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

International Nuclear Information System (INIS)

Ishizu, H.; Yamada, T.

2013-01-01

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

Homogeneity and evaluation of the new NIST leaf certified reference materials

International Nuclear Information System (INIS)

Becker, D.A.

1990-01-01

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

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.

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

International Nuclear Information System (INIS)

2009-01-01

, 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 129 I on a Mediterranean sea water sample. The material was designed for the analysis of low level 129 I in sea water. The sample, after successful certification, has been issued as a certified reference material for 129 I 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

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-07-01

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

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

International Nuclear Information System (INIS)

Tamura, Shuzo; Hashitani, Hiroshi

1982-06-01

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

COMAR - database for certified reference materials

International Nuclear Information System (INIS)

Klich, H.; Caliste, J.P.

1988-01-01

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

Development of certified reference material of mineral composition of natural water designed to control of turbidity measurement accuracy

Directory of Open Access Journals (Sweden)

Liudmila I. Gorjaeva

2017-01-01

Full Text Available Introduction. The results of development of a certified reference material (CRM of mineral composition of natural water are presented. A solution prepared from the material of the CRM specimen imitates mineral composition of natural surface water. The certified values are mass fractions of nitrate ions, chloride ions, fluoride ions, and total iron and turbidity according to formazine scale. Materials and methods. The certified values of mass concentrations of the components were determined using calculated experimental evaluation procedure;the certified turbidity value was determinedusing the certified turbidimetric method. Results. The relative expanded uncertainty (k = 2 of the certified turbidity values does not exceed 5 %, the same value for mass concentrationsis not more than 3.5 %. Relative standard uncertainty from heterogeneity does not exceed 1.0 %. The shelf life of the developed CRM is set to 3 years. Discussion and conclusion. Developed CRM was registered in the State Register of CRM's as GSO 10815-2016. The CRM is designed to control the accuracy of results of the certified characteristics measurements, including proficiency testing of laboratories using interlaboratory comparative tests. The CRM can be used for validation of measurement procedures.

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

Directory of Open Access Journals (Sweden)

Tatiana Forti

2016-06-01

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-06-15

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

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

Science.gov (United States)

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

2016-01-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2015-01-01

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

Application of the 226Ra-230Th-234U and 227Ac-231Pa-235U radiochronometers to uranium certified reference materials

International Nuclear Information System (INIS)

Rolison, J.M.; Treinen, K.C.; McHugh, K.C.; Gaffney, A.M.; Williams, R.W.

2017-01-01

Uranium certified reference materials (CRM) issued by New Brunswick Laboratory were subjected to dating using four independent uranium-series radiochronometers. In all cases, there was acceptable agreement between the model ages calculated using the 231 Pa- 235 U, 230 Th- 234 U, 227 Ac- 235 U or 226 Ra- 234 U radiochronometers and either the certified 230 Th- 234 U model date (CRM 125-A and CRM U630), or the known purification date (CRM U050 and CRM U100). The agreement between the four independent radiochronometers establishes these uranium certified reference materials as ideal informal standards for validating dating techniques utilized in nuclear forensic investigations in the absence of standards with certified model ages for multiple radiochronometers. (author)

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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...

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

Science.gov (United States)

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

2017-01-01

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

Certified reference materials - beech leaves and spruce needles - for the quality control in monitoring damage in forests by acid deposition

Energy Technology Data Exchange (ETDEWEB)

Maier, E A; Griepink, B [Commission of the European Communities, Brussels (Belgium). Community Bureau of Reference; Muntau, H [Commission of the European Communities, Ispra (Italy). Joint Research Centre

1989-12-01

The chemical determination of various elements in leaves or needles allows to establish the damage caused by acid deposition. To control the quality of such determinations the Community Bureau of Reference (BCR) produced two Certified Reference Materials: Beech leaves (CRM No. 100) and Spruce needles (CRM No. 101). After a careful preparation procedure, a homogeneity study and a long term stability study, the materials were certified for: Cl, N, P and S in CRM No. 100, Al, Ca, Cl, Mg, Mn, N, P, S and Zn in CRM No. 101. Indicative values on the content of 19 majors and trace elements are also reported. (orig.).

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

Czech Academy of Sciences Publication Activity Database

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

2015-01-01

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

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

International Nuclear Information System (INIS)

2013-01-01

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

A new marine sediment certified reference material (CRM) for the determination of persistent organic contaminants: IAEA-459.

Science.gov (United States)

Tolosa, Imma; Cassi, Roberto; Huertas, David

2018-04-11

A new marine sediment certified reference material (IAEA 459) with very low concentrations (μg kg -1 ) for a variety of persistent organic contaminants (POPs) listed by the Stockholm Convention, as well as other POPs and priority substances (PSs) listed in many environmental monitoring programs was developed by the IAEA. The sediment material was collected from the Ham River estuary in South Korea, and the assigned final values were derived from robust statistics on the results provided by selected laboratories which demonstrated technical and quality competence, following the guidance given in ISO Guide 35. The robust mean of the laboratory means was assigned as certified values, for those compounds where the assigned value was derived from at least five datasets and its relative expanded uncertainty was less than 40% of the assigned value (most of the values ranging from 8 to 20%). All the datasets were derived from at least two different analytical techniques which have allowed the assignment of certified concentrations for 22 polychlorinated biphenyl (PCB) congeners, 6 organochlorinated (OC) pesticides, 5 polybrominated diphenyl ethers (PBDEs), and 18 polycyclic aromatic hydrocarbon (PAHs). Mass fractions of compounds that did not fulfill the criteria of certification are considered information values, which include 29 PAHs, 11 PCBs, 16 OC pesticides, and 5 PBDEs. The extensive characterization and associated uncertainties at concentration levels close to the marine sediment quality guidelines will make CRM 459 a valuable matrix reference material for use in marine environmental monitoring programs.

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.

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

Science.gov (United States)

Yang, Dezhi; Wang, Fengfeng; Zhang, Li; Gong, Ningbo; Lv, Yang

2015-05-01

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.

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

Directory of Open Access Journals (Sweden)

Egor P Sobina

2017-01-01

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

A new certified reference material for benzene measurement in air on a sorbent tube: development and proficiency testing

Energy Technology Data Exchange (ETDEWEB)

Caurant, A. [Laboratoire National de Metrologie et d' Essais, Paris (France); Universite Paris 12 et CNRS (UMR 7583), Faculte des Sciences et Technologie, Laboratoire Inter-universitaire des Systemes Atmospheriques, Unite Mixte de Recherche Universite Paris 7 (France); Lalere, B.; Schbath, M.C.; Stumpf, C.; Sutour, C.; Mace, T.; Vaslin-Reimann, S. [Laboratoire National de Metrologie et d' Essais, Paris (France); Quisefit, J.P.; Doussin, J.F. [Universite Paris 12 et CNRS (UMR 7583), Faculte des Sciences et Technologie, Laboratoire Inter-universitaire des Systemes Atmospheriques, Unite Mixte de Recherche Universite Paris 7 (France)

2010-11-15

A certified matrix reference material (CRM) for the measurement of benzene in ambient air has been developed at Laboratoire National de Metrologie et d'Essais. The production of these CRMs was conducted using a gravimetric method fully traceable to the International System of Units. The CRMs were prepared by sampling an accurate mass of a gaseous primary reference material of benzene, using a high-precision laminar flowmeter and a mass flow controller, with a PerkinElmer sampler filled with Carbopack trademark X sorbent. The relative standard deviations obtained for the preparation of a batch of 20 tubes loaded with 500 ng of benzene were below 0.2%. Each CRM is considered independent from the others and with its own certified value and an expanded uncertainty estimated to be within 0.5%, lower than the uncertainties of benzene CRMs already available worldwide. The stability of these materials was also established up to 12 months. These CRMs were implemented during proficiency testing, to evaluate the analytical performances of seven French laboratories involved in benzene air monitoring. (orig.)

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)

Venchiarutti, C.; Richter, S.; Jakopic, R.; Aregbe, Y.; Varga, Z.; Nicholl, A.; Krajko, J.; Mayer, K.

2016-01-01

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 230 Th/ 234 U 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)

Elemental Quantification and Residues Characterization of Wet Digested Certified and Commercial Carbon Materials

KAUST Repository

Simoes, Filipa R. F.; Batra, Nitin M.; Warsama, Bashir H.; Canlas, Christian; Patole, Shashikant; Yapici, Tahir F.; Costa, Pedro M. F. J.

2016-01-01

.g., graphene and nanotubes) has suffered from the lack of efficient digestion steps and certified reference materials (CRM). Here, various commercial and certified graphitic carbon materials were subjected to a

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

Directory of Open Access Journals (Sweden)

E. P. Sobina

2016-01-01

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

Feasibility studies to establish at the Kazakhstan Ulba metallurgical plant the manufacturing capability to produce low-enriched uranium certified reference materials

Energy Technology Data Exchange (ETDEWEB)

Kuzminski, Jozef [Los Alamos National Laboratory; Nesuhoff, J [NBL; Cratto, P [NBL; Pfennigwerth, G [Y12 NATIONAL SEC. COMPLEX; Mikhailenko, A [ULBA METALLURGICAL PLANT; Maliutina, I [ULBA METALLURGICAL PLANT; Nations, J [GREGG PROTECTION SERVICES

2009-01-01

One of the salient features of the transition plan that the United States Department of Energy/National Nuclear Security Administration (DOE/NNSA) is presently implementing in the Former Soviet Union countries is the availability of uranium certified reference materials for calibration of nondestructive assay (NDA) measurement equipment. To address this challenge, DOE/NNSA and U.S. national laboratories have focused their cooperative efforts on establishing a reliable source for manufacturing, certifying, and supplying of such standards. The Ulba Metallurgical Plant (UMP), Kazakhstan, which processes large quantities of low-enriched uranium to produce ceramic fuel pellets for nuclear-powered reactors, is well situated to become a key supplier of low-enriched uranium certified reference materials for the country and Central Asia region. We have recently completed Phase I of a feasibility study to establish at UMP capabilities of manufacturing these standards. In this paper we will discuss details of a proposed methodology for uranium down-blending, material selection and characterization, and a proposed methodology of measurement by destructive (DA) and non-destructive (NDA) analysis to form a database for material certification by the competent State authorities in the Republic of Kazakhstan. In addition, we will discuss the prospect for manufacturing of such standards at UMP.

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

DEFF Research Database (Denmark)

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

2016-01-01

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

Mineral oil content in sediments and soils: comparability, traceability and a certified reference material for quality assurance

Energy Technology Data Exchange (ETDEWEB)

Becker, Roland; Buge, Hans-Gerhard; Bremser, Wolfram; Nehls, Irene [Federal Institute for Materials Research and Testing (BAM), Berlin (Germany)

2006-06-15

The performance of twelve laboratories with previously established proficiency in the determination of the mineral oil content in a fresh water sediment is described. The summation parameter total petrol hydrocarbon (TPH) is defined according to ISO 16703:2004 with regard to the sample preparation to be applied, the flame ionisation detection (FID) and the boiling range of C{sub 10}-C{sub 40} to be integrated. Comprehensive tests of homogeneity and stability have been carried out on the candidate material using appropriate models. The outcome of the study served as the basis for the certification of the candidate reference material as ERM-CC015a. The certified mass fraction is 1,820{+-}130mgkg{sup -1}and traceability was established by using an appropriate calibration standard certified for the mass fraction of C{sub 10}-C{sub 40}. The interlaboratory scatter of measurement results in this exercise can largely be explained by the variability of the individual calibrations based on this common calibration standard. (orig.)

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

International Nuclear Information System (INIS)

Kucera, J.; Horakova, J.; Soukal, L.

1997-01-01

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)

Discrepancy of sodium mass fraction determined by INAA in the NIST SRM1547 and SRM1515 reference materials and their certified values

International Nuclear Information System (INIS)

Kamenik, Jan; Kucera, Jan

2015-01-01

Determination of sodium content in NIST standard reference materials (SRM) SRM 1547 and SRM 1515 in recent years yielded values higher than NIST certified values. Similarly, increased values were published for SRM 1547 by several laboratories, however, published sodium values SRM 1515 are in general in agreement with the certified value. Additional analysis of SRM 1547 and SRM 1515 using NIST SRM 3152a Sodium Standard Solution as a calibrator confirmed increased Na values. Inhomogeneity indicating external contamination of the stock material was not found. Moreover, increased Na value was also determined for freshly opened bottle of SRM 1547 material. Analysis of the historical material A-2 from our archive, which is identical with SRM 1515 and was distributed by NIST prior to the SRM 1515 certification and stored in a polyethylene vial, yielded a value in agreement with the certified value. A hypothesis was formulated that sodium in SRM 1547 and SRM 1515 materials could have been increasing after certification, perhaps due to the release of sodium from the glass bottle. (author)

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

International Nuclear Information System (INIS)

Takashima, Kyoichiro

1991-03-01

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)

Development of a certified reference material for composition of high-purity copper as a transfer standard within GET 176-2013

Directory of Open Access Journals (Sweden)

Veniamin M. Zyskin

2017-01-01

Full Text Available Introduction. The paper gives information on the development of a certified reference material (CRM for composition of high-purity copper (Cu CRM UNIIM. The CRM is included as the transfer standard into the State primary standard of the mass (molar fraction and mass (molar concentration of the component in liquid and solid substances and materials based on coulometry GET 176-2013.Materials and methods. The CRM represents pieces of oxygen-free copper wire rod, brand KMB, produced according to GOST R 53803-2010, weighing from 0.5 to 1g. The CRM is packed in plastic vials with the capacity of 30 or 50 cm3. The certified characteristic of the CRM is copper mass fraction in copper wire rod, expressed in percentages. The certified value for copper mass fraction was established by the primary method of controlled-potential coulometry using the State primary standard GET 176-2013.Results. The permitted interval of the certified value for copper mass fraction in the CRM is from 99,950 % to 100,000 %. The relative expanded uncertainty (k=2 of the certified value for copper mass fraction does not exceed 0,030 %; the relative standard uncertainty due to inhomogeneity does not exceed 0.010 %; the relative standard uncertainty due to instability does not exceed 0.010 %. The shelf life of the developed CRM is 10 years provided that standard storage conditions are ensured.Discussion and conclusions. The developed CRM is included into the State register of type approved RMs under the number GSO 10800-2016. The CRM of high-purity copper (Cu CRM UNIIM as a transfer standard is intended for reproduction, storage and transfer of the copper mass fraction unit to other reference materials and chemical reagents by the method of comparison using a comparator and by conducting direct measurements. This CRM may also be used:– for verification of measuring instruments (MIs according to the state verification schedule described in GOST R 8.735.0-2014,– for calibration

Reference materials and representative test materials: the nanotechnology case

International Nuclear Information System (INIS)

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

2013-01-01

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

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

Science.gov (United States)

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

2011-03-01

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

Elemental Quantification and Residues Characterization of Wet Digested Certified and Commercial Carbon Materials

KAUST Repository

Simoes, Filipa R. F.

2016-10-25

Inductively coupled plasma optical emission spectroscopy (ICP-OES) is a common, relatively low cost, and straightforward analytical technique for the study of trace quantities of metals in solid materials, but its applicability to nanocarbons (e.g., graphene and nanotubes) has suffered from the lack of efficient digestion steps and certified reference materials (CRM). Here, various commercial and certified graphitic carbon materials were subjected to a

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.

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

International Nuclear Information System (INIS)

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

1993-01-01

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

Certified reference materials for organic contaminants for use in monitoring of the aquatic environment

NARCIS (Netherlands)

Boer, de J.; McGovern, E.

2001-01-01

Over the last three decades organic contaminants have been of increasing importance in environmental monitoring. Dioxins, furans, polychlorinated biphenyls and organochlorine pesticides have determined the environmental research agenda. This has led to an increasing demand for certified reference

Preparation and characterization of the fish reference material

International Nuclear Information System (INIS)

Ulrich, Joao Cristiano

2011-01-01

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

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.

