Quebec, H3A 2T5 (Canada)

    2011-01-01

    A detailed examination of the original calibration data for the laboratory version of the Mars Exploration Rover alpha particle X-ray spectrometer is undertaken to ascertain if the results from a suite of certified geochemical reference materials (GRMs) agree with the APXS calibration based upon homogeneous standards which was established in the previous paper. Various discrepancies, some of them large, are observed for specific elements in specific rock types, and it is argued on the basis of X-ray diffraction analyses of the GRMS that these are caused by the mineral phase structure of the rocks. Elements present in accessory mineral phases can be subject to very large errors, necessitating caution in interpretation of trace element results from the APXS. Some of the discrepancies can be dealt with by developing sub-calibrations, each of which is 'tuned' to a specific rock type. This approach has the potential to provide more accurate APXS analysis of unknown rocks than a calibration scheme based upon a simple averaging over many rock types within a GRM suite, or over a mix of rock and homogeneous standards. It also has the potential to measure the content of mineralogically bound water provided that a means of determining the distance from sample to detector is available.

  19. On the role of neutron activation analysis in the certification of a new reference material for trace-element studies, mixed human diet, H-9

    International Nuclear Information System (INIS)

    A new biological reference material, which is representative of diets consumed in Finland, was characterized by means of an intercomparison exercise conducted by the IAEA in the second half of 1985 and in 1986. Results for 35 elements received from 79 participants in 33 countries were evaluated. A certificate of analysis was issued with provisional certified values for 22 elements and information values for 2 elements. Neutron activation analysis (NAA) provided approximately one third of all the results reported. Instrumental NAA was used approximately 5 times as frequently as radiochemical NAA. Overall, NAA played an important role in providing useful data for the following 20 elements: Al, As, Br, Cl, Co, Cr, Cs, F, Fe, Hg, I, K, Mn, Mo, Na, Rb, Sb, Sc, Se and Zn. In comparison with the main competing non-nuclear method (usually atomic absorption spectrometry), NAA showed a larger dispersion of results for Cd, Cu, K and Mg, and a smaller degree of dispersion for Co, Cr, Hg and Se. (author) 17 refs.; 2 figs.; 3 tabs

  20. Uptake of oxygen in a coal standard reference materialR determined by fast (14-MeV) neutron activation analysis

    International Nuclear Information System (INIS)

    A fast (14-MeV) neutron activation analysis procedure was employed to directly measure mass fractions oxygen in coal samples. The procedure demonstrated sufficient precision and accuracy to determine a relative change of about 5% or more, in the oxygen mass fraction of about 12%. The procedure was applied to test samples of the newly developed SRM 1632c Trace Elements in Coal (Bituminous). The samples had been stored at three conditions: in liquid nitrogen vapor and at room temperature in the original containers packaged under argon, and for accelerated aging at 50 deg C open to air. Following six months storage increments, duplicate samples of each of twelve bottles of the SRM were measured for each storage condition. In addition each sample was processed through ten separate analytical runs yielding a total of some 720 measurements per storage duration. Oxygen was determined by comparison to a primary standard potassium dichromate and the accuracy of the method was assessed through the analysis of replicate samples of three reference materials that are certified for oxygen content. The initial 6-months test period indicated uptake of oxygen in the open-air storage. (author)

  1. Characterization of a high depth-resolution tantalum pentoxide sputter profiling reference material

    International Nuclear Information System (INIS)

    A major of surface analysis instruments concerns composition depth profiling. In many instances poor depth resolution is obtained, one cause of which is poor beam alignment and uniformity. To enable instrument users to optimise instrument settings and know (1) the instrument contribution to depth resolution and (2) the ion etch rate, tantalum pentoxide reference materials have been developed with thicknesses of 30 nm and 100 nm and interface widths, measured by AES, of 1.5 and 1.7 nm respectively. The effects of argon ion beam energy, electron beam current density, sputtering geometry and gas purity effects on etch rate and interface width are measured and interpreted in terms of basic parameters, showing that the material is a well-behaved model system that is robust and easily used. The precise shape of the interface and preferential sputtering effects are also analysed. (author)

  2. Soil contamination in plant samples and in botanical reference materials. Signature, quantification and consequences

    International Nuclear Information System (INIS)

    Individual samples of several sets of plants (lichens, tobacco, spruce needles, grass, botanical reference materials) show highly significant correlations of Al, Fe, Hf, La, Na, Th, Ti and V with Sc. These correlations result from the terrigenous part of aerosols deposited on and measured together with the plants. The composition of this contamination is almost uniform among the different plant sets and can be approximated by the composition of the upper continental crust. The mass of the terrigenous material ranges from 100 mg/g plant. Its presence is expected to lead to concentrations of the above and of other elements that deviate substantially from those of plants without contamination. This is proved by the comparison of two sets of spruce needles, one of which was measured without and the other after removal of the aerosol. (author)

