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  • 1
    Publication Date: 2011-06-21
    Description:    Within the scope of a project of the “European Association of National Metrology Institutes” (EURAMET), a European metrological dissemination system (network) providing traceable reference values assigned to matrix materials for validation purposes is described and put to the test. It enables testing laboratories (TL) to obtain comparable results for measurements under the “EU Water Framework Directive 2000/60/EC” (WFD) and thus, to comply with a core requirement of this very directive. The dissemination system is characterized by the fact that it is available to all laboratories throughout Europe which intend to perform measurements in the context of the WFD and that it can ensure sustainable metrological traceability to the International System of Units (SI) as a reference point for the measurement results. This dissemination system is set up in a hierarchical manner and links up the level of the national metrology institutes (NMI) with that of the TLs via an intermediate level of calibration laboratories (CL) by comparison measurements. The CLs are expert laboratories with respect to the measurement of the analytes considered here (within the project, the CLs are called potential calibration laboratories (PCL)) and are additionally involved in the organization of comparison measurements within the scope of regional quality assurance (QA) systems. Three comparison measurements have been performed to support the approach. A total of about 130 laboratories participated in this exercise with the focus on the measurement of the priority substances Pb, Cd, Hg, and Ni defined in the WFD. The elemental concentrations in the water samples roughly corresponded to one of the established environmental quality standards (EQS), the annual average concentration (AA-EQS), which is defined in the daughter Directive 2008/105/EC of the WFD. It turned out that a significant number of TLs still need to improve their measurement methods in order to be able to fulfill the minimum requirements of the WFD, in particular, with regard to the elements Cd and Hg probably due to their low EQS values. Furthermore, it became obvious that the hierarchical dissemination system suggested here actually corresponds to the measuring capabilities of the three participating groups (NMIs, PCLs, and TLs). Content Type Journal Article Pages 1-10 DOI 10.1007/s00769-011-0792-z Authors Detlef Schiel, Physikalisch-Technische Bundesanstalt (PTB), Braunschweig, Germany Olaf Rienitz, Physikalisch-Technische Bundesanstalt (PTB), Braunschweig, Germany Reinhard Jährling, Physikalisch-Technische Bundesanstalt (PTB), Braunschweig, Germany Bernd Güttler, Physikalisch-Technische Bundesanstalt (PTB), Braunschweig, Germany Ralf Matschat, BAM Bundesanstalt für Materialforschung und -prüfung, Berlin, Germany Holger Scharf, BAM Bundesanstalt für Materialforschung und -prüfung, Berlin, Germany Jürgen Birkhahn, BAM Bundesanstalt für Materialforschung und -prüfung, Berlin, Germany Guillaume Labarraque, Laboratoire National de Métrologie et d’Essais (LNE), Paris, France Paola Fisicaro, Laboratoire National de Métrologie et d’Essais (LNE), Paris, France Ulrich Borchers, IWW Water Centre, Mülheim, Germany David Schwesig, IWW Water Centre, Mülheim, Germany Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
    Print ISSN: 0949-1775
    Electronic ISSN: 1432-0517
    Topics: Chemistry and Pharmacology
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  • 2
    Publication Date: 2011-06-21
    Description: Congress, conferences, workshops and courses Content Type Journal Article Pages 1-2 DOI 10.1007/s00769-011-0794-x Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
    Print ISSN: 0949-1775
    Electronic ISSN: 1432-0517
    Topics: Chemistry and Pharmacology
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  • 3
    Publication Date: 2011-06-21
    Description:    This work describes the evaluation of several parameters for the preparation of a tuna fish candidate as a reference material (RM) in order to measure the total As mass fraction by slurry sampling graphite furnace atomic absorption spectrometry (SLS-GF AAS) and slurry sampling hydride generation atomic absorption spectrometry (SLS-HG AAS). The main parameters investigated were the homogeneity, analyte segregation and composition during material production. For candidate RM preparation, tuna fish was collected at a local market, cleaned, freeze-dried and treated using different procedures as follows: (1) ground in a cutting mill and separated in different particle sizes (2) ground in cryogenic mill. The mass fraction of As in the cryogenically ground sample was (4.77 ± 0.19) μg g −1 for SLS-GF AAS and (4.61 ± 0.34) μg g −1 for SLS-HG AAS. The accuracy of the procedures was checked with tuna fish certified reference material (BCR 627) with recoveries of 102 and 94% for SLS-GF AAS and SLS-HG AAS, respectively. The homogeneity factor was calculated for different pretreatment procedures and for particle sizes in the range of 500–150 μg, indicating good homogeneity, except for raw fish. There was no observed analyte segregation and no losses, no contamination and no changes in the microdistribution of material during preparation. Content Type Journal Article Pages 1-6 DOI 10.1007/s00769-011-0796-8 Authors V. M. O. Carioni, Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, Santo André, SP 09210-170, Brazil R. Chelegão, Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, Santo André, SP 09210-170, Brazil J. Naozuka, Departamento de Ciências Exatas e da Terra, Universidade Federal de São Paulo, Diadema, SP 09972-270, Brazil C. S. Nomura, Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, Santo André, SP 09210-170, Brazil Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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    Topics: Chemistry and Pharmacology