1990-01-01

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

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

International Nuclear Information System (INIS)

Pauwels, J.

1988-01-01

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

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

International Nuclear Information System (INIS)

Pauwels, J.; Ingelbrecht, C.

1990-01-01

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

The importance of reference materials in doping-control analysis.

Science.gov (United States)

Mackay, Lindsey G; Kazlauskas, Rymantas

2011-08-01

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

The application of HPLC-F and GC-MS to the analysis of selected hydroxy polycylic hydrocarbons in two certified fish bile reference materials

NARCIS (Netherlands)

Jonsson, G.; Beyer, J.; Wells, D.; Ariese, F.

2003-01-01

Four selected hydroxy polycyclic aromatic hydrocarbons (OH-PAHs), 2-hydroxy-naphthalene (2-OH-NPH), 1-hydroxy-phenanthrene (1-OH-PHE), 1-hydroxy-pyrene (1-OH-PYR) and 3-hydroxy-benzo[a]pyrene (3-OH-BaP) have been analysed in two certified fish bile reference materials (CRMs) for exposure monitoring

The application of HPLC-F and GC-MS to the analysis of selected hydroxy polycyclic hydrocarbons in two certified fish bile reference materials

NARCIS (Netherlands)

Jonsson, G.; Beyer, J.; Wells, D.E.; Ariese, F.

2003-01-01

Four selected hydroxy polycyclic aromatic hydrocarbons (OH-PAHs), 2-hydroxy-naphthalene (2-OH-NPH), 1-hydroxy-phenanthrene (1-OH-PHE), 1-hydroxy-pyrene (1-OH-PYR) and 3-hydroxy-benzo[a]pyrene (3-OH-BaP) have been analysed in two certified fish bile reference materials (CRMs) for exposure monitoring

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)

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

2007-01-01

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)

The Kjeldahl method as a primary reference procedure for total protein in certified reference materials used in clinical chemistry. I. A review of Kjeldahl methods adopted by laboratory medicine.

Science.gov (United States)

Chromý, Vratislav; Vinklárková, Bára; Šprongl, Luděk; Bittová, Miroslava

2015-01-01

We found previously that albumin-calibrated total protein in certified reference materials causes unacceptable positive bias in analysis of human sera. The simplest way to cure this defect is the use of human-based serum/plasma standards calibrated by the Kjeldahl method. Such standards, commutative with serum samples, will compensate for bias caused by lipids and bilirubin in most human sera. To find a suitable primary reference procedure for total protein in reference materials, we reviewed Kjeldahl methods adopted by laboratory medicine. We found two methods recommended for total protein in human samples: an indirect analysis based on total Kjeldahl nitrogen corrected for its nonprotein nitrogen and a direct analysis made on isolated protein precipitates. The methods found will be assessed in a subsequent article.

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

, bivalves, and marine mammals as well as a range of marine certified reference materials, and the results were compared to values published in the literature. For fish and marine mammals, the results were in most cases below the limit of detection. For other sample types, inorganic arsenic concentrations up...

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

International Nuclear Information System (INIS)

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

2013-01-01

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

New reference materials improvement of methods of measurements

International Nuclear Information System (INIS)

Marchandise, H.

1985-01-01

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

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

Science.gov (United States)

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

2012-07-01

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

A 244Pu spike reference material CBNM IRM-042A

International Nuclear Information System (INIS)

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

1991-01-01

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

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...

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

International Nuclear Information System (INIS)

1986-12-01

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

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-12-15

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

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

International Nuclear Information System (INIS)

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

1993-01-01

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

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

International Nuclear Information System (INIS)

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

1986-01-01

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

Biological and environmental reference materials in neutron activation analysis work

International Nuclear Information System (INIS)

Guinn, V.P.; Gavrilas, M.

1990-01-01

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

Biological reference materials and analysis of toxic elements

Energy Technology Data Exchange (ETDEWEB)

Subramanian, R; Sukumar, A

1988-12-01

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

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

Science.gov (United States)

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

2015-04-01

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

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)

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.)

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

International Nuclear Information System (INIS)

Ohata, Masaki; Kidokoro, Toshihiro; Kurahashi, Masayasu; Hioki, Akiharu

2010-01-01

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)

DH-1a: a certified uranium-thorium reference ore

International Nuclear Information System (INIS)

Steger, H.F.; Bowman, W.S.; Zechanowitsch, G.

1981-09-01

A 122-kg sample of uranium-thorium ore, DH-1a, from Elliot Lake, Ontario, was prepared as a compositional reference material to replace the similar certified ore, DH-1. DH-1a was ground to minus 74μm, blended in one lot, and bottled in 200 g units. The homogeneity of DH-1a with respect to uranium was confirmed using the volumetric umpire method. The recommended value for uranium is based on the data from the confirmation of homogeneity. For thorium, twelve laboratories provided results in a free choice analytical program. A statistical analysis of the data gave a recommended value of 0.263 percent for uranium and 0.091 percent for thorium

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-07-15

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

Development of a certified reference material (NMIJ CRM 7512-a) for the determination of trace elements in milk powder.

Science.gov (United States)

Zhu, Yanbei; Narukawa, Tomohiro; Miyashita, Shin-ichi; Kuroiwa, Takayoshi; Inagaki, Kazumi; Chiba, Koichi; Hioki, Akiharu

2013-01-01

A certified reference material (CRM), NMIJ CRM 7512-a, was developed for the determination of trace elements in milk powder. At least three independent analytical methods were applied to characterize the certified value of each element; all of these analytical methods were based on microwave acid digestions and carried out using different analytical instruments. The certified value was given on a dry-mass basis, where the dry-mass correction factor was obtained by drying the sample at 65°C for 15 to 25 h. The certified values in the units of mass fractions for 13 elements were as follows: Ca, 8.65 (0.38) g kg(-1); Fe, 0.104 (0.007) g kg(-1); K, 8.41 (0.33) g kg(-1); Mg, 0.819 (0.024) g kg(-1); Na, 1.87 (0.09) g kg(-1); P, 5.62 (0.23) g kg(-1); Ba, 0.449 (0.013) mg kg(-1); Cu, 4.66 (0.23) mg kg(-1); Mn, 0.931 (0.032) mg kg(-1); Mo, 0.223 (0.012) mg kg(-1); Rb, 8.93 (0.31) mg kg(-1); Sr, 5.88 (0.20) mg kg(-1); and Zn, 41.3 (1.4) mg kg(-1), where the numbers in the parentheses are the expanded uncertainties with a coverage factor of 2. The expanded uncertainties were estimated considering the contribution of the analytical methods, the method-to-method variance, the sample homogeneity, the dry-mass correction factor, and the concentrations of the standard solutions for calibration. The concentrations of As (2.1 μg kg(-1)), Cd (0.2 μg kg(-1)), Cr (1.3 μg kg(-1)), Pb (0.3 μg kg(-1)), and Y (64 μg kg(-1)) were given as information values for the present CRM.

Single-particle characterization of 'Asian Dust' certified reference materials using low-Z particle electron probe X-ray microanalysis

International Nuclear Information System (INIS)

Hwang, Hee Jin; Ro, Chul-Un

2006-01-01

In order to clearly elucidate whether Asian Dust particles experience chemical modification during long-range transport, it is necessary to characterize soil particles where Asian Dust particles originate. If chemical compositions of source soil particles are well characterized, then chemical compositions of Asian Dust particles collected outside source regions can be compared with those of source soil particles in order to find out the occurrence of chemical modification. Asian Dust particles are chemically and morphologically heterogeneous, and thus the average composition and the average aerodynamic diameter (obtainable by bulk analysis) are not much relevant if the chemical modifications of the particles must be followed. The major elemental composition and abundance of the particle types that are potential subjects of chemical modification can only be obtained using single-particle analysis. A single particle analytical technique, named low-Z particle electron probe X-ray microanalysis (low-Z particle EPMA), was applied to characterize two certified reference materials (CRMs) for Asian Dust particles, which were collected from a loess plateau area and a desert of China. The CRMs were defined by bulk analyses to provide certified concentrations for 13 chemical elements. Using the low-Z particle EPMA technique, the concentrations of major chemical species such as aluminosilicates, SiO 2 , CaCO 3 , and carbonaceous species were obtained. Elemental concentrations obtained by the low-Z particle EPMA are close to the certified values, with considering that the single particle and bulk analyses employ very different approaches. There are still some discrepancies between those concentration values, resulting from analyses of particles with different sizes, different sample amounts analyzed, and uncertainties involved in the single particle analysis

Phosphated minerals to be used as radioactive reference materials

International Nuclear Information System (INIS)

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

2003-01-01

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

High Precision Zinc Stable Isotope Measurement of Certified Biological Reference Materials Using the Double Spike Technique and Multiple Collector-ICP-MS.

Science.gov (United States)

Moore, Rebekah E T; Larner, Fiona; Coles, Barry J; Rehkämper, Mark

2017-04-01

Biological reference materials with well-characterised stable isotope compositions are lacking in the field of 'isotope biochemistry', which seeks to understand bodily processes that rely on essential metals by determining metal stable isotope ratios. Here, we present Zn stable isotope data for six biological reference materials with certified trace metal concentrations: fish muscle, bovine muscle, pig kidney, human hair, human blood serum and human urine. Replicate analyses of multiple aliquots of each material achieved reproducibilities (2sd) of 0.04-0.13‰ for δ 66/64 Zn (which denotes the deviation of the 66 Zn/ 64 Zn ratio of a sample from a pure Zn reference material in parts per 1000). This implies only very minor isotopic heterogeneities within the samples, rendering them suitable as quality control materials for Zn isotope analyses. This endorsement is reinforced by (i) the close agreement of our Zn isotope data for two of the samples (bovine muscle and human blood serum) to previously published results for different batches of the same material and (ii) the similarity of the isotopic data for the samples (δ 66/64 Zn ≈ -0.8 to 0.0‰) to previously published Zn isotope results for similar biological materials. Further tests revealed that the applied Zn separation procedure is sufficiently effective to enable accurate data acquisition even at low mass resolving power (M/ΔM ≈ 400), as measurements and analyses conducted at much higher mass resolution (M/ΔM ≈ 8500) delivered essentially identical results.

Determination of rare earth and uranium in reference biological materials certified by the method of neutron activation analysis

International Nuclear Information System (INIS)

Pereira, Lais H.P.; Saiki, Mitiko

2013-01-01

The objective of this study was to evaluate the precision and accuracy of the determinations of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and U in certified reference materials (CRMs). To solve the problem of interference from fission products of U in the determination of lanthanides were obtained correction factors for this interference for 140 La, 141 Ce, 143 Ce, 153 Sm and 147 Nd. The experimental procedure of Neutron Activation Analysis consisted of irradiating aliquots of each of the CRMs with synthetic standards of elements under thermal neutron flux of the IEA-R1 nuclear reactor, followed by gamma-ray spectrometry using a high-resolution hyperpurity GE detector. The analyzes of CRMs indicate good accuracy and precision of results, demonstrating the feasibility of applying of established procedure in NAA of elements studied in organic vegetable matrices

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

International Nuclear Information System (INIS)

Snell, J.P.

2009-01-01

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

k0-NAA applied to certified reference materials and hair samples. Evaluation of exposure level in a galvanising industry

International Nuclear Information System (INIS)

Menezes, M.A. de B.C.; Pereira Maia, E.C.

2000-01-01

The k 0 parametric neutron activation analysis has been applied since 1995 in the Radiochemical Sector/CDTN, Belo Horizonte, Brazil. Several certified reference materials were studied with the aim of analysing biological samples. This work is related to an IAEA co-ordinated research project whose goal is to make a survey of the exposures to metals related to occupational diseases. It has been conducted by CDTN and government departments of health. The hair samples as bioindicators were donated by galvanising factory workers in Belo Horizonte. This city and surrounding area are important industrial centres and that industry is responsible for the majority of patients who look for medical assistance because of metal contamination. The Al, Co, Cu, Cr, La, Mn, Sb and V concentrations determined in the workers' samples suggest endogenous contamination. (author)

Preparation and certification of reference materials for the nuclear industry

International Nuclear Information System (INIS)

Wagner, J.F.

1994-01-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-07-15

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

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

International Nuclear Information System (INIS)

Landsberger, S.; Davidson, W.F.

1985-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-11-01

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

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

International Nuclear Information System (INIS)

Noyori, Amanda; Saiki, Mitiko

2017-01-01

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

Determination of the carbon, hydrogen and nitrogen contents of alanine and their uncertainties using the certified reference material L-alanine (NMIJ CRM 6011-a).

Science.gov (United States)

Itoh, Nobuyasu; Sato, Ayako; Yamazaki, Taichi; Numata, Masahiko; Takatsu, Akiko

2013-01-01

The carbon, hydrogen, and nitrogen (CHN) contents of alanine and their uncertainties were estimated using a CHN analyzer and the certified reference material (CRM) L-alanine. The CHN contents and their uncertainties, as measured using the single-point calibration method, were 40.36 ± 0.20% for C, 7.86 ± 0.13% for H, and 15.66 ± 0.09% for N; the results obtained using the bracket calibration method were also comparable. The method described in this study is reasonable, convenient, and meets the general requirement of having uncertainties ≤ 0.4%.

Catalogue of reference materials of interest to nuclear energy

International Nuclear Information System (INIS)

1974-12-01

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

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

International Nuclear Information System (INIS)

Jacimovic, R.

2014-01-01

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

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...

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

International Nuclear Information System (INIS)

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

2004-01-01

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

Characterization of the NIST shellfish Standard Reference Material 4358

International Nuclear Information System (INIS)

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

2013-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-10-15

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Preparation and analysis of a marble reference material

International Nuclear Information System (INIS)

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

1988-01-01

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

Development and use of reference materials and quality control materials

International Nuclear Information System (INIS)

2003-04-01

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

Development and use of reference materials and quality control materials

Energy Technology Data Exchange (ETDEWEB)

NONE

2003-04-01

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

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)

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

International Nuclear Information System (INIS)

Muramatsu, Y.; Parr, R.M.

1985-12-01

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

Development of natural matrix reference materials for monitoring environmental radioactivity

International Nuclear Information System (INIS)

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

1992-01-01

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2002-01-01

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

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

Directory of Open Access Journals (Sweden)

D. A. Chupakhin

2016-01-01

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

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

International Nuclear Information System (INIS)

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

1990-01-01

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

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

International Nuclear Information System (INIS)

De Boer, J.

1999-01-01

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

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

Science.gov (United States)

Quevauviller, P; Bennink, D; Bøwadt, S

2001-05-01

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

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.)

BL-2a and BL-4a: certified uranium reference ores

International Nuclear Information System (INIS)

Steger, H.F.; Bowman, W.S.; Zechanowitsch, G.; Sutarno, R.

1982-05-01

Samples of two uranium ores BL-2a and BL-4a from Beaverlodge, Saskatchewan, were prepared as compositional reference materials to replace the similar certified ores, BL-2 and BL-4, of which the stock had been exhausted. Each ore was ground to minus 74 μm, blended in one lot and bottled in 200-g units. The homogeneity of the ores with respect to uranium was confirmed by both a neutron activation and a fluorimetric analytical procedure performed by two commercial laboratories. The recommended value for uranium is based on the results of one determination on each of 25 bottles by the volumetric-umpire method performed at CANMET. A statistical analysis of the data gave a recommended value for uranium of 0.426% for BL-2a and 0.1248% for BL-4a

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

Science.gov (United States)

Muntau, H

2001-06-01

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

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

International Nuclear Information System (INIS)

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

2001-01-01

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

Certification of biological candidates reference materials by neutron activation analysis

Science.gov (United States)

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

2018-03-01

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

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

International Nuclear Information System (INIS)

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

1991-01-01

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

Differences in serum thyroglobulin measurements by 3 commercial immunoradiometric assay kits and laboratory standardization using Certified Reference Material 457 (CRM-457).