  3. 1984 EC enquiry into the needs for nuclear reference materials (Z>89)

    International Nuclear Information System (INIS)

    For years now, experts in the nuclear field have expressed and pointed out the widespread need for Nuclear Reference Materials (NRMs) in the whole of the nuclear fuel cycle. NRMs were defined as actinides with well-characterized chemical, isotopic and/or physical properties for use as a common base for the calibration of instruments and checking of analytical methods. Since nuclear energy from fission reactors is an increasing contributor to the electricity generating capacity in the EC, there is an equivalent demand for accurate analytical measurements in the various stages of the fuel cycle and in associated fields such as: commercial transactions, production control, nuclear material accounting (safeguards), waste disposal, environmental and health physics, research and development. An essential element for improving analyses and measurements is the availability and use of the appropriate NRMs

  4. 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.

  5. Determination of perfluorinated compounds in human plasma and serum standard reference materials using independent analytical methods

    Energy Technology Data Exchange (ETDEWEB)

    Reiner, Jessica L. [National Institute of Standards and Technology, Analytical Chemistry Division, Gaithersburg, MD (United States); National Institute of Standards and Technology, Analytical Chemistry Division, Hollings Marine Laboratory, Charleston, SC (United States); Phinney, Karen W. [National Institute of Standards and Technology, Analytical Chemistry Division, Gaithersburg, MD (United States); Keller, Jennifer M. [National Institute of Standards and Technology, Analytical Chemistry Division, Hollings Marine Laboratory, Charleston, SC (United States)

    2011-11-15

    Perfluorinated compounds (PFCs) were measured in three National Institute of Standards and Technology (NIST) Standard Reference Materials (SRMs) (SRMs 1950 Metabolites in Human Plasma, SRM 1957 Organic Contaminants in Non-fortified Human Serum, and SRM 1958 Organic Contaminants in Fortified Human Serum) using two analytical approaches. The methods offer some independence, with two extraction types and two liquid chromatographic separation methods. The first extraction method investigated the acidification of the sample followed by solid-phase extraction (SPE) using a weak anion exchange cartridge. The second method used an acetonitrile extraction followed by SPE using a graphitized non-porous carbon cartridge. The extracts were separated using a reversed-phase C{sub 8} stationary phase and a pentafluorophenyl (PFP) stationary phase. Measured values from both methods for the two human serum SRMs, 1957 and 1958, agreed with reference values on the Certificates of Analysis. Perfluorooctane sulfonate (PFOS) values were obtained for the first time in human plasma SRM 1950 with good reproducibility among the methods (below 5% relative standard deviation). The nominal mass interference from taurodeoxycholic acid, which has caused over estimation of the amount of PFOS in biological samples, was separated from PFOS using the PFP stationary phase. Other PFCs were also detected in SRM 1950 and are reported. SRM 1950 can be used as a control material for human biomonitoring studies and as an aid to develop new measurement methods. (orig.)

  6. Experimental performance evaluation of a compton suppression system by an analysis of geological reference materials

    International Nuclear Information System (INIS)

    Compton scattering is one of major sources inducing a high background when a gamma ray spectrum is acquired from a radioactive sample. The high background spectrum deteriorates the detection sensitivity for an analysis of the nuclide of interest. To improve the detection sensitivity by the reduction of the spectrum background, a Compton suppression system (CSS) applying an anti coincidence mode was developed and has been used for a neutron activation analysis. A Compton suppression system (CSS) was implemented for an instrumental neutron activation analysis (INAA) at an NAA laboratory of the Korea Atomic Energy Research Institute (KAERI) in 2009. The CSS consists of a high purity Ge (HPGe) detector and bismuth germinate (BGO) with electronic modules. An evaluation of the performance of the CSS was carried out based on the measurement of the gamma ray emitting source and the detectable nuclides created thorough neutron activation of biological reference materials. This study was executed to evaluate the performance of the CSS for geological standard reference materials (SRMs). Four geological SRMs produced by the National Institute of Standards and Technology (NIST) in the USA were selected and irradiated using an NAA 1 irradiation hole at HANARO. Gamma ray spectra with normal mode and anti coincidence mode were acquired at the same time, and advantage factors of CSS for each nuclide detected were calculated on the basis of the signal to noise ratio

  7. Extensive sequencing of seven human genomes to characterize benchmark reference materials.

    Science.gov (United States)

