TY - JOUR A1 - Hein, Sebastian A1 - Philipp, Rosemarie A1 - Duewer, D.L. A1 - Gasca-Aragon, H. A1 - Lippa, K. A1 - Toman, B. A1 - Bremser, Wolfram A1 - Calderon, M.A.Á. A1 - Castorena, A.P. A1 - Caixeiro, J.M.R. A1 - Do Rego, E.C.P. A1 - Rosso, A. A1 - De Arechavaleta, R. A1 - O'Connor, G. A1 - Holcombe, G. A1 - Ellison, S.L.R. A1 - Splett, J.D. A1 - Schantz, M.M. A1 - Sharpless, K.E. A1 - Croft, M. A1 - Archer, M. A1 - De Vos, J. A1 - Konopelko, L.A. A1 - Kustikov, Y. T1 - Final report on CCQM-K79: Comparison of value-assigned CRMs and PT materials: Ethanol in aqueous matrix N2 - The 2010 CCQM-K79 'Comparison of value-assigned CRMs and PT materials: Ethanol in aqueous media' is the second key comparison directly testing the chemical measurement services provided to customers by National Metrology Institutes (NMIs) and Designated Institutes (DIs). CCQM-K79 compared the assigned ethanol values of proficiency test (PT) and certified reference materials (CRMs) using measurements made on these materials under repeatability conditions. Nine NMIs submitted 27 CRM or value-assigned PT materials for evaluation. These materials represent many of the higher-order reference materials then available for this commercially and forensically important measurand. The assigned ethanol mass fraction in the materials ranged from 0.1 mg/kg to 334 mg/kg. All materials were stored and prepared according the specifications provided by each NMI. Samples were processed and analyzed under repeatability conditions by one analytical team using a gas chromatography with flame ionization detection (GC-FID) method of demonstrated trueness and precision. Given the number of materials and the time required for each analysis, the majority of the measurements were made in two measurement campaigns ('runs'). Due to a shipping delay from one NMI, an unanticipated third campaign was required. In all three campaigns, replicate analyses (three injections of one preparation separated in time) were made for one randomly selected unit of each of the 27 materials. Nine of the 27 materials were gravimetrically diluted before measurement to provide solutions with ethanol mass fraction in the established linear range of the GC-FID method. The repeatability measurement value for each analyzed solution was estimated as the mean of all replicate values. The within- and between-campaign variance components were estimated using one-way ANOVA. Markov Chain Monte Carlo Bayesian analysis was used to estimate 95% level-of-confidence coverage intervals for the mean values. Uncertainty-weighted generalized distance regression was used to establish the key comparison reference function (KCRF) relating the assigned values to the repeatability measurements. On the basis of leave-one-out cross-validation, all of the assigned values for all 27 materials were deemed equivalent at the 95% level of confidence. These materials were used to define the KCRF. Parametric bootstrap Monte Carlo was used to estimate 95% level-of-confidence coverage intervals for the degrees of equivalence of materials, d ± U95(d), and of the participating NMIs, D ± U95(D). Because of the very wide range of ethanol mass fraction in the materials, these degrees of equivalence are expressed in percent relative form: %d ± U95(%d) and %D ± U95(%D). The median of the absolute values of the %D for the participating NMIs is less than 0.05% with a median U95(%D) of less than 1%. These results demonstrate that the participating NMIs have the ability to correctly value-assign CRMs and proficiency test materials for ethanol in aqueous media and similar measurands. PY - 2013 U6 - https://doi.org/10.1088/0026-1394/50/1A/08005 SN - 0026-1394 SN - 1681-7575 VL - 50 IS - 1A / Technical Suppl. 2013 / 08005 SP - 1 EP - 49 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-27730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Flores, E. A1 - Idrees, F. A1 - Moussay, P. A1 - Viallon, J. A1 - Wielgosz, R. A1 - Fernández, T. A1 - Ramírez, S. A1 - Rojo, A. A1 - Shinji, U. A1 - Waldén, J. A1 - Sega, M. A1 - Sang-Hyub, O. A1 - Macé, T. A1 - Couret, C. A1 - Qiao, H. A1 - Smeulders, D. A1 - Guenther, F.R. A1 - Thorn, W.J. III A1 - Tshilongo, J. A1 - Ntsasa, N.G. A1 - Stovcík, V. A1 - Valková, M. A1 - Konopelko, L. A1 - Gromova, E. A1 - Nieuwenkamp, G. A1 - Wessel, R. M. A1 - Milton, M. A1 - Harling, A. A1 - Vargha, G. A1 - Tuma, Dirk A1 - Kohl, Anka A1 - Schulz, Gert T1 - Final report on international comparison CCQM-K74: Nitrogen dioxide, 10 µmol/mol N2 - There is a high international priority