Science.gov (United States)

Lee, Ji In; Kim, Ji Young; Choi, Joon Young; Kim, Hee Kyung; Jang, Hye Won; Hur, Kyu Yeon; Kim, Jae Hyeon; Kim, Kwang-Won; Chung, Jae Hoon; Kim, Sun Wook

2010-09-01

Serum thyroglobulin (Tg) is essential in the follow-up of patients with differentiated thyroid carcinoma (DTC). However, interchangeability and standardization between Tg assays have not yet been achieved, even with the development of an international Tg standard (Certified Reference Material 457 [CRM-457]). Serum Tg from 30 DTC patients and serially diluted CRM-457 were measured using 3 different immunoradiometric assays (IRMA-1, IRMA-2, IRMA-3). The intraclass correlation coefficient (ICC) method was used to describe the concordance of each IRMA to CRM-457. The serum Tg measured by 3 different IRMAs correlated well (r > .85, p CRM-457, showed the best ICC (p(1) = .98) for the CRM-457. Hospitals caring for patients with DTC should either set their own cutoffs for IRMAs for Tg based on their patient pools, or adopt IRMAs standardized to CRM-457 and calibrate their laboratory using CRM-457.

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

International Nuclear Information System (INIS)

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

1989-01-01

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

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

International Nuclear Information System (INIS)

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

2007-12-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-12-15

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

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

International Nuclear Information System (INIS)

Seward, R.W.

1975-06-01

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

Determination of metal concentrations in certified plastic reference materials after small-size autoclave and microwave-assisted digestion followed with inductively coupled plasma optical emission spectrometry

Science.gov (United States)

Lehtimäki, Esa; Väisänen, Ari

2017-01-01

The digestion methods for the determination of As, Cd, Cr, Pb, Sb, Sn and Zn concentrations in plastic samples using microwave-assisted digestion (MW-AD) and small-size autoclave digestion was developed. The certified polyethylene, polypropylene, polyvinyl chloride and acrylonitrile butadiene styrene certified reference materials were used in order to find digestion method working properly for several sample matrices. Efficiency of the digestion methods was evaluated by analyzing the residual carbon in digests by TOC analyzer. MW-AD using a mixture of 7 mL of HNO3 and 3 mL of H2O2 as a digestion solution resulted in excellent recoveries for As, Cd, Pb, Sb and Zn, and were in the range of 92-107% for all the analytes except Pb in polyethylene material. Autoclave digestion using 5 mL of concentrated HNO3 as a digestion solution resulted in similar recoveries with the exception of a higher As recovery (98%). Tin recovery resulted in low level after both MW-AD and autoclave digestion. Autoclave digestion was further developed resulting in a partially open two-step digestion process especially for the determination of Sn and Cr. The method resulted in higher recoveries of Sn and Cr (87 and 76%) but with the lower concentration of easily volatile As, Cd and Sb.

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

International Nuclear Information System (INIS)

Woittiez, J.R.W.

1990-01-01

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

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

International Nuclear Information System (INIS)

Freitas, M.C.

1993-01-01

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

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

Science.gov (United States)

Sharpless, K E; Gill, L M

2000-01-01

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

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

International Nuclear Information System (INIS)

Moreira, Edson Goncalves

2010-01-01

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

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.

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

International Nuclear Information System (INIS)

Crawford, D.W.

1990-07-01

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

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

International Nuclear Information System (INIS)

Dung, Ho Manh; Vu, Cao Dong; Y, Truong; Sy, Nguyen Thi

2006-01-01

The airborne particulate matter (APM) samples have been collected in 2004 using two types of polycarbonate membrane filter PM 2.5 and PM 2.5-10 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 k 0 -INAA procedure using K o -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 k 0 -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)

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

Science.gov (United States)

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

2010-05-01

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

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

Science.gov (United States)

In't Veld, P H

1998-11-24

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

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

Science.gov (United States)

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

2004-01-01

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

The development and certification of Standard Reference Materials (SRMs) to assess and ensure accurate measurement of Pb in the environment.

Science.gov (United States)

Fassett, J D; MacDonald, B S

2001-08-01

The National Institute of Standards and Technology (NIST) has had a major quality-assurance role in the federal effort to reduce lead poisoning of children in the United States through its mission of ensuring the accuracy of chemical measurements. NIST certifies reference materials (standard reference materials--SRMs) that are used to benchmark measurements by secondary and field methods of analysis--to ensure that decisions of great health and economic impact are soundly based on good measurement science. Over the past 10 years, in cooperation with the US Environmental Protection Agency (EPA), US Department of Housing and Urban Development (HUD), and the United States Geological Survey (USGS), NIST has prepared and certified SRMs for lead content in soil, indoor dust, and paint. The role of these materials in meeting regulatory and abatement needs is described and their certified values are summarized.

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

International Nuclear Information System (INIS)

Ihnat, Milan

2002-01-01

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

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)

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

1997-01-01

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)

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

International Nuclear Information System (INIS)

2011-01-01

Reference Materials are an important requirement for any sort of quantitative chemical and radiochemical analysis. Laboratories need them for calibration and quality control throughout their analytical work. The IAEA started to produce reference materials in the early 1960's to meet the needs of the analytical laboratories in its Member States that required reference materials for quality control of their measurements. The initial efforts were focused on the preparation of environmental reference materials containing anthropogenic radionuclides for use by those laboratories employing nuclear analytical techniques. These reference materials were characterized for their radionuclide content through interlaboratory comparison involving a core group of some 10 to 20 specialist laboratories. The success of these early exercises led the IAEA to extend its activities to encompass both terrestrial and marine reference materials containing primordial radionuclides and trace elements. Within the frame of IAEA activities in production and certification of reference materials, this report describes the certification of the IAEA-444 and IAEA-445: soil and water spiked with gamma emitting radionuclides respectively. Details are given on methodologies and data evaluation

The synthesis and certification of zirconia certified reference materials (CRM) as a processed result of zircon sand

International Nuclear Information System (INIS)

Samin; Supriyanto C; Sajima

2016-01-01

In order to support the pilot plant of zirconia production at PSTA-BATAN, synthesis and certification of zirconia certified reference materials (CRM) is absolutely needed. The synthesis and certification of zirconia CRM has been carried out from the row material of zirconium oxide chloride as a processed result of Kalimantan zircon sand. Zirconium oxide chloride dissolved in distilled water (1:10), added by ammonia at pH 10, it was formed a zirconium hydroxide precipitate. Zirconium hydroxide was heated at 110 °C and calcination at a temperature of 900 °C in order to obtain zirconia. Zirconia was dried at 110 °C, crushed and sieved to obtain a grain size of 200 mesh qualify. Zirconia powder was homogenized and then treated by homogenation test, stabilization test, characterization test and water content test. In the evaluation of the test data showed that candidate of CRM zirconia were homogeneous, stable, contain the monoklin of baddeleyite minerals and the water content obtained was less than 1%. It was concluded that zirconia powder are already physical qualified as CRM. Certificate of test results on parameters of zirconia CRM from 7 accredited laboratories using statistical methods obtained 9 oxides were ZrO_2 : (95.422 ± 0.027)%; HfO_2: (1.443 ± 0.004)%; SiO_2 : (0.535 ± 0.002)%; Al_2O_3 : (0.362 ± 0.012)%; Fe_2O_3 : (0.028 ± 0.003)%; TiO_2: (0.026 ± 0.001) %; Na_2O: (0.262 ± 0.026)%; Nd_2O_3 : (0.0367 ± 0.007)%; CeO_2: (0.131 ± 0.013)%. This certification was traceable to BCS-CRM No. 358 zirconia from BAS-France. (author)

Development of certified matrix-based reference material of genetically modified rice event TT51-1 for real-time PCR quantification.

Science.gov (United States)

Jiang, Yu; Yang, Hui; Quan, Sheng; Liu, Yinan; Shen, Ping; Yang, Litao

2015-09-01

In 2009, the genetically modified (GM) rice event TT51-1 with an engineered insect resistance trait became the first GM rice event to be granted certification for safe production in China, and its derivative lines Bt 63 and Huahui No.1 are expected to be commercialized soon. The development of certified reference material (CRM) for TT51-1 is necessary to monitor and inspect the TT51-1 event and its derivates. In this work, we developed four matrix-based TT51-1 rice CRMs (TT51-1a, TT51-1b, TT51-1c, and TT51-1d) with different TT51-1 mass fraction ratios by blending seed powders of homozygous TT51-1 and its recipient cultivar Minghui 63. The between-bottle homogeneity and the within-bottle homogeneity were tested, and good results were obtained. The potential degradation during transportation and shelf life were evaluated, and demonstrated an expiration period of at least 36 months. The characterization values of the four TT51-1 CRMs based on the mass fraction ratio were 1000.000 ± 51.430 g/kg, 49.940 ± 4.620 g/kg, 9.990 ± 1.110 g/kg, and 4.990 ± 0.620 g/kg, respectively. The characterization values based on the copy number ratio were certified by digital PCR analysis as 97.442 ± 5.253 %, 4.851 ± 0.486 %, 1.042 ± 0.135 %, and 0.556 ± 0.073 %, respectively. These results suggested that the TT51-1 matrix-based CRMs developed are of high quality and can be used as potential calibrators for TT51-1 GM rice inspection and monitoring.

Certification of caffeine reference material purity by ultraviolet/visible spectrophotometry and high-performance liquid chromatography with diode-array detection as two independent analytical methods.

Science.gov (United States)

Shehata, A B; Rizk, M S; Rend, E A

2016-10-01

Caffeine reference material certified for purity is produced worldwide, but no research work on the details of the certification process has been published in the literature. In this paper, we report the scientific details of the preparation and certification of pure caffeine reference materials. Caffeine was prepared by extraction from roasted and ground coffee by dichloromethane after heating in deionized water mixed with magnesium oxide. The extract was purified, dried, and bottled in dark glass vials. Stratified random selection was applied to select a number of vials for homogeneity and stability studies, which revealed that the prepared reference material is homogeneous and sufficiently stable. Quantification of caffeine purity % was carried out using a calibrated UV/visible spectrophotometer and a calibrated high-performance liquid chromatography with diode-array detection method. The results obtained from both methods were combined to drive the certified value and its associated uncertainty. The certified value of the reference material purity was found to be 99.86% and its associated uncertainty was ±0.65%, which makes the candidate reference material a very useful calibrant in food and drug chemical analysis. Copyright © 2016. Published by Elsevier B.V.

Certification of caffeine reference material purity by ultraviolet/visible spectrophotometry and high-performance liquid chromatography with diode-array detection as two independent analytical methods

Directory of Open Access Journals (Sweden)

A.B. Shehata

2016-10-01

Full Text Available Caffeine reference material certified for purity is produced worldwide, but no research work on the details of the certification process has been published in the literature. In this paper, we report the scientific details of the preparation and certification of pure caffeine reference materials. Caffeine was prepared by extraction from roasted and ground coffee by dichloromethane after heating in deionized water mixed with magnesium oxide. The extract was purified, dried, and bottled in dark glass vials. Stratified random selection was applied to select a number of vials for homogeneity and stability studies, which revealed that the prepared reference material is homogeneous and sufficiently stable. Quantification of caffeine purity % was carried out using a calibrated UV/visible spectrophotometer and a calibrated high-performance liquid chromatography with diode-array detection method. The results obtained from both methods were combined to drive the certified value and its associated uncertainty. The certified value of the reference material purity was found to be 99.86% and its associated uncertainty was ±0.65%, which makes the candidate reference material a very useful calibrant in food and drug chemical analysis.

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

International Nuclear Information System (INIS)

Suzuki, Shogo; Hirai, Shoji

1990-01-01

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

Final certification of two new reference materials for inorganic trace analysis

International Nuclear Information System (INIS)

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

2004-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-09-15

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

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

International Nuclear Information System (INIS)

Mandiwana, Khakhathi L.; Panichev, Nikolay

2010-01-01

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

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.

Need for organic reference materials in marine science

Energy Technology Data Exchange (ETDEWEB)

Wells, D.E.

1988-12-01

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

Application of reference materials for quality assessment in neutron activation analysis

International Nuclear Information System (INIS)

Obrusnik, I.; Eckschlager, K.

1993-01-01

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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

International Nuclear Information System (INIS)

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

2000-01-01

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

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

International Nuclear Information System (INIS)

1994-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

NONE

1994-07-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-07-15

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

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.

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

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt

1995-01-01

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

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.

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)

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.

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

A comparison of chemical reference materials for solution calorimeters.

Science.gov (United States)

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

2005-08-11

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

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

Directory of Open Access Journals (Sweden)

Shikha Awasthi

2017-06-01

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

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

International Nuclear Information System (INIS)

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

1990-01-01

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

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

A reference material for the determination of overall migration from a plastic coextrudate into the fatty food simulant olive oil was produced and certified in an interlaboratory study. The analyses were carried out according to the ENV 1186 standard from the European Committee for Standardization...... (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...

Development of a certified reference material (NMIJ CRM 7531-a) for the determination of trace cadmium and other elements in brown rice flour.

Science.gov (United States)

Miyashita, Shin-ichi; Inagaki, Kazumi; Narukawa, Tomohiro; Zhu, Yanbei; Kuroiwa, Takayoshi; Hioki, Akiharu; Chiba, Koichi

2012-01-01

A certified reference material (CRM) for trace cadmium and other elements in brown rice flour was developed at the National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder after drying and frozen pulverization of fresh brown rice obtained from a Japanese domestic market. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), ICP high-resolution mass spectrometry, isotope-dilution ICP-MS, ICP optical emission spectrometry, and graphite-furnace atomic-absorption spectrometry. Property values were provided for six elements (Mn, Fe, Cu, Zn, As, and Cd). The concentration range of the property values was from 0.280 mg kg(-1) of As to 31.8 mg kg(-1) of Zn. The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, characterization, difference among analytical methods, dry-mass correction factor, and calibration standard. The range of the relative combined standard uncertainties was from 1.1% of Zn to 1.6% of As.

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

International Nuclear Information System (INIS)

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

2011-01-01

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

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)

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

International Nuclear Information System (INIS)

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

2003-01-01

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

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

International Nuclear Information System (INIS)

Kobayashi, K.; Kudo, K.

1979-01-01

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

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

International Nuclear Information System (INIS)

2002-01-01

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

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

International Nuclear Information System (INIS)

2002-06-01

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

Preparation, characterization and certification of uranium isotope reference materials

International Nuclear Information System (INIS)

Oliveira Junior, Olivio Pereira de

2006-01-01

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

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

Directory of Open Access Journals (Sweden)

Maria Helena Wohlers Morelli Cardoso

2010-06-01

Full Text Available Neste trabalho são apresentados os resultados dos estudos de estabilidade referentes à produção de um material de referência certificado. Foram avaliados níveis residuais de concentração dos agrotóxicos γ-HCH, fenitrotiona, clorpirifós e procimidona em polpa de tomate. A pasteurização e a irradiação gama foram empregadas à polpa de tomate, visando manter a integridade da amostra candidata a material de referência. A polpa foi preparada e dividida em duas partes. Cada parte foi fortificada com os referidos agrotóxicos na faixa de concentração de 0,1 a 0,2 mg.kg-1. Uma das partes foi submetida à pasteurização a 90 °C por 4 minutos e a outra parte foi irradiada com dose de 2,0 kGy depois de homogeneizada. A estabilidade e a incerteza da amostra, correspondente ao período de tempo avaliado, foram determinadas através da análise de regressão em conjunto com a ANOVA. Os resultados indicaram que ambos os procedimentos de preparo da amostra são adequados para a conservação da polpa de tomate fortificada com os quatro agrotóxicos, com vantagem para o tratamento por irradiação com a dose de 2,0 kGy.This research presents the results of stability studies regarding the production of certified reference materials. The residual concentration levels of four pesticides, namely γ-HCH, fenitrothion, chlorpyrifos, and procymidone were investigated. Pasteurization combined with gamma irradiation was used to maintain the integrity of the mixture tested as a reference material candidate. The pulp was prepared and split into two parts. Each part was then spiked with those pesticides in the concentration range of 0.1 to 0.2 mg.kg-1 in tomato pulp. One of them was submitted to pasteurization at 90 °C for 4 minutes after being homogenized, and the other was irradiated with a gamma dose of 2.0 kGy. The material stability and the corresponding uncertainty during the period of time evaluated were determined using regression analysis and

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

Science.gov (United States)

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

2008-10-01

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

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

International Nuclear Information System (INIS)

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

1992-01-01

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

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

Science.gov (United States)

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

2008-12-01

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

Determination of trace elements in the human hair reference material, HH-I, by neutron activation analysis and atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Coetzee, P.; Pieterse, H.