    Zook, Justin M; Catoe, David; McDaniel, Jennifer; Vang, Lindsay; Spies, Noah; Sidow, Arend; Weng, Ziming; Liu, Yuling; Mason, Christopher E; Alexander, Noah; Henaff, Elizabeth; McIntyre, Alexa B R; Chandramohan, Dhruva; Chen, Feng; Jaeger, Erich; Moshrefi, Ali; Pham, Khoa; Stedman, William; Liang, Tiffany; Saghbini, Michael; Dzakula, Zeljko; Hastie, Alex; Cao, Han; Deikus, Gintaras; Schadt, Eric; Sebra, Robert; Bashir, Ali; Truty, Rebecca M; Chang, Christopher C; Gulbahce, Natali; Zhao, Keyan; Ghosh, Srinka; Hyland, Fiona; Fu, Yutao; Chaisson, Mark; Xiao, Chunlin; Trow, Jonathan; Sherry, Stephen T; Zaranek, Alexander W; Ball, Madeleine; Bobe, Jason; Estep, Preston; Church, George M; Marks, Patrick; Kyriazopoulou-Panagiotopoulou, Sofia; Zheng, Grace X Y; Schnall-Levin, Michael; Ordonez, Heather S; Mudivarti, Patrice A; Giorda, Kristina; Sheng, Ying; Rypdal, Karoline Bjarnesdatter; Salit, Marc

    2016-01-01

    The Genome in a Bottle Consortium, hosted by the National Institute of Standards and Technology (NIST) is creating reference materials and data for human genome sequencing, as well as methods for genome comparison and benchmarking. Here, we describe a large, diverse set of sequencing data for seven human genomes; five are current or candidate NIST Reference Materials. The pilot genome, NA12878, has been released as NIST RM 8398. We also describe data from two Personal Genome Project trios, one of Ashkenazim Jewish ancestry and one of Chinese ancestry. The data come from 12 technologies: BioNano Genomics, Complete Genomics paired-end and LFR, Ion Proton exome, Oxford Nanopore, Pacific Biosciences, SOLiD, 10X Genomics GemCode WGS, and Illumina exome and WGS paired-end, mate-pair, and synthetic long reads. Cell lines, DNA, and data from these individuals are publicly available. Therefore, we expect these data to be useful for revealing novel information about the human genome and improving sequencing technologies, SNP, indel, and structural variant calling, and de novo assembly. PMID:27271295

  8. Performance testing of irradiation facility rabbit system pneumatic reactor RSG-GAS using standard reference material

    International Nuclear Information System (INIS)

    The irradiation facility function test of rabbit system pneumatic (RS-5) has been done using standard reference material SRM 1633 Coal Fly ash through the sending station. Long irradiation of about 4-5 seconds. The results of qualitative analysis showed that the dominant elements listed in the certificate can be detected are Al, Ca, Mg, Si, Na, Ti, V, Mn. But only an element of Mn and Na which has a relative refractive values below 10%. And the other elements have a value relative refractive index 25% - 60%. The significant difference of value was not influenced by the position of irradiation in the reactor facility but due to the influence of the time difference between the sample and the standard count, and the half-life nuclide itself. Overall it can be said that the performance of the irradiation facility pneumatic rabbit system is good, but needs to be tested again by using different standard reference materials, in order to obtain the test results of analysis that can be trusted. (author)

  9. Soot Reference Materials for instrument calibration and intercomparisons: a workshop summary with recommendations

    Directory of Open Access Journals (Sweden)

    D. Baumgardner

    2012-03-01

    Full Text Available Soot, which is produced from biomass burning and the incomplete combustion of fossil and biomass fuels, has been linked to regional and global climate change and to negative health problems. Scientists measure soot using a variety of methods in order to quantify source emissions and understand its atmospheric chemistry, reactivity under emission conditions, interaction with solar radiation, influence on clouds, and health impacts. A major obstacle currently limiting progress is the absence of established standards or reference materials for calibrating the many instruments used to measure the various properties of soot.

    The current state of availability and practicability of soot standard reference materials (SRMs was reviewed by a group of 50 international experts during a workshop in June of 2011. The workshop was convened to summarize the current knowledge on soot measurement techniques, identify the measurement uncertainties and limitations related to the lack of SRMs, and identify attributes of SRMs that, if developed, would reduce measurement uncertainties. The workshop established that suitable SRMs are available for calibrating some, but not all, measurement methods. The community of single-particle sootphotometer (SP2 users identified a suitable SRM, fullerene soot, but users of instruments that measure light absorption by soot collected on filters did not. Similarly, those who use thermal optical analysis (TOA to analyze the organic and elemental carbon components of soot were not satisfied with current SRMs. The workshop produced recommendations for the development of new SRMs that would be suitable for the different soot measurement methods.