attached to activities which reduce NOx in the atmosphere. The current level of permitted emissions is typically between 50 µmol/mol and 100 µmol/mol, but lower values are expected in the future. Currently, ambient air quality monitoring regulations also require the measurement of NOx mole fractions as low as 0.2 µmol/mol. The production of accurate standards at these levels of mole fractions requires either dilution of a stable higher concentration gas standard or production by a dynamic technique, for example one based on permeation tubes. The CCQM-K74 key comparison was designed to evaluate the level of comparability of National Metrology Institutes' measurement capabilities and standards for nitrogen dioxide (NO2) at a nominal mole fraction of 10 µmol/mol. The measurements of this key comparison took place from June 2009 to May 2010. Seventeen laboratories took part in this comparison coordinated by the BIPM and VSL. The key comparison reference value was based on BIPM measurement results, and the standard measurement uncertainty of the reference value was 0.042 µmol/mol. This key comparison demonstrated that the results of the majority of the participants agreed within limits of ±3% relative to the reference value. The results of only one laboratory lay significantly outside these limits. Likewise this comparison made clear that a full interpretation of the results of the comparison needed to take into account the presence of nitric acid (in the range 100 nmol/mol to 350 nmol/mol) in the cylinders circulated as part of the comparison, as well as the possible presence of nitric acid in the primary standards used by participating laboratories. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA). DatesIssue 1A (Technical Supplement 2012) KW - Ringversuch KW - NO2 KW - Spurenverunreinigungen KW - Meßverfahren PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08005 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 08005 SP - 1 EP - 117 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-25927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Flores, E. A1 - Idrees, F. A1 - Moussay, P. A1 - Viallon, J. A1 - Wielgosz, R. A1 - Fernández, T. A1 - Rojo, A. A1 - Ramírez, S. A1 - Aoki, N. A1 - Kato, K. A1 - Jeongsoon, L. A1 - Moon, D. A1 - Kim, J.-S. A1 - Harling, A. A1 - Milton, M. A1 - Smeulders, D. A1 - Guenther, F.R. A1 - Gameson, L. A1 - Botha, A. A1 - Tshilongo, J. A1 - Ntsasa, N.G. A1 - Valková, M. A1 - Konopelko, L. A1 - Kustikov, Y.A. A1 - Ballandovich, V. S. A1 - Gromova, E.V. A1 - Tuma, Dirk A1 - Kohl, Anka A1 - Schulz, Gert T1 - Final report of the pilot study CCQM-P110-B1: A comparison of nitrogen dioxide (NO2) in nitrogen standards at 10 µmol/mol by Fourier transform infrared spectroscopy (FT-IR) N2 - This pilot study compares the performance of participants in analyzing gas mixtures of nitrogen dioxide in nitrogen by comparison with in-house gravimetric standards using Fourier transformed infrared spectroscopy (FT-IR). In this study the same gas mixtures were used as in the key comparison CCQM-K74, which was designed to evaluate the level of comparability of National Metrology Institutes' measurement capabilities for nitrogen dioxide (NO2) at a nominal mole fraction of 10 µmol/mol. In the comparison CCQM-K74 most of the participants used chemiluminescence, with a small number using UV absorption or FT-IR spectroscopy, and thus it is of interest to improve understanding of the comparative performance of these techniques because they do not exhibit any cross-sensitivity to nitric acid (HNO3), which was known to be present in the mixtures used for the comparison. The results of this pilot study indicate good consistency and a level of agreement similar to that reported in the comparison CCQM-K74, demonstrating that FT-IR can be operated as a comparison method when calibrated with appropriate gas standards and can achieve similar measurement uncertainties to chemiluminescence and UV absorption techniques. An additional pilot study, CCQM-P110-B2, was conducted on the same gas mixtures in parallel with this pilot study. The second study addressed FT-IR spectroscopy when used to measure the gas mixtures with respect to reference spectra. The results of this second study will be reported elsewhere. Main text. To reach the main text of this paper, click on Final Report. The final report has been peer-reviewed and approved for publication by the CCQM-GAWG. DatesIssue 1A (Technical Supplement 2012) KW - Ringversuch KW - NO2 KW - Spurenverunreinigungen KW - FT-IR-Spektroskopie PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08006 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 08006 SP - 1 EP - 76 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-25928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kato, K. A1 - Watanabe, T. A1 - Heine, Hans-Joachim A1 - Boissière, Claudia A1 - Schulz, Gert A1 - Woo, J.