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  • 4
    Publication Date: 2011-06-10
    Description:    An approach to estimating measurement error variances for any instrument having round-off effects that might also have instrument bias is presented. Recently finite instrument resolution effects on error variances have been studied, but negligible instrument bias was assumed and the contexts were different than considered here. Our intent is to use repeated measurements on several standards to estimate the instrument’s random and systematic error variances. Recognizing that rounding impacts item bias and variance in a manner that depends on the true value, an approach is presented to estimate random error variance and instrument systematic error variance. The key finding is that item-specific bias can interfere with the estimation of overall instrument bias unless appropriate error modeling and associated inference steps are taken. Content Type Journal Article Pages 1-13 DOI 10.1007/s00769-011-0791-0 Authors T. Burr, Statistical Sciences, Los Alamos National Laboratory, P. O. Box 1663, MS F600, Los Alamos, NM 87545, USA M. S. Hamada, Statistical Sciences, Los Alamos National Laboratory, P. O. Box 1663, MS F600, Los Alamos, NM 87545, USA T. Cremers, Nuclear Process Infrastructure, Los Alamos National Laboratory, P.O. Box 1663, MS G735, Los Alamos, NM 87545, USA B. P. Weaver, Statistical Sciences, Los Alamos National Laboratory, P. O. Box 1663, MS F600, Los Alamos, NM 87545, USA J. Howell, Department of Mechanical Engineering, University of Glasgow, University Avenue, Glasgow, G12 8QQ Scotland, UK S. Croft, Nuclear Safeguards Science and Technology, Los Alamos National Laboratory, P.O. Box 1663, MS E540, Los Alamos, NM 87545, USA S. B. Vardeman, Departments of Statistics and Industrial and Manufacturing Systems Engineering, Iowa State University, Ames, IA 50011, USA Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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    Topics: Chemistry and Pharmacology
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  • 5
    Publication Date: 2011-06-23
    Description:    The results of and findings from an interlaboratory comparison among laboratories carrying out food testing of pesticide residues in the APEC (Asia–Pacific Economic Cooperation) region are presented and discussed to show critical roles of chemical metrology infrastructure in establishing traceability of measurements and in supporting existing measurement capability in safety and quality of food trade. The study material, which was prepared and certified by Korea Research Institute of Standards and Science (KRISS), was freeze-dried Chinese cabbage powder fortified with two organophosphorous pesticides (diazinon and chlorpyrifos). Among 14 participants, 12 laboratories were accredited based on ISO/IEC17025 and one laboratory was under assessment for the accreditation at the time of this study. Though all participants demonstrated very good intra-day repeatability and inter-day intermediate precision, many of them showed a large bias from the certified values. It is suggested that in addition to the accreditation system, economies are encouraged to develop appropriate chemical metrology infrastructure, which could effectively support laboratories to assure measurement traceability to SI, for which NMIs could play significant roles through their metrological services recognized in Mutual Recognition Arrangement (MRA) of the International Committee for Weights and Measures (Comité International des Poids et Mesures, CIPM). Content Type Journal Article Pages 1-7 DOI 10.1007/s00769-011-0795-9 Authors Byungjoo Kim, Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science, Yuseong, Daejeon, 305-340 Korea Seonghee Ahn, Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science, Yuseong, Daejeon, 305-340 Korea Yoshito Mitani, Centro Nacional de Metrologia, Municipio deEl Marques, 76246 Queretrao, Mexico Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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    Topics: Chemistry and Pharmacology
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  • 6
    Publication Date: 2011-06-11