  10. Extensive sequencing of seven human genomes to characterize benchmark reference materials

    Science.gov (United States)

    Zook, Justin M.; Catoe, David; McDaniel, Jennifer; Vang, Lindsay; Spies, Noah; Sidow, Arend; Weng, Ziming; Liu, Yuling; Mason, Christopher E.; Alexander, Noah; Henaff, Elizabeth; McIntyre, Alexa B.R.; Chandramohan, Dhruva; Chen, Feng; Jaeger, Erich; Moshrefi, Ali; Pham, Khoa; Stedman, William; Liang, Tiffany; Saghbini, Michael; Dzakula, Zeljko; Hastie, Alex; Cao, Han; Deikus, Gintaras; Schadt, Eric; Sebra, Robert; Bashir, Ali; Truty, Rebecca M.; Chang, Christopher C.; Gulbahce, Natali; Zhao, Keyan; Ghosh, Srinka; Hyland, Fiona; Fu, Yutao; Chaisson, Mark; Xiao, Chunlin; Trow, Jonathan; Sherry, Stephen T.; Zaranek, Alexander W.; Ball, Madeleine; Bobe, Jason; Estep, Preston; Church, George M.; Marks, Patrick; Kyriazopoulou-Panagiotopoulou, Sofia; Zheng, Grace X.Y.; Schnall-Levin, Michael; Ordonez, Heather S.; Mudivarti, Patrice A.; Giorda, Kristina; Sheng, Ying; Rypdal, Karoline Bjarnesdatter; Salit, Marc

    2016-01-01

    The Genome in a Bottle Consortium, hosted by the National Institute of Standards and Technology (NIST) is creating reference materials and data for human genome sequencing, as well as methods for genome comparison and benchmarking. Here, we describe a large, diverse set of sequencing data for seven human genomes; five are current or candidate NIST Reference Materials. The pilot genome, NA12878, has been released as NIST RM 8398. We also describe data from two Personal Genome Project trios, one of Ashkenazim Jewish ancestry and one of Chinese ancestry. The data come from 12 technologies: BioNano Genomics, Complete Genomics paired-end and LFR, Ion Proton exome, Oxford Nanopore, Pacific Biosciences, SOLiD, 10X Genomics GemCode WGS, and Illumina exome and WGS paired-end, mate-pair, and synthetic long reads. Cell lines, DNA, and data from these individuals are publicly available. Therefore, we expect these data to be useful for revealing novel information about the human genome and improving sequencing technologies, SNP, indel, and structural variant calling, and de novo assembly.

  11. 7 CFR 1221.4 - Certified organization.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 10 2010-01-01 2010-01-01 false Certified organization. 1221.4 Section 1221.4 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (MARKETING... organization. Certified organization means any organization that has been certified by the Secretary...

  12. 7 CFR 1280.103 - Certified organization.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 10 2010-01-01 2010-01-01 false Certified organization. 1280.103 Section 1280.103 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (MARKETING... organization. Certified organization means any organization which has been certified by the Secretary...

  13. Preparation and evaluation of the homogeneity of milk as a candidate reference material for carbon-14

    International Nuclear Information System (INIS)

    A pilot project was initiated to study the feasibility of preparing milk as a candidate reference material for 14C near environmental levels. Two materials, MK-B at natural level of 14C and MK-C4 at an elevated level, have been prepared from pasteurized 2% dairy milk. MK-C4 was spiked with an appropriate amount of 14C-methylated casein tracer to achieve the elevated level. Several samples from MK-B and MK-C4 have been analyzed to test the homogeneity of these materials for the distribution of 14C. The samples were combusted in oxygen under 20 atmospheres pressure using a Parr bomb. The 14C concentrations were determined by liquid scintillation counting using Carbo-Sorb/Permafluor E+ cocktail. The results indicate that these materials are homogeneous with respect to 14C concentration even in sub-sample sizes of 0.25 g of the freeze-dried material. The precision of our 14C measurements, as expressed by the % relative standard deviation, is within 5%. The accuracy has been tested by analyzing replicate samples of the IAEA 14C quality assurance materials, C-3 (cellulose) and C-6 (ANU sucrose) and found to be within 3%. The lower limits of detection are 0.08, 0.05 and 0.02 Bq.g-1 of carbon for 20 ml of liquid scintillation mixture (Carbo-Sorb/Permafluor E+ = ∼0.67) loaded with up to 0.4g of carbon from the sample and counted for 3 cycles of 60, 180 and 1000 min each, respectively. Our measurements of 14C specific activities of MK-B and MK-C4 are 0.26 ± 0.01 and 15.3 ± 0.4 Bq.g-1 of carbon, respectively. (author)

  14. 24 CFR 1710.504 - Cooperation among certified states and between certified states and the Secretary.

    Science.gov (United States)

    2010-04-01

    ... 24 Housing and Urban Development 5 2010-04-01 2010-04-01 false Cooperation among certified states and between certified states and the Secretary. 1710.504 Section 1710.504 Housing and Urban....504 Cooperation among certified states and between certified states and the Secretary. (a) By...