1986-01-01

Analytical procedures are presented and problem areas identified with regard to the determination of trace elements in IAEA powdered human hair reference material, HH-I, of limited sample size (100-200 mg), by NAA and graphite furnace AAS. Results obtained for the twelve elements As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Sb, Se, and Zn studied in human hair and other biological reference material like orchard leaves, seaplant material, and copepod compare satisfactorily with the certified values

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.

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

International Nuclear Information System (INIS)

Siddique, N.; Waheed, S.

2009-01-01

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

Determination of sampling constants in NBS geochemical standard reference materials

International Nuclear Information System (INIS)

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

1986-01-01

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

Development of a certified reference material (NMIJ CRM 7505-a) for the determination of trace elements in tea leaves.

Science.gov (United States)

Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Kuroiwa, Takayoshi; Chiba, Koichi

2011-01-01

A certified reference material (CRM) for trace elements in tea leaves has been developed in National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder (<90 µm) after frozen pulverization of washed and dried fresh tea leaves from a tea plant farm in Shizuoka Prefecture, Japan. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), high-resolution (HR-) ICP-MS, isotope-dilution (ID-) ICP-MS, inductively coupled plasma optical emission spectrometry (ICP-OES), graphite-furnace atomic-absorption spectrometry (GF-AAS) and flame atomic-absorption spectrometry (FAAS). Property values were provided for 19 elements (Ca, K, Mg, P, Al, B, Ba, Cd, Cu, Fe, Li, Mn, Na, Ni, Pb, Rb, Sr, Zn and Co) and informative values for 18 elements (Ti, V, Cr, Y, and all of the lanthanides, except for Pm whose isotopes are exclusively radioactive). The concentration ranges of property values and informative values were from 1.59% (mass) of K to 0.0139 mg kg(-1) of Cd and from 0.6 mg kg(-1) of Ti to 0.0014 mg kg(-1) of Lu, respectively. Combined relatively standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, analytical methods, characterization, calibration standard, and dry-mass correction factor. The range of the relative combined standard uncertainties was from 1.5% of Mg and K to 4.1% of Cd.

Certified Reference Material for Use in 1H, 31P, and 19F Quantitative NMR, Ensuring Traceability to the International System of Units.

Science.gov (United States)

Rigger, Romana; Rück, Alexander; Hellriegel, Christine; Sauermoser, Robert; Morf, Fabienne; Breitruck, KathrinBreitruck; Obkircher, Markus

2017-09-01

In recent years, quantitative NMR (qNMR) spectroscopy has become one of the most important tools for content determination of organic substances and quantitative evaluation of impurities. Using Certified Reference Materials (CRMs) as internal or external standards, the extensively used qNMR method can be applied for purity determination, including unbroken traceability to the International System of Units (SI). The implementation of qNMR toward new application fields, e.g., metabolomics, environmental analysis, and physiological pathway studies, brings along more complex molecules and systems, thus making use of 1H qNMR challenging. A smart workaround is possible by the use of other NMR active nuclei, namely 31P and 19F. This article presents the development of three classes of qNMR CRMs based on different NMR active nuclei (1H, 31P, and 19F), and the corresponding approaches to establish traceability to the SI through primary CRMs from the National Institute of Standards and Technology and the National Metrology Institute of Japan. These TraceCERT® qNMR CRMs are produced under ISO/IEC 17025 and ISO Guide 34 using high-performance qNMR.

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.

Multielement comparison of instrumental neutron activation analysis techniques using reference materials

International Nuclear Information System (INIS)

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

1995-01-01

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

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

International Nuclear Information System (INIS)

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

1993-01-01

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

Uranium reference materials

International Nuclear Information System (INIS)

Donivan, S.; Chessmore, R.

1987-07-01

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

Development of Certified Matrix-Based Reference Material as a Calibrator for Genetically Modified Rice G6H1 Analysis.

Science.gov (United States)

Yang, Yu; Li, Liang; Yang, Hui; Li, Xiaying; Zhang, Xiujie; Xu, Junfeng; Zhang, Dabing; Jin, Wujun; Yang, Litao

2018-04-11

The accurate monitoring and quantification of genetically modified organisms (GMOs) are key points for the implementation of labeling regulations, and a certified reference material (CRM) acts as the scaleplate for quantifying the GM contents of foods/feeds and evaluating a GMO analytical method or equipment. Herein we developed a series of CRMs for transgenic rice event G6H1, which possesses insect-resistant and herbicide-tolerant traits. Three G6H1 CRMs were produced by mixing seed powders obtained from homozygous G6H1 and its recipient cultivar Xiushui 110 at mass ratios of 49.825%, 9.967%, and 4.986%. The between-bottle homogeneity and within-bottle homogeneity were thoroughly evaluated with consistent results. The potential DNA degradation in transportation and shelf life were evaluated with an expiration period of at least 12 months. The property values of three CRMs (G6H1 a , G6H1 b , G6H1 c ) were given as (49.825 ± 0.448) g/kg, (9.967 ± 1.757) g/kg, and (4.986 ± 1.274 g/kg based on mass fraction ratio, respectively. Furthermore, the three CRMs were characterized with values of (5.01 ± 0.08)%, (1.06 ± 0.22)%, and (0.53 ± 0.11)% based on the copy number ratio using the droplet digital PCR method. All results confirmed that the produced G6H1 matrix-based CRMs are of high quality with precise characterization values and can be used as calibrators in GM rice G6H1 inspection and monitoring and in evaluating new analytical methods or devices targeting the G6H1 event.

A certified urea reference material (NMIJ CRM 6006-a) as a reliable calibrant for the elemental analyses of amino acids and food samples.

Science.gov (United States)

Itoh, Nobuyasu; Yamazaki, Taichi; Sato, Ayako; Numata, Masahiko; Takatsu, Akiko

2014-01-01

We examined the reliability of a certified reference material (CRM) for urea (NMIJ CRM 6006-a) as a calibrant for N, C, and H in elemental analyzers. Only the N content for this CRM is provided as an indicative value. To estimate the C and H contents of the urea CRM, we took into account the purity of the urea and the presence of other identified impurities. When we examined the use of various masses of the calibrant (0.2 to 2 mg), we unexpectedly observed low signal intensities for small masses of H and N, but these plateaued at about 2 mg. We therefore analyzed four amino acid CRMs and four food CRMs on a 2-mg scale with the urea CRM as the calibrant. For the amino acid CRMs, the differences in the analytical and theoretical contents (≤0.0026 kg/kg) were acceptable with good repeatability (≤0.0013 kg/kg in standard deviation; n = 4). For food CRMs, comparable repeatabilities to those obtained with amino acid CRMs (≤0.0025 kg/kg in standard deviation; n = 4) were obtained. The urea CRM can therefore be used as a reliable calibrant for C, H, and N in an elemental analyzer.

Nanogram determination of arsenic in biological reference materials by non-destructive Compton suppression neutron activation analysis

International Nuclear Information System (INIS)

Petra, M.; Landsberger, S.; Swift, G.

1990-01-01

Non-destructive epithermal neutron activation analysis in conjunction with Compton suppression has been applied to determine arsenic in seven biological standard reference materials from the National Institute of Standards and Technology. The accuracy is in excellent agreement with all the certified values and compilation results. For four of the materials detection limits between 1-4 ng/g were easily achieved while for three others they ranged from 18-50 ng/g. Overall analytical precision typically varied between 2-4% for five of the reference materials while for two other it was between 12-16%. These methods clearly demonstrate that through a judicious approach of anti-coincidence techniques, nanogram quantities of arsenic can be reliably determined without the need for labor intensive chemical separations. (orig.)

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

International Nuclear Information System (INIS)

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

2002-01-01

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

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

International Nuclear Information System (INIS)

Greenberg, R.R.; Zeisler, R.; Mackey, E.A.

2006-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1989-04-15

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

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

Science.gov (United States)

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

2017-11-07

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

IAEA biological reference materials

International Nuclear Information System (INIS)

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

1988-01-01

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

Iodine in different food articles and standard reference materials

International Nuclear Information System (INIS)

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

1990-01-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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

International Nuclear Information System (INIS)

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

1996-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Towards absolute quantification of allergenic proteins in food--lysozyme in wine as a model system for metrologically traceable mass spectrometric methods and certified reference materials.

Science.gov (United States)

Cryar, Adam; Pritchard, Caroline; Burkitt, William; Walker, Michael; O'Connor, Gavin; Burns, Duncan Thorburn; Quaglia, Milena

2013-01-01

Current routine food allergen quantification methods, which are based on immunochemistry, offer high sensitivity but can suffer from issues of specificity and significant variability of results. MS approaches have been developed, but currently lack metrological traceability. A feasibility study on the application of metrologically traceable MS-based reference procedures was undertaken. A proof of concept involving proteolytic digestion and isotope dilution MS for quantification of protein allergens in a food matrix was undertaken using lysozyme in wine as a model system. A concentration of lysozyme in wine of 0.95 +/- 0.03 microg/g was calculated based on the concentrations of two peptides, confirming that this type of analysis is viable at allergenically meaningful concentrations. The challenges associated with this promising method were explored; these included peptide stability, chemical modification, enzymatic digestion, and sample cleanup. The method is suitable for the production of allergen in food certified reference materials, which together with the achieved understanding of the effects of sample preparation and of the matrix on the final results, will assist in addressing the bias of the techniques routinely used and improve measurement confidence. Confirmation of the feasibility of MS methods for absolute quantification of an allergenic protein in a food matrix with results traceable to the International System of Units is a step towards meaningful comparison of results for allergen proteins among laboratories. This approach will also underpin risk assessment and risk management of allergens in the food industry, and regulatory compliance of the use of thresholds or action levels when adopted.

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

International Nuclear Information System (INIS)

Kucera, J.; Soukal, L.

1993-01-01

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

Certification of a reference material for determination of total cyanide in soil to support implementation of the International Standard ISO 11262:2011.

Science.gov (United States)

Scharf, Holger; Bremser, Wolfram

2015-04-01

Cyanides are among the most important inorganic pollutants to be tested and monitored in environmental compartments. They can be distinguished and determined as free cyanide, weak acid dissociable cyanide or as total cyanide. However, in any case obtained, measurement results are operationally defined referring to the applied analytical method. In 2011, the International Standard ISO 11262 has been published which specifies a normative analytical method for the determination of total cyanide in soil. The objective of the project described in this paper was to provide the first soil reference material (CRM) certified for its mass fraction of total cyanide on the basis of this standard. A total of 12 German laboratories with proven experience in the determination of cyanides in environmental samples participated in the certification study. Measurement results were evaluated in full compliance with the requirements of ISO Guide 35. Taking into account the results of the inter-laboratory comparison as well as the outcome of the homogeneity and stability studies, a certified mass fraction of total cyanide of 21.1 mg/kg and an expanded uncertainty (k = 2) of 1.3 mg/kg were assigned to the material. The reference material has been issued as CRM BAM-U114.

Characterization of standard reference material 2944, Bi-ion-doped glass, spectral correction standard for red fluorescence

International Nuclear Information System (INIS)

DeRose, Paul C.; Smith, Melody V.; Anderson, Jeffrey R.; Kramer, Gary W.

2013-01-01

Standard Reference Material (SRM) 2944 is a cuvette-shaped, Bi-ion-doped glass, recommended for optimal use for relative spectral correction of emission from 590 nm to 805 nm and day-to-day performance verification 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 and temperature coefficient of fluorescence intensity. The expanded uncertainties (k=2) in the certified spectrum are about 4% around the nominal peak maximum at 704 nm and increase to about 6% at the wings, using an excitation wavelength of 515 nm. -- Highlights: ► The fluorescence emission spectrum of SRM 2944 was determined for spectral correction. ► This Bi-ion-doped glass has been certified in the fluorescence region from 530 nm to 830 nm. ► Fluorescence properties of the glass were determined, e.g., anisotropy, lifetime. ► SRM 2944 is photostable under common visible lamp excitation, when UV light is not present

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

International Nuclear Information System (INIS)

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

1992-01-01

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

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)

Miura, T.; Kuroiwa, T.; Chiba, K.; Matsue, H.

2008-01-01

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)

Preparation and certification of hijiki reference material, NMIJ CRM 7405-a, from the edible marine algae hijiki (Hizikia fusiforme).

Science.gov (United States)

Narukawa, Tomohiro; Inagaki, Kazumi; Zhu, Yanbei; Kuroiwa, Takayoshi; Narushima, Izumi; Chiba, Koichi; Hioki, Akiharu

2012-02-01

A certified reference material, NMIJ CRM 7405-a, for the determination of trace elements and As(V) in algae was developed from the edible marine hijiki (Hizikia fusiforme) and certified by the National Metrology Institute of Japan (NMIJ), the National Institute of Advanced Industrial Science and Technology (AIST). Hijiki was collected from the Pacific coast in the Kanto area of Japan, and was washed, dried, powdered, and homogenized. The hijiki powder was placed in 400 bottles (ca. 20 g each). The concentrations of 18 trace elements and As(V) were determined by two to four independent analytical techniques, including (ID)ICP-(HR)MS, ICP-OES, GFAAS, and HPLC-ICP-MS using calibration solutions prepared from the elemental standard solution of Japan calibration service system (JCSS) and the NMIJ CRM As(V) solution, and whose concentrations are certified and SI traceable. The uncertainties of all the measurements and preparation procedures were evaluated. The values of 18 trace elements and As(V) in the CRM were certified with uncertainty (k = 2).

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...

Nuclear microprobe analysis of the standard reference materials

International Nuclear Information System (INIS)

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

2002-01-01

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

Consensus values for NIST biological and environmental Standard Reference Materials

International Nuclear Information System (INIS)

Roelandts, I.; Gladney, E.S.

1998-01-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Study of the structure and development of the set of reference materials of composition and structure of heat resisting nickel and intermetallic alloys

Directory of Open Access Journals (Sweden)

E. B. Chabina

2016-01-01

Full Text Available Relevance of research: There are two sizes (several microns and nanodimensional of strengthening j'-phase in single-crystal heat resisting nickel and intermetallic alloys, used for making blades of modern gas turbine engines (GTD. For in-depth study of structural and phase condition of such alloys not only qualitative description of created structure is necessary, but quantitative analysis of alloy components geometrical characteristics. Purpose of the work: Development of reference material sets of heat resisting nickel and intermetallic alloy composition and structure. Research methods: To address the measurement problem of control of structural and geometrical characteristics of single-crystal heat resisting and intermetallic alloys by analytical microscopy and X-ray diffraction analysis the research was carried out using certified measurement techniques on facilities, entered in the Register of Measurement Means of the Russian Federation. The research was carried out on microsections, foils and plates, cut in the plane {100}. Results: It is established that key parameters, defining the properties of these alloys are particle size of strengthening j' -phase, the layer thickness of j-phase between them and parameters of phases lattice. Metrological requirements for reference materials of composition and structure of heat resisting nickel and intermetallic alloys are formulated. The necessary and sufficient reference material set providing the possibility to determine the composition and structure parameters of single-crystal heat resisting nickel and intermetallic alloys is defined. The developed RM sets are certified as in-plant reference materials. Conclusion: The reference materials can be used for graduation of spectral equipment when conducting element analysis of specified class alloys; for calibration of means of measuring alloy structure parameters; for measurement of alloys phases lattice parameters; for structure reference pictures

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

Energy Technology Data Exchange (ETDEWEB)

Shimizu, Yoshitaka, E-mail: y-shimizu@aist.go.jp; Ohte, Yoko; Kato, Kenji

2013-09-20

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.