    Description:    A marine certified reference material (CRM), IAEA-452, prepared with scallop ( Pecten maximus ) sample was recently produced by the International Atomic Energy Agency (IAEA) and certified for trace elements and methyl mercury (MeHg). The Scallop ( Pecten maximus ) sample is commonly found and consumed seafood and is also used as bio-indicators for trace metal contamination in marine pollution studies. This paper presents the sample preparation methodology, material homogeneity and stability studies, evaluation of certification campaign results, the assignment of property values and their associated uncertainty. The reference values and associated expanded uncertainty for 9 trace elements (As, Cd, Cr, Cu, Fe, Hg, Mn, Pb and Zn) and MeHg in scallop sample are established. The informative value for one more element (Ni) is also given. The new CRM can be used for the development and validation of analytical methods for determination of trace elements and methyl mercury in seafood and also for quality assurance/quality control purposes. Content Type Journal Article Pages 1-9 DOI 10.1007/s00769-011-0793-y Authors E. Vasileva, International Atomic Energy Agency, Environment Laboratories, 4 Quai Antoine 1er, Principality of Monaco, Monaco 98000, Monaco S. Azemard, International Atomic Energy Agency, Environment Laboratories, 4 Quai Antoine 1er, Principality of Monaco, Monaco 98000, Monaco J. Oh, International Atomic Energy Agency, Environment Laboratories, 4 Quai Antoine 1er, Principality of Monaco, Monaco 98000, Monaco P. Bustamante, Littoral, Environnement et Sociétés (LIENSs), UMR 6250 CNRS-Université de La Rochelle, 2 rue Olympe de Gouges, 17042 La Rochelle, France M. Betti, International Atomic Energy Agency, Environment Laboratories, 4 Quai Antoine 1er, Principality of Monaco, Monaco 98000, Monaco Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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    Topics: Chemistry and Pharmacology
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  • 7
    Publication Date: 2011-05-18
    Description:    Mycotoxins are important non-anthropogenic food and feed contaminants, which can be present on almost every agricultural commodity. Effective consumer protection therefore essentially depends on food surveillance by reliable quantitative analysis enabled by appropriate quality control. Certified (matrix) reference materials (CRMs) are versatile tools to support quality assurance. However, in the case of ochratoxin A (OTA), a hepato- and nephrotoxic mycotoxin, which is regulated in various foods, there is a lack of suitable CRMs. This lack has now been overcome by the development of two European Reference Materials (ERM ® ) for the determination of OTA in roasted coffee (ERM ® -BD475) and red wine (ERM ® -BD476). This article discusses the material preparation process as well as the results of homogeneity and stability testing. Furthermore, the results of the in-house certification studies carried out at BAM Federal Institute for Materials Research and Testing are presented and discussed. Interlaboratory comparison studies involving selected expert laboratories with documented expertise in the field of mycotoxin analysis were conducted to confirm the certified values determined by BAM. The certified ochratoxin A values and their corresponding expanded uncertainties ( k  = 2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: (6.0 ± 0.6) μg kg −1 for roasted coffee, ERM ® -BD475, and (0.52 ± 0.11) μg L −1 for red wine, ERM ® -BD476. Content Type Journal Article Pages 1-9 DOI 10.1007/s00769-011-0783-0 Authors Matthias Koch, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany Wolfram Bremser, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany Robert Köppen, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany Rita Krüger, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany Tatjana Rasenko, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany David Siegel, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany Irene Nehls, Division 1.2 “Organic Chemical Analysis; Reference Materials”, BAM Federal Institute for Materials Research and Testing, Richard-Willstätter-Str. 11, 12489 Berlin, Germany Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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    Topics: Chemistry and Pharmacology
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  • 8
    Publication Date: 2011-05-07
    Description:    A metrological approach is used for investigating multi-component out-of-specification (OOS) test results of pesticide residues concentration in tomatoes. As a case study, 169 test results were obtained in Israel in 2009. Five of the test results were OOS test results exceeding the national legal maximum residue limits ( MRL ). Only one of them was classified definitely (with more than 0.99 confidence) as caused by a farmer’s/producer’s problem. The other four OOS test results were probably metrologically related, i.e., compatible with MRL when considering the measurement uncertainty associated with the test results. A new parameter—the ratio of a test result to MRL —was proposed for analysis of tomatoes monitoring multi-residue data as a common statistical sample from the same population for different pesticide residues. Weibull distribution was found adequate for modeling the empirical distribution of the parameter values. Probability of future OOS test results was estimated, and global risks of farmer/producer and consumer/buyer were evaluated. Acceptance limits for the test results, such as “warning and action lines” in quality control charts, were calculated by taking into account the measurement uncertainties. Content Type Journal Article Pages 1-7 DOI 10.1007/s00769-011-0780-3 Authors Ilya Kuselman, The National Physical Laboratory of Israel (INPL), Givat Ram, 91904 Jerusalem, Israel Paulina Goldshlag, Laboratory for Pesticide Residue Analysis, Plant Protection and Inspection Services (PPIS), P.O.Box 78, 50250 Bet-Dagan, Israel Francesca Pennecchi, Istituto Nazionale di Ricerca Metrologica (INRIM), 73 Strada delle Cacce, 10135 Turin, Italy Cathy Burns, Food and Drug Administration (FDA), 6th Ave and Kipling St, DFC-Bldg 20, Denver, CO 80225, USA Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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  • 9