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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)

  17. Ion exchange separation of lead from strontium in certified reference samples and spectrophotometric determination of lead as extractable ion-pair of eosin2- and the lead-cryptand (2.2.2)2+ complex

    International Nuclear Information System (INIS)

    A two-step procedure including anion exchange separation of lead from strontium in geological reference samples and a spectrophotometric determination of the separated lead as lead-cryptate (2.2.2) complex is presented. The exchangeable anion Cl- of the ion exchange resin (Dowex 1x4) is changed to Br- in 6M HBr solution. Lead is quantitatively retained in the column from 0.5M HBr medium, while Sr2+, Ba2+, Ca2+, Mg2+, Na+, K+, Fe3+, Cr3+, and Al3+ are passed through. Subsequently the retained Ph is eluted from the column with 6M HBr. The separation efficiency of the resin is controlled using mixed standard solution of (Pb, Sr, Ca, Mg, Ba, Na, K, Fe, Cr and Al), and radioactive tracer of 85Sr and 131Ba. The resin selectivity coefficient (K) of separating Pb from Sr is found to be KSrPb∼109. The Spectrophotometric method of lead determination is based on the formation of lead-crytate (2.2.2) complex at pH 8.3 using borate/HCl as a buffer solution. Then the ion-pair of eosin2+ and lead-cryptand (2.2.2) complex is extracted with chloroform, finally the absorbance of the extractable legend is measured at 550 nm. The extraction recovery, accuracy, precision, linearity and detection limit of the spectrophotometric method are 99.58%, 1.7%, 0.080μg mL-1, o-9μg mL-1, and 0.060μg mL-1, respectively. (author)

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

    International Nuclear Information System (INIS)

    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

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

    International Nuclear Information System (INIS)

    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. Using environmental reference materials for quality assurance in spanish radiochemical laboratories

    International Nuclear Information System (INIS)

    In order to achieve international acceptance of results, laboratories must be in a position to demonstrate that their results are reliable and traceable to SI units of measurement. Laboratories can provide objective evidence of their performance through participation in external quality assessment schemes sometimes referred to as proficiency tests (PT). To achieve this objective for environmental radioactivity laboratories in Spain, CSN, in collaboration with CIEMAT, has organised periodical intercomparison exercises to provide these laboratories with the means to assess the quality of their results. In order to implement the ISO/IUPAC/AOAC Harmonised Protocol for the Proficiency Testing of Analytical Laboratories, CIEMAT has been collaborating with the IAEA-AQCS during the last two exercises and has used IAEA reference materials as test samples. The first PT was organised using the IAEA-SED-1 which is a lake sediment containing K40, Ra226, Ac228, Cs137, Sr90, and Pu-(239+240), while the second PT used IAEA-Soil- 6 for the same set of radionuclides. This paper presents the results reported for the second test as well as a comparison of the participants' performance in both tests. The application of this Harmonised Protocol has provided an objective assessment of the performance of the laboratories, enabling them to evaluate and make appropriate modifications to their procedures

  1. The IAEA programme and perspectives for environmental radionuclide monitoring and preparation of reference materials

    International Nuclear Information System (INIS)

    For more than thirty years, the laboratories of the International Atomic Energy Agency have been involved in the monitoring of environmental radioactivity and in the world-wide provision of reference materials for radionuclides in environmental matrices. The occurrence of hot particles in selected sites and their morphological, structural, chemical and radiochemical characteristics have to be better investigated in order to identify possible correlations with the contaminating event and to assess the associated radiological risks. Research on radionuclides in the environment will also be extended to the measurement and compilation of data on the contaminants introduced by non-nuclear industrial activities and agrochemical treatments. In response to the world-wide trend towards increased reliability, comparability and traceability of chemical and radiochemical measurements, The IAEA will revise, develop and document a set of reference analytical procedures for naturally occurring radionuclides, which will supplement the current revision of procedures for anthropogenic radionuclides. The IAEA will enhance its support provided to the laboratories in the Member States for the implementation of a quality system and to achieve traceability of their radiometric measurements. Furthermore the IAEA will continue to provide training and maintain comparability and reliability of environmental radiochemical measurements by organizing proficiency tests and interlaboratory comparisons. These tests and exercises will also be used by the IAEA to monitor and evaluate the capability and preparedness of its ALMERA (Analytical Laboratories for Measuring Environmental Radioactivity) Network

  2. Determination of butoxyacetic acid (biomarker of ethylene glycol monobutyl ether exposure) in human urine candidate reference material

    Czech Academy of Sciences Publication Activity Database

    Sperlingova, I.; Dabrowská, L.; Stránský, V.; Duskova, S.; Kučera, Jan; Tvrdíková, M.; Tichý, M.

    2010-01-01

    Roč. 397, č. 2 (2010), s. 433-438. ISSN 1618-2642. [12th International Symposium on Biological and Environmental Reference Materials Keble Coll. Oxford, 07.07.2009-10.07.2009] Institutional research plan: CEZ:AV0Z10480505 Keywords : Candidate reference material * Ethylene glycol monobutyl ether * Metabolite Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 3.841, year: 2010

  3. 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)

    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

  4. Soot reference materials for instrument calibration and intercomparisons: a workshop summary with recommendations

    Directory of Open Access Journals (Sweden)

    D. Baumgardner

    2012-08-01

    Full Text Available Soot, which is produced from biomass burning and the incomplete combustion of fossil and biomass fuels, has been linked to regional and global climate change and to negative health problems. Scientists measure the properties of soot using a variety of methods in order to quantify source emissions and understand its atmospheric chemistry, reactivity under emission conditions, interaction with solar radiation, influence on clouds, and health impacts. A major obstacle currently limiting progress is the absence of established standards or reference materials for calibrating the many instruments used to measure the various properties of soot.