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

Science.gov (United States)

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

2007-02-01

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

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

International Nuclear Information System (INIS)

2002-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

NONE

2002-07-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Determination of polychlorinated dibenzo-p-dioxin and dibenzofuran congeners in air particulate and marine sediment standard reference materials (SRMs).

Science.gov (United States)

Chiu, C H; Turle, R; Poole, G; Thibert, B; Brubaker, W W; Schantz, M M; Wise, S A

2001-02-01

Due to the limited number of environmental matrix certified reference materials (CRMs) with assigned values for natural levels of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), an interlaboratory study was undertaken by the National Institute of Standards and Technology (NIST) and Environment Canada to establish reference concentration values for selected PCDD/Fs in two well-characterized NIST Standard Reference Materials (SRMs): SRM 1649a (Urban Dust) and SRM 1944 (New York/New Jersey Waterway Sediment). Results from 14 laboratories were used to provide reference values for the seventeen 2, 3, 7, 8-substituted PCDD/F congeners, the totals for individual tetra- through hepta-substituted PCDD/F homologues, and the total amount of tetra- through hepta-substituted PCDD/Fs. The mass fractions for the individual 2, 3, 7, 8-substituted congeners range from approximately 0.01 microg/kg to 7 microg/kg dry mass.

Characterize and Homogeneity Test of Phthalate and Phosphate Buffer as Reference Materials Candidate for Determination Ofacidic Value

OpenAIRE

Sujarwo, Sujarwo; Nuryatini, Nuryatini

2013-01-01

Measurement of pH is closely related to everyday life, such as in the area of environment, food and beverage, pharmaceuticals, and even metabolism process in human body. To ensure the quality of pH measurement, pH metershould be calibrated regularly and checked each time before used. Calibration and performance checking of pH meter requires traceable standard. The standard should be linked to CRM (Certified Reference Materials). Research Center for Chemistry - Indonesian Institute of Sciences...

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

Science.gov (United States)

Layne, G. D.

2009-12-01

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

International directory of certified radioactive sources

Energy Technology Data Exchange (ETDEWEB)

Grosse, G; Bambynek, W

1983-01-01

This directory lists the products of 16 suppliers of certified reference materials (CRM) of radioactivity as given in their catalogues. Included are only products for which certificates are delivered and whose uncertainties are given according to the rules defined in ICRU Report No. 12, ''Certification of Standardized Radioactive Sources'' (International Commission on Radiation and Measurements, Washington, 1968). Only those products are included of which the standard uncertainties according to the above rules are less than 10%. Prices of the products are not mentioned since they frequently change. The products are divided into four groups: Radioactive Solutions, Radioactive Gases, Solid Sources and Sources for Liquid Scintillation Counting).

International directory of certified radioactive sources

International Nuclear Information System (INIS)

Grosse, G.; Bambynek, W.

1983-01-01

This directory lists the products of 16 suppliers of certified reference materials (CRM) of radioactivity as given in their catalogues. Included are only products for which certificates are delivered and whose uncertainties are given according to the rules defined in ICRU Report No. 12, ''Certification of Standardized Radioactive Sources'' (International Commission on Radiation and Measurements, Washington, 1968). Only those products are included of which the standard uncertainties according to the above rules are less than 10%. Prices of the products are not mentioned since they frequently change. The products are divided into four groups: Radioactive Solutions, Radioactive Gases, Solid Sources and Sources for Liquid Scintillation Counting). (orig./WL)

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Comparability of reference values

International Nuclear Information System (INIS)

Rossbach, M.; Stoeppler, M.

1993-01-01

Harmonization of certified values in Reference Materials (RMs) can be carried out by applying nuclear analytical techniques to RMs of various matrix types and concentration levels. Although RMs generally should not be used as primary standards the cross evaluation of concentrations in RMs leads to better compatibility of reference values and thus to a greater agreement between analytical results from different laboratories using these RMs for instrument calibration and quality assurance. (orig.)

The Kjeldahl method as a primary reference procedure for total protein in certified reference materials used in clinical chemistry. II. Selection of direct Kjeldahl analysis and its preliminary performance parameters.

Science.gov (United States)

Vinklárková, Bára; Chromý, Vratislav; Šprongl, Luděk; Bittová, Miroslava; Rikanová, Milena; Ohnútková, Ivana; Žaludová, Lenka

2015-01-01

To select a Kjeldahl procedure suitable for the determination of total protein in reference materials used in laboratory medicine, we reviewed in our previous article Kjeldahl methods adopted by clinical chemistry and found an indirect two-step analysis by total Kjeldahl nitrogen corrected for its nonprotein nitrogen and a direct analysis made on isolated protein precipitates. In this article, we compare both procedures on various reference materials. An indirect Kjeldahl method gave falsely lower results than a direct analysis. Preliminary performance parameters qualify the direct Kjeldahl analysis as a suitable primary reference procedure for the certification of total protein in reference laboratories.

Contribution of nuclear analysis methods to the certification of BCR reference materials for non-metals in non-ferrous metals

International Nuclear Information System (INIS)

Pauwels, J.

1979-01-01

A number of reference materials for oxygen in different non-ferrous metals have been certified by BCR in the frame of a multidisciplinary Community project. The contribution of nuclear analysis methods is illustrated by several examples concerning the optimization of sample preparation techniques, the analysis of low and high oxygen non-ferrous metals and the extension of the program to other non-metals, especially nitrogen and carbon. (author)

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...

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

Science.gov (United States)

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

2016-01-01

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

Production of NDA Working Reference Materials for the Capability Evaluation Project

International Nuclear Information System (INIS)

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

1998-01-01

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

Determination of Sr, Ba, Rb, and Cs in biological reference materials using a radiochemical NAA group separation procedure

International Nuclear Information System (INIS)

Mizera, J.; Randa, Z.

2008-01-01

Strontium, barium, rubidium, and cesium in selected, predominantly biological, reference materials (NIST 1515, 1547, 1549, 1566a, 1571, 1577b, 2704, CTA-OTL-1, and Bowen's Kale) were determined using neutron activation analysis (NAA) in two different analytical modes - instrumental NAA with epithermal neutrons (ENAA), and NAA with radiochemical group separation of Sr-Ba and Rb-Cs (RNAA). The ENAA mode was based on long-term (5 h) irradiation of samples in a Cd shielding. The RNAA procedure was based on long-term (20 h) irradiation of samples, their decomposition / dissolution by alkaline-oxidative fusion, and precipitation of Sr and Ba sulfates, and sorption of Rb and Cs onto ammonium phosphomolybdate (APM). Both methods provided element contents in the analyzed reference materials consistent with certified and/or literature values. (author)

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

International Nuclear Information System (INIS)

Buerger, S.; Mathew, K.J.; Mason, P.; Narayanan, U.

2009-01-01

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)

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

International Nuclear Information System (INIS)

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

2006-01-01

Preparation, examination and certification of the new matrix reference material of biological origin: 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 dm 3 PE drum rotated in three directions. Preliminary homogeneity testing by X-ray fluorescence (XRF) method and final checking of homogeneity by neutron activation analysis (NAA) after distribution of the material into containers revealed, that it is sufficiently homogeneous at least for a sample size ≥ 100 mg. In order to assure the long-term stability, all containers with INCT-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 o C. Short-term stability was examined by the determination of concentrations of the selected elements in the bottle stored in the CO 2 incubator at 37 o C. The material was certified on the basis of a worldwide interlaboratory comparison, in which 92 laboratories from 19 countries participated providing 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

Preparation and certification of trace mercury in water standard reference materials

International Nuclear Information System (INIS)

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

1976-01-01

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

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

International Nuclear Information System (INIS)

1996-05-01

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

Reference material manufacture and certification for the AVNG

Energy Technology Data Exchange (ETDEWEB)

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

2010-07-09

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

Reference material manufacture and certification for the AVNG

Energy Technology Data Exchange (ETDEWEB)

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

2010-01-01

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

Reference material manufacture and certification for the AVNG

International Nuclear Information System (INIS)

2010-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-05-28

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

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)

Munoz, L; Andonie, O; Kohnenkamp, I

2000-01-01

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

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

International Nuclear Information System (INIS)

1985-03-01

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)

A Development Strategy for Creating a Suite of Reference Materials for the in-situ Microanalysis of Non-conventional Raw Materials

Science.gov (United States)

Renno, A. D.; Merchel, S.; Michalak, P. P.; Munnik, F.; Wiedenbeck, M.

2010-12-01

Recent economic trends regarding the supply of rare metals readily justify scientific research into non-conventional raw materials, where a particular need is a better understanding of the relationship between mineralogy, microstructure and the distribution of key metals within ore deposits (geometallurgy). Achieving these goals will require an extensive usage of in-situ microanalytical techniques capable of spatially resolving material heterogeneities which can be key for understanding better resource utilization. The availability of certified reference materials (CRMs) is an essential prerequisite for (1) validating new analytical methods, (2) demonstrating data quality to the contracting authorities, (3) supporting method development and instrument calibration, and (4) establishing traceability between new analytical approaches and existing data sets. This need has led to the granting of funding by the European Union and the German Free State of Saxony for a program to develop such reference materials . This effort will apply the following strategies during the selection of the phases: (1) will use exclusively synthetic minerals, thereby providing large volumes of homogeneous starting material. (2) will focus on matrices which are capable of incorporating many ‘important’ elements while avoid exotic compositions which would not be optimal matrix matches. (3) will emphasise those phases which remain stable during the various microanalytical procedure. This initiative will assess the homogeneity of the reference materials at sampling sizes ranging between 50 and 1 µm; it is also intended to document crystal structural homogeneity too, as this too may potentially impact specific analytical methods. As far as possible both definitive methods as well as methods involving matrix corrections will be used for determining the compositions of the of the individual materials. A critical challenge will be the validation of the determination of analytes concentrations

Nuclear measurements and reference materials

International Nuclear Information System (INIS)

1988-01-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Reference materials and interlaboratory comparison for actinide analysis

International Nuclear Information System (INIS)

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

2008-01-01

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

Science.gov (United States)

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

2008-07-01

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

RL-1: a certified uranium reference ore

International Nuclear Information System (INIS)

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

1985-06-01

A 145-kg sample of a uranium ore from Rabbit Lake, Saskatchewan, has been prepared as a compositional reference material. RL-1 was ground to minus 74 μm and mixed in one lot. Approximately one half of this ore was bottled in 100-g units, the remainder being stored in bulk. The homogeneity of RL-1 with respect to uranium and nickel was confirmed by neutron activation and X-ray fluorescence analytical techniques. In a 'free choice' analytical program, 13 laboratories contributed results for one or more of uranium, nickel and arsenic in one bottle of RL-1. Based on a statistical analysis of the data, the following recommended values were assigned: U, 0.201%; Ni, 185 μg/g; and As, 19.6 μg/g

Development of a reference material for routine performance monitoring of methods measuring polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and dioxin-like polychlorinated biphenyls.

Science.gov (United States)

Selliah, S S; Cussion, S; MacPherson, K A; Reiner, E J; Toner, D

2001-06-01

Matrix-matched environmental certified reference materials (CRMs) are one of the most useful tools to validate analytical methods, assess analytical laboratory performance and to assist in the resolution of data conflicts between laboratories. This paper describes the development of a lake sediment as a CRM for polychorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (DLPCBs). The presence of DLPCBs in the environment is of increased concern and analytical methods are being developed internationally for monitoring DLPCBs in the environment. This paper also reports the results of an international interlaboratory study involving thirty-five laboratories from seventeen countries, conducted to characterize and validate levels of a sediment reference material for PCDDs, PCDFs and DLPCBs.

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).

Analysis of SMELS and reference materials for validation of the k0-based internal monostandard NAA method using in-situ detection efficiency

Science.gov (United States)

Acharya, R.; Swain, K. K.; Reddy, A. V. R.

2010-10-01

Three synthetic multielement standards (SMELS I, II and III) and two reference materials (RMs), SL-3 and Soil-7 of IAEA were analyzed for validation of the k0-based internal monostandard neutron activation analysis (IM-NAA) method utilizing in-situ relative detection efficiency. The internal monostandards used in SMELS and RMs were Au and Sc, respectively. The samples were irradiated in Apsara and Dhruva reactors, BARC and radioactive assay was carried out using a 40% relative efficiency HPGe detector coupled to an 8 k MCA. Concentrations of 23 elements were determined in both SMELS and RMs. In the case of RMs, concentrations of a few elements, whose certified values are not available, could also be determined. The % deviations for the elements determined in SMELS with respect to the assigned values and RMs with respect to certified values were within ±8%. The Z-score values at 95% confidence level for most of the elements in both the materials were within ±1.

Re-evaluation and extension of the scope of elements in US Geological Survey Standard Reference Water Samples

Science.gov (United States)

Peart, D.B.; Antweiler, Ronald C.; Taylor, Howard E.; Roth, D.A.; Brinton, T.I.

1998-01-01

More than 100 US Geological Survey (USGS) Standard Reference Water Samples (SRWSs) were analyzed for numerous trace constituents, including Al, As, B, Ba, Be, Bi, Br, Cd, Cr, Co, Cu, I, Fe, Pb, Li, Mn, Mo, Ni, Rb, Sb, Se, Sr, Te, Tl, U, V, Zn and major elements (Ca, Mg, Na, SiO2, SO4, Cl) by inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry. In addition, 15 USGS SRWSs and National Institute of Standards and Technology (NIST) standard reference material (SRM) 1641b were analyzed for mercury using cold vapor atomic fluorescence spectrometry. Also USGS SRWS Hg-7 was analyzed using isotope dilution-inductively coupled plasma mass spectrometry. The results were compared with the reported certified values of the following standard reference materials: NIST SRM 1643a, 1643b, 1643c and 1643d and National Research Council of Canada Riverine Water Reference Materials for Trace Metals SLRS-1, SLRS-2 and SLRS-3. New concentration values for trace and major elements in the SRWSs, traceable to the certified standards, are reported. Additional concentration values are reported for elements that were neither previously published for the SRWSs nor traceable to the certified reference materials. Robust statistical procedures were used that were insensitive to outliers. These data can be used for quality assurance/quality control purposes in analytical laboratories.

Application of direct solid sample analysis for the determination of chlorine in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Santos de Gois, Jefferson; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Welz, Bernhard [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil)

2015-03-01

This work describes a methodology developed to carry out Cl determination in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis. The solid samples were directly weighed into graphite ‘cups’ and inserted into the graphite furnace. The RF power and the carrier gas flow rate were optimized at 1300 W and 0.7 L min{sup −1}, respectively. Calibration could be carried out using aqueous standard solutions with pre-dried modifiers (Pd + Nd or Pd + Ca) or using solid certified reference materials with the same pre-dried modifiers or without the use of modifiers. The limit of quantification was determined as 5 μg g{sup −1} under optimized conditions and the Cl concentration was determined in five certified reference materials with certified concentrations for Cl, in addition to three certified reference materials, for which certified values for Cl were unavailable; in the latter case, the results were compared with those obtained using high-resolution continuum source molecular absorption spectrometry. Good agreement at a 95% statistical confidence level was achieved between determined and certified or reference values. - Highlights: • Direct determination of chlorine in solid biological materials is described for the first time using ICP-MS. • Calibration against aqueous standards is feasible. • The method is accurate and sensitive, regardless of the composition of the solid sample.