    Publication Date: 2011-04-06
    Description:    Several rapid and automated microbiological methods have been introduced by food control laboratories because they allow microbiological quality (e.g. contamination with spoilage microorganisms and/or pathogens) of products to be checked or hygiene monitoring undertaken during production. This study evaluated three applications of the TEMPO ® system; an automated method based on the most-probable-number technique, performed in parallel with the relevant ISO standard method for comparison. Escherichia coli certified reference material and soft cheese samples contaminated artificially with E. coli were used throughout the study. Performance characteristics including precision, bias and limit of detection of E. coli (EC), coliforms (TC) and viable aerobic mesophilic microflora (TVC) were determined with particular attention given to low-level contamination, which typically occur in manufacturing and retail as well as storage and consumption at home. TEMPO ® EC was more precise than TEMPO ® TC whilst TEMPO ® TVC showed the most variation. Moreover, higher numbers of E. coli were obtained with TEMPO ® EC than TEMPO ® TC. Reliability of the system depended on the specificity of detection of the targeted group of microorganisms as well on the method. Although, methods like TEMPO ® offer convenience, they often lack the necessary clarity in terms of operational details, measurement principles and data processing necessary for reliable routine use. Installation of an ‘expert modus’ to facilitate access to original data would significantly increase commercial confidence in the application and use of these systems. Content Type Journal Article Pages 1-11 DOI 10.1007/s00769-011-0772-3 Authors U. Zitz, Department of Food Sciences and Technology, Institute of Food Sciences, BOKU-University of Natural Resources and Life Sciences, Vienna, Muthgasse 18, 1190 Vienna, Austria K. J. Domig, Department of Food Sciences and Technology, Institute of Food Sciences, BOKU-University of Natural Resources and Life Sciences, Vienna, Muthgasse 18, 1190 Vienna, Austria A. Hoehl, Department of Food Sciences and Technology, Institute of Food Sciences, BOKU-University of Natural Resources and Life Sciences, Vienna, Muthgasse 18, 1190 Vienna, Austria H. Weiss, Institute of Biometry and Data Processing, Free University of Berlin, Oertzenweg 19b, 14163 Berlin, Germany P-Th. Wilrich, Institute of Statistics and Econometrics, Free University of Berlin, Garystraße 21, 14195 Berlin, Germany W. Kneifel, Department of Food Sciences and Technology, Institute of Food Sciences, BOKU-University of Natural Resources and Life Sciences, Vienna, Muthgasse 18, 1190 Vienna, Austria Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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  • 10
    Publication Date: 2011-06-06
    Description:    Different size fractions with aerodynamic diameters of (9.0–10.0) μm, (5.8–9.0) μm, (4.7–5.8) μm, (3.3–4.7) μm, (2.1–3.3) μm, (1.1–2.1) μm, (0.7–1.1) μm, and (0.4–0.7) μm of PM 10 were collected on glass fiber filter using 8-stage Andersen cascade impactor. Samples were extracted using microwave acid digestion, and analysis was performed by Direct Mercury Analyzer, DMA-80. Uncertainty resulted due to sampling and analytical procedure was calculated by applying bottom-up approach. Significant sources of uncertainty are estimated, and an uncertainty budget is prepared for each fraction. Repeatability showed maximum contribution to uncertainty budget followed by calibration curve and volume of air. Estimated expanded relative uncertainties at the 95% confidence interval for particulate-bound mercury in different size fractions were between 15 and 26%. Content Type Journal Article Pages 1-7 DOI 10.1007/s00769-011-0785-y Authors D. G. Gajghate, Air Pollution Control (APC) Division, National Environmental Engineering Research Institute (NEERI), Nehru Marg, Nagpur, 440 020 India V. V. Khaparde, Air Pollution Control (APC) Division, National Environmental Engineering Research Institute (NEERI), Nehru Marg, Nagpur, 440 020 India T. M. Pustode, Air Pollution Control (APC) Division, National Environmental Engineering Research Institute (NEERI), Nehru Marg, Nagpur, 440 020 India P. P. Pipalatkar, Air Pollution Control (APC) Division, National Environmental Engineering Research Institute (NEERI), Nehru Marg, Nagpur, 440 020 India C. V. Chalapati Rao, Air Pollution Control (APC) Division, National Environmental Engineering Research Institute (NEERI), Nehru Marg, Nagpur, 440 020 India Journal Accreditation and Quality Assurance: Journal for Quality, Comparability and Reliability in Chemical Measurement Online ISSN 1432-0517 Print ISSN 0949-1775
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    Topics: Chemistry and Pharmacology
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