    The current state of availability and practicability of soot standard reference materials (SRMs was reviewed by a group of 50 international experts during a workshop in June of 2011. The workshop was convened to summarize the current knowledge on soot measurement techniques, identify the measurement uncertainties and limitations related to the lack of soot SRMs, and identify attributes of SRMs that, if developed, would reduce measurement uncertainties. The workshop established that suitable SRMs are available for calibrating some, but not all, measurement methods. The community of users of the single-particle soot-photometer (SP2, an instrument using laser-induced incandescence, identified a suitable SRM, fullerene soot, but users of instruments that measure light absorption by soot collected on filters did not. Similarly, those who use thermal optical analysis (TOA to analyze the organic and elemental carbon components of soot were not satisfied with current SRMs. The workshop, and subsequent, interactive discussions, produced a number of recommendations for the development of new SRMs, and their implementation, that would be suitable for the different soot measurement methods.

  5. 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. PMID:25929442

  6. Compatibility of OMRI certified surfactants with three entomopathogenic fungi

    Science.gov (United States)

    The Organic Materials Review Institute (OMRI) is a nonprofit organization providing an independent review of products intended for use in organic production systems to certify compliance with U.S. National organic standards. Since all adjuvants to be used in organic agriculture production are requir...

  7. Certifiable Java for Embedded Systems

    DEFF Research Database (Denmark)

    Schoeberl, Martin; Dalsgaard, Andreas Engelbredt; Hansen, Rene Rydhof;

    2014-01-01

    The Certifiable Java for Embedded Systems (CJ4ES) project aimed to develop a prototype development environment and platform for safety-critical software for embedded applications. There are three core constituents: A profile of the Java programming language that is tailored for safety......-critical applications, a predictable Java processor built with FPGA technology, and an Eclipse based application development environment that binds the profile and the platform together and provides analyses that help to provide evidence that can be used as part of a safety case. This paper summarizes key contributions...

  8. Twenty five years of reference material activity at Agriculture and Agri-Food Canada.

    Science.gov (United States)

    Ihnat, M

    2001-06-01

    In the mid 1970s, the available RMs, notably Bowen's Kale and Orchard Leaves and Bovine liver from National Bureau of Standards (NBS), although of great benefit, were overwhelmingly insufficiently representative, in respect of matrix and elemental composition, of the wide range of natural products submitted for analysis and in worldwide commerce. To provide additional coverage, an RM development project was initiated with input from cooperating analysts leading to an Agriculture and Agri-Food Canada/National Institute of Standards and Technology (NIST) cooperative venture and development of a total of 12 different agricultural/food RMs. With a total of 303 concentration values for 34 elements and a wide range of matrix components such as ash, silica, protein, fat, carbohydrate and fiber, these RMs significantly augment the world repertoire of biological control materials. A final material under consideration is a highly reliable, discrete, synthetic RM for quality control and calibration. This paper summarizes the research and developmental activities undertaken during the past quarter of a century related to RM development at Agriculture and Agri-Food Canada and includes a short historical background, conceptual considerations, preparation, physical characterization, homogeneity estimation, chemical characterization, calculation of recommended reference values and associated uncertainties, methodology development and application, and performance of inorganic analytical methods in a multielement, multilaboratory, collaborative characterization campaign. PMID:11451252

  9. Diffusion and adsorption in porous silica considered as a reference material for crystalline rock

    International Nuclear Information System (INIS)

    In the present study, well-characterized mesoporous silica was used as a reference material for crystalline rock. Saturation-leaching and through-diffusion tracer experiments were systematically carried out to determine the adsorption capacity factors and apparent and effective diffusivities for the radioactive tracers 3H, 22Na and 36Cl. The ionic strength of the supporting NaCl electrolyte, in equilibrium with atmospheric air, was either 0.002 M or 0.1 M. The apparent diffusivities derived from saturation-leaching experiments reveal that equilibrium adsorption on a negatively charged silica surface does not act to retard the mass transfer of sodium ions. The steady-state diffusion results are found to demonstrate the increasing breakthrough for sodium with decreasing ionic strength of the background electrolyte in comparison to 3H. These observations are consistent with the picture of chloride ion exclusion and of the diffuse double layer surface-excess for sodium ions being transported in the direction of the macroscopic concentration gradient. Furthermore, they are shown to be at odds with the widely adopted macroscopic pore diffusion model, which neglects the mobility of the counter-ion surface-excess. Copyright (2001) Material Research Society

  10. Development of a candidate reference material for adventitious virus detection in vaccine and biologicals manufacturing by deep sequencing

    OpenAIRE

    Edward T Mee; Preston, Mark D.; Minor, Philip D.; ,; Huang, Xuening; Nguyen, Jenny; Wall, David; Hargrove, Stacey; Fu, Thomas; Xu, George; Li, Li; Cote, Colette; Delwart, Eric; Li, Linlin; Hewlett, Indira

    2016-01-01

    Background Unbiased deep sequencing offers the potential for improved adventitious virus screening in vaccines and biotherapeutics. Successful implementation of such assays will require appropriate control materials to confirm assay performance and sensitivity. Methods A common reference material containing 25 target viruses was produced and 16 laboratories were invited to process it using their preferred adventitious virus detection assay. Results Fifteen laboratories returned results, obtai...