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

International Nuclear Information System (INIS)

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

1983-05-01

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

Measurement of the fluorine content of three NBS standard reference materials by use of the /sup 19/F(p, p'. gamma. )/sup 19/F reaction

Energy Technology Data Exchange (ETDEWEB)

Hanson, A L; Kraner, H W; Shroy, R E; Jones, K W [Brookhaven National Lab., Upton, NY (USA)

1984-08-01

The fluorine contents of National Bureau of Standards (NBS) Standard Reference Materials (SRM) 91, opal glass; 120b, phosphate rock; and 2671a, freeze-dried urine; have been measured using the /sup 19/F(p,p'..gamma..)/sup 19/F reaction at a proton energy of 3.1 MeV. The results are in good agreement with the values certified by the NBS.

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)

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

International Nuclear Information System (INIS)

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

1979-01-01

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

Critical assessment of the performance of electronic moisture analyzers for small amounts of environmental samples and biological reference materials.

Science.gov (United States)

Krachler, M

2001-12-01

Two electronic moisture analyzers were critically evaluated with regard to their suitability for determining moisture in small amounts (environmental matrices such as leaves, needles, soil, peat, sediments, and sewage sludge, as well as various biological reference materials. To this end, several homogeneous bulk materials were prepared which were subsequently employed for the development and optimization of all analytical procedures. The key features of the moisture analyzers included a halogen or ceramic heater and an integrated balance with a resolution of 0.1 mg, which is an essential prerequisite for obtaining precise results. Oven drying of the bulk materials in a conventional oven at 105 degrees C until constant mass served as reference method. A heating temperature of 65degrees C was found to provide accurate and precise results for almost all matrices investigated. To further improve the accuracy and precision, other critical parameters such as handling of sample pans, standby temperature, and measurement delay were optimized. Because of its ponderous heating behavior, the performance of the ceramic radiator was inferior to that of the halogen heater, which produced moisture results comparable to those obtained by oven drying. The developed drying procedures were successfully applied to the fast moisture analysis (1.4-6.3 min) of certified biological reference materials of similar provenance to the investigated the bulk materials. Moisture results for 200 mg aliquots ranged from 1.4 to 7.8% and good agreement was obtained between the recommended drying procedure for the reference materials and the electronic moisture analyzers with absolute uncertainties amounting to 0.1% and 0.2-0.3%, respectively.

Preparation of plant-specific NDA reference material

International Nuclear Information System (INIS)

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

1983-01-01

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

Determination of platinum, palladium, iridium and gold on selected geological reference materials by radiochemical neutron activation analysis: comparison of procedures based on aqua regia leaching and sodium peroxide sintering

International Nuclear Information System (INIS)

Nogueira, C.A.; Figueiredo, A.M.G.

1995-01-01

A rapid and sensitive neutron activation method for the determination of platinum, palladium, iridium and gold in rocks is described. The procedure consists of thermal neutron irradiation of about 250 mg of sample, followed by chemical treatment of the rock, precipitation of gold and the platinum group elements with tellurium and high-resolution gamma-ray spectrometry with a hyper-pure Ge detector. Two different methods were used for the chemical treatment of the rock: aqua regia leaching and sintering with sodium peroxide. The procedures were evaluated by analysis of the certified reference material SARM-7 and the reference material CHR-Pt+. (author)

Determination of platinum, palladium, iridium and gold on selected geological reference materials by radiochemical neutron activation analysis: comparison of procedures based on aqua regia leaching and sodium peroxide sintering

Energy Technology Data Exchange (ETDEWEB)

Nogueira, C.A.; Figueiredo, A.M.G. [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

1995-05-01

A rapid and sensitive neutron activation method for the determination of platinum, palladium, iridium and gold in rocks is described. The procedure consists of thermal neutron irradiation of about 250 mg of sample, followed by chemical treatment of the rock, precipitation of gold and the platinum group elements with tellurium and high-resolution gamma-ray spectrometry with a hyper-pure Ge detector. Two different methods were used for the chemical treatment of the rock: aqua regia leaching and sintering with sodium peroxide. The procedures were evaluated by analysis of the certified reference material SARM-7 and the reference material CHR-Pt+. (author).

NBS activities in biological reference materials

Energy Technology Data Exchange (ETDEWEB)

Rasberry, S.D.

1988-12-01

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

Reference material systems: a sourcebook for material assessment

Energy Technology Data Exchange (ETDEWEB)

Bhagat, N. (ed.)

1976-12-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

15 CFR 230.3 - New Standard Reference Materials.

Science.gov (United States)

2010-01-01

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

Application of the Instrumental Neutron Activation Analysis and High Performance Liquid Chromatography (HPLC) in the rare earth elements determination in reference geological materials

International Nuclear Information System (INIS)

Figueiredo, Ana M.G.; Moraes, Noemia M.P. de; Shihomatsu, Helena M.

1997-01-01

Instrumental Neutron Activation Analysis (INAA) and High Performance Liquid Chromatography (HPLC) were applied to the determination of rare earth elements (REE) in the geological reference materials AGV-1, G-2 and GSP-1 (USGS). Results obtained by both techniques showed good agreement with certified values, giving relative errors less than 10%. The La, Ce, Nd, Sm, Eu, Tb, Yb and Lu REE elements were determined. All the REE except Dy and Y were determined by HPLC. The reference material G94, employed in the International Proficiency Test for Analytical Geochemistry Laboratories (GeoTP1) was analysed. The results obtained are a contribution to REE contents in this sample. The INAA and HPLC application to the determination of REE in this kind of matrix is also discussed. (author). 10 refs., 1 fig., 5 tabs

Determination of rare earth and uranium in reference biological materials certified by the method of neutron activation analysis; Determinacao de terras raras e de uranio em materiais biologicos de referencia certificados pelo metodo de analise por ativacao com neutrons

Energy Technology Data Exchange (ETDEWEB)

Pereira, Lais H.P.; Saiki, Mitiko, E-mail: laispaciulli@gmail.com, E-mail: mitiko@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2013-07-01

The objective of this study was to evaluate the precision and accuracy of the determinations of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and U in certified reference materials (CRMs). To solve the problem of interference from fission products of U in the determination of lanthanides were obtained correction factors for this interference for {sup 140}La, {sup 141}Ce, {sup 143}Ce, {sup 153}Sm and {sup 147}Nd. The experimental procedure of Neutron Activation Analysis consisted of irradiating aliquots of each of the CRMs with synthetic standards of elements under thermal neutron flux of the IEA-R1 nuclear reactor, followed by gamma-ray spectrometry using a high-resolution hyperpurity GE detector. The analyzes of CRMs indicate good accuracy and precision of results, demonstrating the feasibility of applying of established procedure in NAA of elements studied in organic vegetable matrices.

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

Science.gov (United States)

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

2013-12-01

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

Nonparametric decision tree: The impact of ISO 9000 on certified and non certified companies Nonparametric decision tree: The impact of ISO 9000 on certified and non certified companies Nonparametric decision tree: The impact of ISO 9000 on certified and non certified companies

Directory of Open Access Journals (Sweden)

Joaquín Texeira Quirós

2013-09-01

Full Text Available Purpose: This empirical study analyzes a questionnaire answered by a sample of ISO 9000 certified companies and a control sample of companies which have not been certified, using a multivariate predictive model. With this approach, we assess which quality practices are associated to the likelihood of the firm being certified. Design/methodology/approach: We implemented nonparametric decision trees, in order to see which variables influence more the fact that the company be certified or not, i.e., the motivations that lead companies to make sure. Findings: The results show that only four questionnaire items are sufficient to predict if a firm is certified or not. It is shown that companies in which the respondent manifests greater concern with respect to customers relations; motivations of the employees and strategic planning have higher likelihood of being certified. Research implications: the reader should note that this study is based on data from a single country and, of course, these results capture many idiosyncrasies if its economic and corporate environment. It would be of interest to understand if this type of analysis reveals some regularities across different countries. Practical implications: companies should look for a set of practices congruent with total quality management and ISO 9000 certified. Originality/value: This study contributes to the literature on the internal motivation of companies to achieve certification under the ISO 9000 standard, by performing a comparative analysis of questionnaires answered by a sample of certified companies and a control sample of companies which have not been certified. In particular, we assess how the manager’s perception on the intensity in which quality practices are deployed in their firms is associated to the likelihood of the firm being certified.Purpose: This empirical study analyzes a questionnaire answered by a sample of ISO 9000 certified companies and a control sample of companies

A simple preparation of calibration curve standards of 134Cs and 137Cs by serial dilution of a standard reference material

International Nuclear Information System (INIS)

Labrecque, J.J.; Rosales, P.A.

1990-01-01

Two sets of calibration standards for 134 Cs and 137 Cs were prepared by small serial dilution of a natural matrix standard reference material, IAEA-154 whey powder. The first set was intended to screen imported milk powders which were suspected to be contaminated with 134 Cs and 137 Cs. Their concentration ranged from 40 to 400 Bq/kg. The other set of calibration standards was prepared to measure the environmental levels of 137 Cs in commercial Venezuelan milk powders. Their concentration ranged from 3 to 10 Bq/kg of 137 Cs. The accuracy of these calibration curves was checked by IAEA-152 and A-14 milk powders. Their measured values were in good agreement with their certified values. Finally, it is shown that these preparation techniques using serial dilution of a standard reference material were simple, rapid, precise, accurate and cost-effective. (author) 5 refs.; 5 figs.; 3 tabs

Could Bad Certifiers Certify Best?

DEFF Research Database (Denmark)

Bizotto, Jacopo; Rudiger, Jesper; Vigier, Adrien

2017-01-01

We study product certification in settings where the certifier maximizes social welfare and bases his decisions on a mixture of information, some of which is voluntarily disclosed by the sellers, and some of which he acquires first hand by testing products. We show that unless the certifier is able...... to pre-commit to a testing strategy, then having better access to information may lead to worse certification quality, by crowding out information disclosed by the sellers. Policy implications are discussed....

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

International Nuclear Information System (INIS)

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

1991-01-01

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

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

International Nuclear Information System (INIS)

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

2001-01-01

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

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

International Nuclear Information System (INIS)

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

1991-01-01

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

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

International Nuclear Information System (INIS)

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

2002-01-01

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

New Carbonate Standard Reference Materials for Boron Isotope Geochemistry

Science.gov (United States)

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

2015-12-01

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

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

Science.gov (United States)

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

2013-02-01

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

AQCS 1989 - Intercomparison runs reference materials

International Nuclear Information System (INIS)

1989-01-01

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-03-01

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

Reference materials for microanalytical nuclear techniques

Energy Technology Data Exchange (ETDEWEB)

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

1994-07-01

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

Multielement determination of trace metals in river water (certified reference material, JSAC 0301-1) by high efficiency nebulization ICP-MS after 100-fold preconcentration with a chelating resin-packed minicolumn

International Nuclear Information System (INIS)

Zhu, Yanbei; Hattori, Ryota; Fujimori, Eiji; Umemura, Tomonari; Haraguchi, Hiroki

2005-01-01

The determination of 34 trace metals in a river water certified reference material (CRM), i.e. JSAC 0301-1, which was issued by the Japan Society for Analytical Chemistry in January 2004, was performed by ICP-MS with a high efficiency nebulizer after preconcentration with a laboratory-made chelating resin-packed minicolumn, with which trace metals were concentrated 100-fold from 50 mL of a river water sample to 0.5 mL of the final analysis solution. Trace metals in JSAC 0301-1 were observed in the concentration range from 19 μg L -1 of Al to 0.000053 μg L -1 of Bi. It was found that most of the concentrations of trace metals, including rare earth elements (REEs), in JSAC 0301-1 were lower than those in JAC 0031, which was also a previously issued CRM prepared with water from the same river as that of JSAC 0301-1. The low concentrations of trace metals in JSAC 0301-1 might be attributed to the fact that there was heavy rain before collecting the original water sample to prepare the present CRM. Furthermore, the REE distribution patterns of JSAC 0301-1, JAC 0031 and the average values of river water samples in Japan were parallel to each other. These results indicate that the distributions of REEs in JSAC 0301-1 and JAC 0031 were the typical ones of river water samples in Japan. (author)

Reactor neutron activation analysis on reference materials from intercomparison runs

International Nuclear Information System (INIS)

Pantelica, A.; Salagean, M.

2003-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Oliveira Junior, Olivio Pereira de

2006-07-01

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

AQCS 1990. Intercomparison runs, reference materials

International Nuclear Information System (INIS)

1990-01-01

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

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)

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

1994-01-01

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

Multivariate approaches for stability control of the olive oil reference materials for sensory analysis - part II: applications.

Science.gov (United States)

Valverde-Som, Lucia; Ruiz-Samblás, Cristina; Rodríguez-García, Francisco P; Cuadros-Rodríguez, Luis

2018-02-09

The organoleptic quality of virgin olive oil depends on positive and negative sensory attributes. These attributes are related to volatile organic compounds and phenolic compounds that represent the aroma and taste (flavour) of the virgin olive oil. The flavour is the characteristic that can be measured by a taster panel. However, as for any analytical measuring device, the tasters, individually, and the panel, as a whole, should be harmonized and validated and proper olive oil standards are needed. In the present study, multivariate approaches are put into practice in addition to the rules to build a multivariate control chart from chromatographic volatile fingerprinting and chemometrics. Fingerprinting techniques provide analytical information without identify and quantify the analytes. This methodology is used to monitor the stability of sensory reference materials. The similarity indices have been calculated to build multivariate control chart with two olive oils certified reference materials that have been used as examples to monitor their stabilities. This methodology with chromatographic data could be applied in parallel with the 'panel test' sensory method to reduce the work of sensory analysis. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Application of a modified BCR sequential extraction (three-step) procedure for the determination of extractable trace metal contents in a sewage sludge amended soil reference material (CRM 483), complemented by a three-year stability study of acetic acid and EDTA extractable metal content.

Science.gov (United States)

Rauret, G; López-Sánchez, J F; Sahuquillo, A; Barahona, E; Lachica, M; Ure, A M; Davidson, C M; Gomez, A; Lück, D; Bacon, J; Yli-Halla, M; Muntau, H; Quevauviller, P

2000-06-01

This paper provides additional data on a sewage sludge amended soil certified reference material, CRM 483, which was certified in 1997 for its EDTA and acetic acid extractable contents of some trace metals, following standardised extraction procedures. The additional work aimed to test the long-term stability of the material and the applicability of an improved version of the BCR three-step sequential extraction procedure on the sewage sludge amended soil (CRM 483). The paper demonstrates the CRM 483 long-term stability for EDTA and acetic acid extractable contents of Cd, Cr, Cu, Ni, Pb and Zn and gives the results (obtained in the framework of an interlaboratory study) for the extractable contents of the same elements in the CRM 483, following the BCR three-step sequential extraction scheme. The aqua regia extractable contents following the ISO 11466 Standard are also given. The data are given as indicative (not certified) values.

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...

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

International Nuclear Information System (INIS)

1999-01-01

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

The uncertainty of reference standards--a guide to understanding factors impacting uncertainty, uncertainty calculations, and vendor certifications.

Science.gov (United States)

Gates, Kevin; Chang, Ning; Dilek, Isil; Jian, Huahua; Pogue, Sherri; Sreenivasan, Uma

2009-10-01

Certified solution standards are widely used in forensic toxicological, clinical/diagnostic, and environmental testing. Typically, these standards are purchased as ampouled solutions with a certified concentration. Vendors present concentration and uncertainty differently on their Certificates of Analysis. Understanding the factors that impact uncertainty and which factors have been considered in the vendor's assignment of uncertainty are critical to understanding the accuracy of the standard and the impact on testing results. Understanding these variables is also important for laboratories seeking to comply with ISO/IEC 17025 requirements and for those preparing reference solutions from neat materials at the bench. The impact of uncertainty associated with the neat material purity (including residual water, residual solvent, and inorganic content), mass measurement (weighing techniques), and solvent addition (solution density) on the overall uncertainty of the certified concentration is described along with uncertainty calculations.