  11. NIST bullet signature measurement system for RM (Reference Material) 8240 standard bullets.

    Science.gov (United States)

    Ma, Li; Song, John; Whitenton, Eric; Zheng, Alan; Vorburger, Theodore; Zhou, Jack

    2004-07-01

    A bullet signature measurement system based on a stylus instrument was developed at the National Institute of Standards and Technology (NIST) for the signature measurements of NIST RM (Reference Material) 8240 standard bullets. The standard bullets are developed as a reference standard for bullet signature measurements and are aimed to support the recently established National Integrated Ballistics Information Network (NIBIN) by the Bureau of Alcohol, Tobacco and Firearms (ATF) and the Federal Bureau of Investigation (FBI). The RM bullets are designed as both a virtual and a physical bullet signature standard. The virtual standard is a set of six digitized bullet signatures originally profiled from six master bullets fired at ATF and FBI using six different guns. By using the virtual signature standard to control the tool path on a numerically controlled diamond turning machine at NIST, 40 RM bullets were produced. In this paper, a comparison parameter and an algorithm using auto-and cross-correlation functions are described for qualifying the bullet signature differences between the RM bullets and the virtual bullet signature standard. When two compared signatures are exactly the same (point by point), their cross-correlation function (CCF) value will be equal to 100%. The measurement system setup, measurement program, and initial measurement results are discussed. Initial measurement results for the 40 standard bullets, each measured at six land impressions, show that the CCF values for the 240 signature measurements are higher than 95%, with most of them even higher than 99%. These results demonstrate the high reproducibility for both the manufacturing process and the measurement system for the NIST RM 8240 standard bullets. PMID:15317178

  12. 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

  13. An evaluation of X-ray microanalytical techniques using reference materials

    International Nuclear Information System (INIS)

    Complete text of publication follows. Techniques for microanalysis using X-ray emission spectrometry are growing in importance as the technological development moves from the micro to the nano scale. It will be increasingly important to be able to make comparable measurements on this scale using a variety of X-ray excitation methods. A number of standards were investigated for suitability, but BCR 126A glass standard proved to be the best option. For the inter-comparison measurements the following X-ray microanalysis techniques were employed: Particle Induced Xray Emission (PIXE); Synchrotron X-ray Fluorescence Microanalysis (μ-SRXRF) and Wavelength Dispersive X-ray Spectrometry (WDS). Series of sequential analyses at the same spot on the glass were carried out to measure the precision of the four different x-ray spectrometry techniques. The relative standard deviations (RSD) of the elemental concentrations measured for elements with Z > 13 are plotted in Figure 1. The precision of the techniques is generally better than 5%, with mean values over the four techniques of 2.3% for Si, 2.5% for K, 5% for Ca, 2.3% for Zn, 5% Ba, and 2% for Pb. Fe, which is present in this glass in a very low concentration (0.004 % wt), is only detected and quantified with μ-SXRF at low energies (up to 10.0 keV), with an average precision of 11%. With a homogeneous sample, the deviation of the individual measurements from the certified values gives an estimation of the accuracy of the analytical technique. This has been investigated by analysing the glass at randomly selected spots with the different techniques and at different beam energies. Overall, the deviation from the certified values is well below 5% for elements such as Si (3.3%), K (3.5%), Zn (4.7%) Ba (4%) and Pb (3%). Other elements such as O, Na, Ca also present small deviations from the certified values (7%, 7% and 5% respectively). Conversely, Mg, Al and Fe deviate as expected. Further details on this work can be found in

  14. Provisional Assessment of Candidate High-Temperature Thermal Conductivity Reference Materials in the EMRP “Thermo” Project

    OpenAIRE

    Wu, J.; Morrell, R; T. Fry; Gnaniah, S.; Gohil, D.; Dawson, A.; Hameury, J.; Koenen, Alain; Hammerschmidt, U.; Turzó-András, E.; Strnad, R.; Blahut, A.

    2015-01-01

    This article describes the provisional assessment of a short list of four candidate high-temperature thermal conductivity reference materials in a European research project, “Thermo.” These four candidate materials are low-density calcium silicate, amorphous silica, high-density calcium silicate, and exfoliated vermiculite. Based on initial tests on material composition and microstructure changes, dimensional stability, mechanical stability, chemical stability and uniformity, the best two can...

  15. Certifying nonlocality from separable marginals

    Science.gov (United States)

    Vértesi, Tamás; Laskowski, Wiesław; Pál, Károly F.

    2014-01-01

    Imagine three parties, Alice, Bob, and Charlie, who share a state of three qubits such that all two-party reduced states A-B, A-C, and B-C are separable. Suppose that they have information only about these marginals but not about the global state. According to recent results, there exists an example for a set of three separable two-party reduced states that is only compatible with an entangled global state. In this paper, we show a stronger result by exhibiting separable two-party reduced states A-B, A-C, and B-C, such that any global state compatible with these marginals is nonlocal. Hence, we obtain that nonlocality of multipartite states can be certified from information only about separable marginals.

  16. Sparsity-certifying Graph Decompositions

    CERN Document Server

    Streinu, Ileana

    2007-01-01

    We describe a new algorithm, the $(k,\\ell)$-pebble game with colors, and use it obtain a characterization of the family of $(k,\\ell)$-sparse graphs and algorithmic solutions to a family of problems concerning tree decompositions of graphs. Special instances of sparse graphs appear in rigidity theory and have received increased attention in recent years. In particular, our colored pebbles generalize and strengthen the previous results of Lee and Streinu and give a new proof of the Tutte-Nash-Williams characterization of arboricity. We also present a new decomposition that certifies sparsity based on the $(k,\\ell)$-pebble game with colors. Our work also exposes connections between pebble game algorithms and previous sparse graph algorithms by Gabow, Gabow and Westermann and Hendrickson.

  17. Physical properties of oil-SPM aggregates : experiments with NIST standard reference material 1941b

    Energy Technology Data Exchange (ETDEWEB)

    Khelifa, A.; Brown, C.E. [Environment Canada, Ottawa, ON (Canada). Emergencies Science and Technology Division, Science and Technology Branch, Environmental Science and Technology Centre; Chun, M.; Eubank, J.L.E. [Waterloo Univ., ON (Canada). Nanotechnology Engineering

    2008-07-01

    Oil spilled in water disperses by a natural process in which suspended particulate matter (SPM) combines with oil droplets to form Oil-SPM aggregates (OSA). This paper presented a newly developed experimental procedure to measure the physical properties of OSAs, including size, settling velocity and effective density. A laboratory setup was created to examine the formation of OSAs in which the sediment Standard Reference Material 1941b was mixed with Arabian Medium and South Louisiana crude oils, and Corexit 9500 chemical dispersants at various concentrations. The study revealed that the hypothesis stating that OSAs are neutrally buoyant and do not settle to the seafloor is not valid. The OSAs appeared to behave as sediment flocs commonly observed in coastal waters. It was concluded that from an oil spill response perspective, the use of chemical dispersant in coaster waters rich in SPM could be problematic since it may enhance oil sedimentation and contaminate the seafloor. However, further research is needed to evaluate the effects of other key factors controlling the fate of OSAs that were not investigated in this study. These include the effect of mixing energy and the settling process of natural flocs. 29 refs., 1 tab., 10 figs.

  18. Results of 14C analysis on low-level reference materials

    International Nuclear Information System (INIS)

    An invitation from the University of Glasgow to participate in an international intercomparison of 14C analysis and the increased need for quality assurance for measurements performed at the Low-Level Laboratory by AECL's Environmental Technologies Branch (ETB), Chalk River Laboratories, prompted the initiation of this work. Standard 14C samples from the IAEA and from the ETB were analyzed and compared to their reference values. All analyses agreed well with reported values and confirmed that the ETB can reliably measure 14C between 50 and 500 Bq/kg C. Samples from the University of Glasgow, Scotland, were also analyzed and reported. The results of counting various CO2 blank materials (dry ice from a CO2-siphon and limestone) showed that the source of CO2 does not have an effect on background count rate or counter efficiency. The ETB's lower limit of detection (LLD) has been calculated to be 10 -20 Bq/kg C and the determination limit (LQ) for samples during the ETB's routine operations has been documented to be 44 Bq/kg C. (author)

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

    International Nuclear Information System (INIS)

    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 110mAg, 82Br, 60Co, 134Cs, 152Eu, 59Fe, 140La, 233Pa (for Th determination), 46Sc and 75Se 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)

  20. Determination of trace quantities of iodine in different sorts of tobacco and biological standard reference materials by rapid radiochemical separation

    International Nuclear Information System (INIS)

    The concentration levels of total iodine obtained by RNAA in different sorts of tobacco, including the reference sample Kentucky Tobacco 2RI, two new candidate reference materials, Oriental Tobacco Leaves (CTA-OTL-1) and Virginia Tobacco Leaves (CTA-VTL-2) prepared in the Institute of Nuclear Chemistry and Technology, Warsaw, and some biological SRMs, are presented and discussed. (author) 51 refs.; 1 fig.; 2 tabs