Generation and Characterization of Six Recombinant Botulinum Neurotoxins as Reference Material to Serve in an International Proficiency Test

Directory of Open Access Journals (Sweden)

Jasmin Weisemann

2015-11-01

Full Text Available The detection and identification of botulinum neurotoxins (BoNT is complex due to the existence of seven serotypes, derived mosaic toxins and more than 40 subtypes. Expert laboratories currently use different technical approaches to detect, identify and quantify BoNT, but due to the lack of (certified reference materials, analytical results can hardly be compared. In this study, the six BoNT/A1–F1 prototypes were successfully produced by recombinant techniques, facilitating handling, as well as improving purity, yield, reproducibility and biosafety. All six BoNTs were quantitatively nicked into active di-chain toxins linked by a disulfide bridge. The materials were thoroughly characterized with respect to purity, identity, protein concentration, catalytic and biological activities. For BoNT/A1, B1 and E1, serotypes pathogenic to humans, the catalytic activity and the precise protein concentration were determined by Endopep-mass spectrometry and validated amino acid analysis, respectively. In addition, BoNT/A1, B1, E1 and F1 were successfully detected by immunological assays, unambiguously identified by mass spectrometric-based methods, and their specific activities were assigned by the mouse LD50 bioassay. The potencies of all six BoNT/A1–F1 were quantified by the ex vivo mouse phrenic nerve hemidiaphragm assay, allowing a direct comparison. In conclusion, highly pure recombinant BoNT reference materials were produced, thoroughly characterized and employed as spiking material in a worldwide BoNT proficiency test organized by the EQuATox consortium.

An investigation of safety climate in OHSAS 18001-certified and non-certified organizations.

Science.gov (United States)

Ghahramani, Abolfazl

2016-09-01

Many organizations worldwide have implemented Occupational Health and Safety Assessment Series (OHSAS) 18001 in their premises because of the assumed positive effects of this standard on safety. Few studies have analyzed the effect of the safety climate in OHSAS 18001-certified organizations. This case-control study used a new safety climate questionnaire to evaluate three OHSAS 18001-certified and three non-certified manufacturing companies in Iran. Hierarchical regression indicated that the safety climate was influenced by OHSAS implementation and by safety training. Employees who received safety training had better perceptions of the safety climate and its dimensions than other respondents within the certified companies. This study found that the implementation of OHSAS 18001 does not guarantee improvement of the safety climate. This study also emphasizes the need for high-quality safety training for employees of the certified companies to improve the safety climate.

Use of gamma spectrometry for analysis of three reference materials

International Nuclear Information System (INIS)

Kinova, L.

2004-01-01

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

Causes of fatal accidents for instrument-certified and non-certified private pilots.

Science.gov (United States)

Shao, Bob Siyuan; Guindani, Michele; Boyd, Douglas D

2014-11-01

Instrument certification (IFR) enhances a pilot's skills in precisely controlling the aircraft and requires a higher level of standards in maintaining heading and altitude compared with the less stringent private pilot certificate. However, there have been no prior studies to compare fatal accident causes for airmen with, and without, this rating, The NTSB accident database was queried for general aviation fatal accidents for private pilots with, and without IFR certification. Exact Poisson tests were used to calculate whether two rate parameters were equal (ratio of 1), normalized to the number of IFR-rated pilots and flight hours in the given time period. Proportion tests were used to determine whether there were significant differences in fatal accident causes between IFR-certified and non-certified pilots. A logistic regression for log-odds success was used in determining the trend and effect of age on fatal accident rates. IFR certification was associated with a reduced risk of accidents due to failure to maintain obstacle/terrain clearance and spatial disorientation for day and night operations respectively. In contrast, the likelihood of fatal accident due to equipment malfunction during day operations was higher for IFR-certified pilots. The fatal accident rate decreased over the last decade for IFR-certified but not for non-IFR-certified private pilots. However, the overall accident rate for IFR-certified private pilots was more than double that of the cohort lacking this certification. Finally, we found a trend for an increased fatality rate with advancing age for both group of pilots. Our findings informs on where training and/or technology should be focused. Both training for aerodynamic stalls, which causes over a quarter of all fatal accidents, should be intensified for both IFR-certified and non-certified private pilots. Similarly, adherence to minimum safe altitudes for both groups of pilots should be encouraged toward reducing the fatal accidents

An outline of reference materials for analysis techniques in China

International Nuclear Information System (INIS)

Zhang Yuanxun; Qian Yine; Zhang Yongping; Tong Yongpeng

1994-01-01

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

An outline of reference materials for analysis techniques in China

Energy Technology Data Exchange (ETDEWEB)

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

1994-07-01

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

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

Science.gov (United States)

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

2000-10-01

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

The standardisation of trace elements in international biological standard reference materials with neutron activation analysis and atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Pieterse, H.

1981-12-01

An investigation was undertaken into the analytical procedures and the identification of problem areas, for the certification of a new biological standard reference material supplied by the International Atomic Energy Agency, namely, a human hair sample designated as HH-I. The analyses comprised the determination of the elements As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Sb, Se, and Zn in the hair sample by using two analytical techniques, namely, Instrumental Neutron Activation Analysis and Atomic Absorption. Three other certified biological reference materials, namely, Orchard Leaves (ORCH-L), Sea Plant Material (SPM-I) and Copepod (MAA-I) were used as control standards. Determinations were made of the moisture content of the samples, using varying conditions of drying, and the necessary corrections were applied to all analytical results so that the final elemental values related to dry weight of samples. Attention was also given to the possible loss of specific elements during ashing of the samples prior to the actual instrumental analysis. The results obtained for the hair sample by the two techniques were in good agreement for the elements Co, Fe, Mn, and Zn, but did not agree for the elements Cr and Sb. As, Hg and Se could only be determined with Instrumental Neutron Activation Analysis, and Cd, Cu and Ni only with Atomic Absorption. Most of the results obtained for the three control standard reference materials were within the ranges specified for the individual elements in each sample. The analytical procedures used for determining Cd, Cr, Cu, Ni and Sb with Instrumental Neutron Activation Analysis and As, Cr, Sb and Se with Atomic Absorption, need further investigation. The measurement of the moisture content and the ashing of samples also require further investigation with a view to improving accuracy

Reference materials for micro-analytical nuclear techniques

International Nuclear Information System (INIS)

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

1994-01-01

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

Biological and environmental reference materials in CENAM.

Science.gov (United States)

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

2001-06-01

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

REFERENCE MATERIALS IN THE SPHERE OF USE OF ATOMIC ENERGY

Directory of Open Access Journals (Sweden)

V. A. Borisov

2015-01-01

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

Use of CRM's as mutual calibrating materials and control of synthetic multielement standards as used in INAA

International Nuclear Information System (INIS)

Rossbach, M.; Stoeppler, M.

1987-01-01

Dilution effects of different multielement synthetic standard solutions were studied by measuring 10-12 different concentrations of the same solution. Peak area comparison of four Certified Reference Materials (CRMs) using one value for the evaluation of the other three repetitively led to the intercomparison (degree of compatibility) of the certified values. The idea of the preparation of each laboratory's 'secondary reference standard' by comparison of synthetic multielement standards with as many CRMs as practically feasible is advocated to improve the reliability of analytical results. (author)

Mox pellet reference material

International Nuclear Information System (INIS)

Perolat, J.P.

1991-01-01

A first batch of MOX pellets certified in plutonium and uranium has been prepared and characterised in France to meet the needs of laboratories which are engaged upon destructive analysis for safeguards purposes especially in fuel fabrication plants. The pellets sintering has been obtained in a special fabrication to achieve an homogeneity better than 0.1%. The plutonium and uranium characterisation by chemical analysis has been carried out by two laboratories using at least two different methods. 1 fig., 5 refs

Artificial radioactivity in the environmental samples as IAEA reference materials

International Nuclear Information System (INIS)

Salagean, M.; Pantelica, A.

1998-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-01

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

Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

International Nuclear Information System (INIS)

Matusiewicz, Henryk; Golik, Bartosz

2004-01-01

A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles 3 (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 μg/g and 1-420 μg/g, respectively. The method could be useful as a routine procedure

Preparation of in-house graphite reference material for boron

International Nuclear Information System (INIS)

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

2016-05-01

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

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)

Rossbach, M.; Kniewald, G.

2002-01-01

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)

Difficulties of Alternatively Certified Teachers

Science.gov (United States)

Schonfeld, Irvin Sam; Feinman, Samantha J.

2012-01-01

This daily diary study followed, over a 2-week period, 252 beginning New York City public school teachers. Seventy percent were alternatively certified (New York City Teaching Fellows) and the rest, traditionally certified teachers. Alternatively certified teachers were more likely to experience stressors such as violent incidents and classroom…

Quality of determinations obtained from laboratory reference samples used in the calibration of X-ray electron probe microanalysis of silicate minerals

International Nuclear Information System (INIS)

Pavlova, Ludmila A.; Suvorova, Ludmila F.; Belozerova, Olga Yu.; Pavlov, Sergey M.

2003-01-01

Nine simple minerals and oxides, traditionally used as laboratory reference samples in the electron probe microanalysis (EPMA) of silicate minerals, have been quantitatively evaluated. Three separate series of data, comprising the average concentration, standard deviation, relative standard deviation, confidence interval and the z-score of data quality, were calculated for 21 control samples derived from calibrations obtained from three sets of reference samples: (1) simple minerals; (2) oxides; and (3) certified glass reference materials. No systematic difference was observed between the concentrations obtained from these three calibration sets when analyzed results were compared to certified compositions. The relative standard deviations obtained for each element were smaller than target values for all determinations. The z-score values for all elements determined fell within acceptable limits (-2< z<2) for concentrations ranging from 0.1 to 100%. These experiments show that the quality of data obtained from laboratory reference calibration samples is not inferior to that from certified reference glasses. The quality of results obtained corresponds to the 'applied geochemistry' type of analysis (category 2) as defined in the GeoPT proficiency testing program. Therefore, the laboratory reference samples can be used for calibrating EPMA techniques in the analysis of silicate minerals and for controlling the quality of results

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

International Nuclear Information System (INIS)

2010-01-01

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

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)

Delgado, Alejandra; Prieto, Ailette; Zuloaga, Olatz; Diego, Alberto de; Madariaga, Juan Manuel

2007-01-01

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 (NaBEt 4 ) or phenylated (NaBPh 4 ) 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 (Hg 2+ ) or silica-gel spiked with both compounds. The methylation rates found (defined as the percentage of Hg 2+ 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 Hg 2+ 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 Hg 2+ species, HgCl 4 2- , was adsorbed on the resin, whereas MeHg + , mainly as MeHgCl, remained in solution. Following the second option, a new method to analyse MeHg + in

Certified randomness in quantum physics.

Science.gov (United States)

Acín, Antonio; Masanes, Lluis

2016-12-07

The concept of randomness plays an important part in many disciplines. On the one hand, the question of whether random processes exist is fundamental for our understanding of nature. On the other, randomness is a resource for cryptography, algorithms and simulations. Standard methods for generating randomness rely on assumptions about the devices that are often not valid in practice. However, quantum technologies enable new methods for generating certified randomness, based on the violation of Bell inequalities. These methods are referred to as device-independent because they do not rely on any modelling of the devices. Here we review efforts to design device-independent randomness generators and the associated challenges.

Neutron activation analysis of biological material

International Nuclear Information System (INIS)

Kucera, J.; Simkova, M.; Obrusnik, I.

1985-01-01

The possibilities are briefly summed up of usino. NAA (neutron activation analysis) for determining element traces in foodstuffs and their intake by organisms, for monitoring changes in the content of important trace elements in tissues and body fluids owing to environmental pollution, for verifying the results of other analytical techniques and for certifying the content of element traces in reference materials. Examples are given of the use of NAA, and the results are summed up of the determination of Cd, Mn and Zn in biological reference materials NBS SRM-1577, Bovine Liver, Bowen's Kale, IAEA Milk Powder A-11 and IAEA Animal Muscle H-4. (E.S.)

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.

BCR: a service to quality assurance in analytical chemistry - some experiences and achievements with regard to reference material preparation

Energy Technology Data Exchange (ETDEWEB)

Griepink, B. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium)); Quevauviller, P. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium)); Maier, E.A. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium)); Vandendriessche, S. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium))

Despite all efforts to improve the quality of results of measurements, intercomparisons demonstrate a considerable discrepancy. This fact was also shown by many of the round robins organised by the BCR (Commission of the European Communities) on inorganic, speciation, and organic determinations in various environmental matrices. It is clear that further efforts have to be made to improve the state of the art of a wide variety of analyses. This means that the demand for certified reference materials (CRMs) is and will be in constant increase. RMs are required for the validation of methods, for proficiency testing or for training purposes. The production of RMs and CRMs resembling the composition of real matrices poses difficult problems for some compounds and is a challenge for the producers. This paper presents some recent experiences and achievements of the BCR in special cases. (orig.)

Reference materials and their role in quality assurance in environmental monitoring

International Nuclear Information System (INIS)

Cortes, Eduardo

2002-01-01

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

Determination of mercury and selenium in biological materials by neutron activation analysis method

International Nuclear Information System (INIS)

Catharino, Marilia G.M.; Vasconcellos, Marina B.A.; Moreira, Edson G.; Cipriano, Roseli; Saiki, Mitiko

2000-01-01

Mercury presents a great number of applications, however, many mercury compounds are highly toxic and may cause diseases or even death. Other element of interest is selenium, as some studies have shown that it may reduce the toxic effects of mercury and other toxic elements, due to its ability to bind to these elements. In this work the mercury concentration in the 'Spiked Human Hair' IAEA-085 and 'Unspiked Human Hair' IAEA-086 certified reference materials, in hair samples of children under dental treatment and in hair samples of an Amazon Region population, subject to mercurial contamination was determined. Selenium determination was done using 77m Se and 75 Se radioisotopes. The selenium concentration was determined also in the (IAEA-085, IAEA-086, 'Dogfish Liver' DOLT-1 and 'Dogfish Muscle' DORM-1) certified reference materials, vitamin supplement and nail clipping samples. (author)

Evaluation of a radioimmunoassay and establishment of a reference interval for salivary cortisol in healthy subjects in Denmark

DEFF Research Database (Denmark)

Hansen, Åse Marie; Garde, A H; Christensen, J M

2003-01-01

A commercial radioimmunoassay (RA) for salivary cortisol was evaluated using certified reference material in water and spiked to pooled saliva in the range 2.1-89.1 nmol/L. A variance component model for describing the effects of age, body mass index (BMI), diurnal variation, gender, days of sick...

A Comparison of Retention Rates of Alternatively Certified and Traditional Certified Teachers.

Science.gov (United States)

Dial, Micah

1992-01-01

A survey of 2,500 teachers entering a large urban school district over the last 7 years showed that alternatively certified teachers were as likely as traditional, university-certified teachers to remain in the profession and pay back the school district's initial investment in teacher training. Many become committed to teaching as a meaningful…

The Relationship Between Teachers' Self-efficacy Perception of Application-Based Educational Technology and Material Development Skills and Their Students' Level Certifying Exam Scores

Directory of Open Access Journals (Sweden)

İlhan Varank

2013-12-01

Full Text Available The purpose of the study is to investigate the relationship between 6th., 7th., and 8th grade Turkish, math, science and technology, social sciences and foreign language teachers' self-efficacy perception of application-based educational technology and material development skills and their students' Level Certifying Exam scores. A total of 256 Turkish, math, science and technology, social sciences and foreign language teachers and their students from 48 elementary schools located in a city and one of its close districts in Inner Aegean area participated in the study. The significance levels of the models established to explain students' Level Certifying Exam performance show differences from subject to subject and from grade to grade. Similar results were found for the significance levels of the variables used in the models

Determination of ancient ceramics reference material by neutron activation analysis

International Nuclear Information System (INIS)

Li Huhou; Sun Jingxin; Wang Yuqi; Lu Liangcai

1986-01-01

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

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 pursuant...

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 pursuant...

7 CFR 945.7 - Certified seed potatoes.

Science.gov (United States)

2010-01-01

... 7 Agriculture 8 2010-01-01 2010-01-01 false Certified seed potatoes. 945.7 Section 945.7... Agreements and Orders; Fruits, Vegetables, Nuts), DEPARTMENT OF AGRICULTURE IRISH POTATOES GROWN IN CERTAIN... Certified seed potatoes. Certified seed potatoes means and includes all potatoes officially certified and...

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

International Nuclear Information System (INIS)

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

1974-12-01

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

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

Science.gov (United States)

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

2018-01-01

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

Use of CRM's as mutual calibrating materials and control of synthetic multielement standards as used in INAA

International Nuclear Information System (INIS)

Rossbach, M.; Stoeppler, M.

1986-01-01

The comparability of analytical results from different laboratories requires accurately known concentrations in the applied standards. Dilution effects of different multielement synthetic standard solutions have been studied by measuring 10 - 12 different concentrations of the same solution. Peak area comparison of four Certified Reference Materials (CRM's) using one value for the evaluation of the other three repetitively led to the intercomparison (degree of compatibility) of the certified values. The idea of the preparation of each laboratory's ''secondary reference standard'' by comparison of synthetic multielement standards with as many CRM's as practically feasible is advocated to improve the reliability of analytical results. (author)

Simultaneous determination of macro and trace elements in biological reference materials by microwave induced plasma optical emission spectrometry with slurry sample introduction

Energy Technology Data Exchange (ETDEWEB)

Matusiewicz, Henryk E-mail: Henryk.Matusiewicz@put.poznan.pl; Golik, Bartosz

2004-05-21

A slurry sampling technique (SST) has been utilized for simultaneous multi-element analysis by microwave-induced plasma optical emission spectrometry (MIP-OES). Slurry samples from a spray chamber are fed directly into the microwave cavity-torch assembly (power 300 W) with no desolvation apparatus. The performance of SST-MIP-OES was demonstrated by the determination of macro (Na, K, Ca, Mg, P) and trace (Cd, Cu, Mn, Sr, Zn) elements in three biological certified reference materials using a V-groove, clog-free Babington-type nebulizer. Slurry concentrations up to 1% m/v (particles <20 {mu}m), prepared in 10% HNO{sub 3} (pH 1.2) containing 0.01% of Triton X-100, were used with calibration by the standard additions method. The method offers relatively good precision (R.S.D. ranged from 7 to 11%) with measured concentrations being in satisfactory agreement with certified values for NRCC TORT-1 (Lobster hepatopancreas), NRCC LUTS-1 (Lobster hepatopancreas) and IAEA-153 (Milk powder). The concentrations of Na, K, Ca, Mg, P and Cd, Cu, Mn, Sr, Zn were determined in the range 90-22 000 {mu}g/g and 1-420 {mu}g/g, respectively. The method could be useful as a routine procedure.

7 CFR 983.7 - Certified pistachios.

Science.gov (United States)

2010-01-01

... 7 Agriculture 8 2010-01-01 2010-01-01 false Certified pistachios. 983.7 Section 983.7 Agriculture... and Orders; Fruits, Vegetables, Nuts), DEPARTMENT OF AGRICULTURE PISTACHIOS GROWN IN CALIFORNIA, ARIZONA, AND NEW MEXICO Definitions § 983.7 Certified pistachios. Certified pistachios are those that meet...

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

Energy Technology Data Exchange (ETDEWEB)

Delgado, Alejandra [Kimika Analitikoa Saila, Euskal Herriko Unibertsitatea, 644 P.K., E-48080 Bilbao (Spain); Prieto, Ailette [Kimika Analitikoa Saila, Euskal Herriko Unibertsitatea, 644 P.K., E-48080 Bilbao (Spain); Zuloaga, Olatz [Kimika Analitikoa Saila, Euskal Herriko Unibertsitatea, 644 P.K., E-48080 Bilbao (Spain); Diego, Alberto de [Kimika Analitikoa Saila, Euskal Herriko Unibertsitatea, 644 P.K., E-48080 Bilbao (Spain)]. E-mail: alberto.dediego@ehu.es; Madariaga, Juan Manuel [Kimika Analitikoa Saila, Euskal Herriko Unibertsitatea, 644 P.K., E-48080 Bilbao (Spain)

2007-01-16

Production of artifact methylmercury (MeHg{sup +}) 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 (NaBEt{sub 4}) or phenylated (NaBPh{sub 4}) 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{sup +} 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{sup +} in the CRM-580 were significantly higher than the certified value. For the IAEA-405, however, the MeHg{sup +} concentration found was always statistically indistinguishable from the certified value. Experiments were also conducted with synthetic samples, such as aqueous mixtures of MeHg{sup +} and inorganic mercury (Hg{sup 2+}) or silica-gel spiked with both compounds. The methylation rates found (defined as the percentage of Hg{sup 2+} present in the sample which methylates to give artifact MeHg{sup +}) ranged from not observable (in certain synthetic aqueous mixtures) to 0.57% (analysis of CRM-580 under certain conditions). As the amount of Hg{sup 2+} 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 Hg{sup 2+} species, HgCl{sub 4} {sup 2-}, was adsorbed on the resin, whereas MeHg{sup +}, mainly as MeHgCl, remained in

Teacher quality: a comparison of National Board-certified and non-Board-certified teachers of deaf students.

Science.gov (United States)

Scheetz, Nanci A; Martin, David S

2006-01-01

THE STUDY was designed to identify specific components of teacher excellence, focusing initially on the characteristics of the small number of teachers of the deaf who are certified by the National Board for Professional Teaching Standards (NBPTS), then comparing those with the characteristics of other teachers identified as master teachers by university faculty in teacher preparation in deafness. Classroom observation, written lesson plans, teacher questionnaires on beliefs, and content analysis of interactive electronic focus groups were used to compare the two groups of teachers. Results indicated similarities between Board-certified and non-Board-certified master teachers in regard to teacher behaviors and commitment to well-founded pedagogical principles. Differences were found in classroom priorities and in the greater level of interconnectivity expressed by Board-certified teachers as the result of becoming Board certified. Recommendations are made for preparing teachers of deaf students.

Certified Schools

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,...

Preparation of reference material for the measurement of natural radioactivity

International Nuclear Information System (INIS)

Ben Tekaya, Malik

2010-01-01

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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)

Paul, R.L.; Clay Davis, W.; Lee Yu; Murphy, K.E.; Bryan, C.E.; Vetter, T.W.; Guthrie, W.F.; Leber, D.D.; Gulchekhra Shakirova; Graylin Mitchell

2014-01-01

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 × 10 14 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). 76 As 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 77 As 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)

Development of thoria certified reference materials-role of NFC

International Nuclear Information System (INIS)

Balaji Rao, Y.; Yadav, R.B.; Ramana Rao, A.V.

2007-01-01

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 ThO 2 CRMs along with their importance in analysis is also explained in the paper. (author)

Graphene-based filament material for thermal ionization

Energy Technology Data Exchange (ETDEWEB)

Hewitt, J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Shick, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Siegfried, M. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2017-09-19

The use of graphene oxide materials for thermal ionization mass spectrometry analysis of plutonium and uranium has been investigated. Filament made from graphene oxide slurries have been 3-D printed. A method for attaching these filaments to commercial thermal ionization post assemblies has been devised. Resistive heating of the graphene based filaments under high vacuum showed stable operation in excess of 4 hours. Plutonium ion production has been observed in an initial set of filaments spiked with the Pu 128 Certified Reference Material.

Immune reactivity of candidate reference materials

NARCIS (Netherlands)

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

2006-01-01

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

Evaluation of a reference material for glycated haemoglobin

NARCIS (Netherlands)

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

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

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

African Journals Online (AJOL)

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

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

International Nuclear Information System (INIS)

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

2002-01-01

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

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

International Nuclear Information System (INIS)

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

2002-01-01

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

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

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

International Nuclear Information System (INIS)

Anderson, D.L.

2013-01-01

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)

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-01-02

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

48 CFR 52.215-21 - Requirements for Certified Cost or Pricing Data and Data Other Than Certified Cost or Pricing...

Science.gov (United States)

2010-10-01

... Cost or Pricing Data and Data Other Than Certified Cost or Pricing Data-Modifications. 52.215-21... Requirements for Certified Cost or Pricing Data and Data Other Than Certified Cost or Pricing Data... Pricing Data and Data Other Than Certified Cost or Pricing Data—Modifications (OCT 2010) (a) Exceptions...

Micro-homogeneity evaluation of a bovine kidney candidate reference material

Energy Technology Data Exchange (ETDEWEB)

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

2017-07-01

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

Characterization of nanoparticles as candidate reference materials

International Nuclear Information System (INIS)

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

2013-01-01

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

Production and certification of reference materials

International Nuclear Information System (INIS)

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

1996-01-01

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

Leakage from medically-certified to self-certified workplace absence among norwegian employees

OpenAIRE

Karlsen, Geir Runar; Ytterstad, Elinor

2017-01-01

Source at https://dx.doi.org/10.1080/20021518.2017.1411119 There are two different kinds of sickness absence in Norway: self-certified absence (SCA), and medically-certified absence (MCA). In this study of 6437 Norwegian employees, we applied logistic regression models for a dichotomous SCA variable on initially 38 independent vari- ables including age and gender. Our findings showed that employees reporting long-term health issues but no record of MCA in the past 12 months (...

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

International Nuclear Information System (INIS)

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

1990-01-01

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

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

International Nuclear Information System (INIS)

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

1993-01-01

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

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

BATING A REFERENCE INSTALLATION BASED ON CONTROLLED-POTENTIAL COULOMETRY METOD IN THE FRAME OF IMPROVING THE STATE PRIMARY STANDARD GET 176 AND ITS MEASUREMENT CAPABILITIES

Directory of Open Access Journals (Sweden)

V. M. Zyskin

2016-01-01

Full Text Available The results of developing of reference installation, based on a controlled-potential coulometry, in the frame of improving the State primary standard of the units of mass (molar fraction and mass (molar concentration of a component in the liquid and solid substances and materials GET 176 are presented. The physical principles of controlled-potential coulometry, content and metrological characteristics of the developed installation are considered. Measurement results of copper, iron and lead contents in the certified reference materials of metals' solutions and CRM of brass produced by BAM, Germany, obtained using reference installation are given.

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

Energy Technology Data Exchange (ETDEWEB)

Cantillo, A.Y.

1995-11-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Cantillo, A.Y.

1995-11-01

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

Standard reference materials analysis for MINT Radiocarbon Laboratory

International Nuclear Information System (INIS)

Noraishah Othman; Kamisah Alias; Nasasni Nasrul

2004-01-01

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

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

CERN Document Server

Herington, E F G

1977-01-01

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

30 CFR 70.202 - Certified person; sampling.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Certified person; sampling. 70.202 Section 70... HEALTH MANDATORY HEALTH STANDARDS-UNDERGROUND COAL MINES Sampling Procedures § 70.202 Certified person; sampling. (a) The respirable dust sampling required by this part shall be done by a certified person. (b...

AQCS intercomparison runs, reference materials 1991

International Nuclear Information System (INIS)

1991-01-01

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

48 CFR 52.215-20 - Requirements for Certified Cost or Pricing Data and Data Other Than Certified Cost or Pricing Data.

Science.gov (United States)

2010-10-01

... Cost or Pricing Data and Data Other Than Certified Cost or Pricing Data. 52.215-20 Section 52.215-20... Certified Cost or Pricing Data and Data Other Than Certified Cost or Pricing Data. As prescribed in 15.408(l), insert the following provision: Requirements for Certified Cost or Pricing Data and Data Other Than...

30 CFR 71.202 - Certified person; sampling.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Certified person; sampling. 71.202 Section 71... Sampling Procedures § 71.202 Certified person; sampling. (a) The respirable dust sampling required by this... on sampling of respirable coal mine dust. (c) A person may be temporarily certified by MSHA to take...

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

Round robin testing of thermal conductivity reference materials

International Nuclear Information System (INIS)

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

1985-07-01

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

Strategies for building reference standards for autoantibodies

Directory of Open Access Journals (Sweden)

Joanna eSheldon

2015-04-01

Full Text Available Producing robust, certified, traceable reference material for autoantibody testing is a vital element in maintaining the validity of results that are generated in the daily clinical laboratory routine. This is a huge challenge because of the high number of variables involved in the detection and measurement of the autoantibodies. The production of such materials is time consuming and needs rigorous attention to detail; this is best achieved by an overarching independent body who will oversee the process in a not for profit manner.Much effort has been made to build international standards for quantitative and qualitative assays based on monoclonal antibodies, obtained from affinity purification and plasmapheresis. The big challenge is to respect individual differences in immune response to the same antigen. A promising ongoing initiative is the construction of pools with monospecific samples from different individuals.

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

Science.gov (United States)

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

2000-07-01

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

Experience of air transport of nuclear fuel material in Japan

International Nuclear Information System (INIS)

Yamashita, T.; Toguri, D.; Kawasaki, M.

2004-01-01

Certified Reference Materials (hereafter called as to CRMs), which are indispensable for Quality Assurance and Material Accountability in nuclear fuel plants, are being provided by overseas suppliers to Japanese nuclear entities as Type A package (non-fissile) through air transport. However, after the criticality accident at JCO in Japan, special law defining nuclear disaster countermeasures (hereafter called as to the LAW) has been newly enforced in June 2000. Thereafter, nuclear fuel materials must meet not only to the existing transport regulations but also to the LAW for its transport

Synthesis of Precision for the Certification of Phosphorus in Biological Materials by INAA

DEFF Research Database (Denmark)

Damsgaard, E.; Heydorn, K.

1987-01-01

The β-emitter32P was used to determine total phosphorus by INAA in Skim Milk Powder RM 63, a material now certified by the EEC Bureau of Reference (BCR). Samples and comparator were irradiated in the Danish reactor DR 3. One month later the samples were dissolved in water and aliquots counted...

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

International Nuclear Information System (INIS)

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

1977-05-01

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

Particle size studies in the preparation of AQCS reference materials

International Nuclear Information System (INIS)

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

1994-01-01

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

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

Science.gov (United States)

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

2014-12-03

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

Results of an international comparison for the determination of radionuclide activity in bilberry material

International Nuclear Information System (INIS)

Wätjen, U.; Altzitzoglou, T.; Ceccatelli, A.; Dikmen, H.; Emteborg, H.; Ferreux, L.; Frechou, C.; La Rosa, J.; Luca, A.; Moreno, Y.; Oropesa, P.; Pierre, S.; Schmiedel, M.

2012-01-01

Radioactivity found in wild food products has assumed greater importance when assessing the total exposure of the population. For this reason, IRMM has been developing a reference material for the activity concentration of three radionuclides in bilberry samples. In order to characterise this new material, a CCRI(II) supplementary comparison was organised. The difficulties encountered in this comparison are discussed, in particular the efficiency calibration for volume sources of gamma-ray emitters, and comparison reference values for 137 Cs and 40 K are calculated. - Highlights: ► CCRI(II) supplementary comparison for Cs-137 and K-40 in bilberry matrix completed. ► Fundamentally different methods used to establish link to SI traceable standards and SIR. ► Variation of results higher than in CCRI(II) key comparisons. ► Comparison reference values will be robust property values of IRMM reference material. ► Certified reference material for radioactivity in food developed.

The development and evaluation of reference materials for food microbiology

NARCIS (Netherlands)

Veld, in 't P.

1998-01-01

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

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

International Nuclear Information System (INIS)

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

1983-10-01

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

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.

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