-C. A1 - Kim, J.S. A1 - Sang-Hyub, O. A1 - Bae, H. K. A1 - Kim, Y.D. A1 - Qiao, H. A1 - Guenther, F.R. A1 - Roderick, G. C. A1 - Miller, W. A1 - Smeulders, D. A1 - Botha, A. A1 - van Rensburg, M.J. A1 - Tshilongo, J. A1 - Leshabane, N. A1 - Ntsasa, N. A1 - Milton, M. A1 - Vargha, G. A1 - Harling, A. A1 - Konopelko, L. A1 - Kustikov, Y.A. A1 - Vasserman, I.I. A1 - Zavyalov, S. V. A1 - Popova, T.A. A1 - Pankratov, V.V. A1 - Pir, M.N. A1 - Maltsev, M.A. A1 - Oudwater, R. A1 - Persijn, S. A1 - van Wijk, J. A1 - Wessel, R. M. T1 - International comparison CCQM-K66: Impurity analysis of methane N2 - This key comparison was performed to demonstrate the capability of NMIs to analyse the purity of methane for use as a source gas in the preparation of standard gas mixtures. This capability is an essential requirement for the preparation of accurate standards of natural gas and some other fuels. Since it is difficult to carry out a comparison with individual samples of pure gas, the sample for this comparison was a synthetic mixture of high purity methane with selected added impurities of nitrogen, argon, carbon dioxide and ethane. These mixtures were prepared by a gas company as a batch of 10 cylinders and their homogeneity and stability were evaluated by NMIJ. The KCRVs for the four different analytes in this key comparison are based on a consensus of values reported by participants. The uncertainties in the degrees of equivalence were calculated by combining the reported uncertainties with the homogeneity of the samples and the uncertainty of the KCRV. The results submitted are generally consistent with the KCRV within the estimated uncertainties. Finally, this comparison demonstrates that the analysis of nitrogen, argon, carbon dioxide and ethane in methane at amount fractions of 1 µmol/mol to 5 µmol/mol is generally possible with an uncertainty of 5% to 10%. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA). DatesIssue 1A (Technical Supplement 2012) KW - Ringversuch KW - Methan KW - Spurenverunreinigungen KW - Gaschromatographie PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08001 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 08001 SP - 1 EP - 76 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-25929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nieuwenkamp, G. A1 - Wessel, R. M. A1 - van der Veen, A.M.H. A1 - Ziel, P. R. A1 - Han, Q. A1 - Tuma, Dirk A1 - Woo, J.-C. A1 - Fuko, J.T. A1 - Szilágyi, N. A1 - Büki, T. A1 - Konopelko, L. A1 - Kustikov, Y.A. A1 - Popova, T.A. A1 - Pankratov, V.V. A1 - Pir, M.N. A1 - Nazarov, E.V. A1 - Ehvalov, L.V. A1 - Timofeev, A.U. A1 - Kuzmina, T.A. A1 - Meshkov, A.V. A1 - Valková, M. A1 - Pätoprsty, V. A1 - Downey, M. A1 - Vargha, G. A1 - Brown, A. A1 - Milton, M. T1 - International comparison CCQM-K77: Refinery gas N2 - Refinery gas is a complex mixture of hydrocarbons and non-combustible gases (e.g., carbon monoxide, carbon dioxide, nitrogen, helium). It is obtained as part of the refining and conversion of crude oil. This key comparison aims to evaluate the measurement capabilities for these types of mixtures. The results of the key comparison indicate that the analysis of a refinery-type gas mixture is for some laboratories a challenge. Overall, four laboratories (VSL, NIM, NPL and VNIIM) have satisfactory results. The results of some participants highlight some non-trivial issues, such as appropriate separation between saturated and unsaturated hydrocarbons, and issues with the measurement of nitrogen, hydrogen and helium. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA). DatesIssue 1A (Technical Supplement 2012) KW - Ringversuch KW - Raffineriegas KW - Chromatographische Analyse PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08003 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 08003 SP - 1 EP - 71 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-25931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noble, J.E. A1 - Wang, L. A1 - Cerasoli, E. A1 - Knight, A.E. A1 - Porter, R.A. A1 - Gray, E. A1 - Howe, C. A1 - Hannes, E. A1 - Corbisier, P. A1 - Wang, J. A1 - Wu, L. A1 - Altieri, I. A1 - Patriarca, M. A1 - Hoffmann, Angelika A1 - Resch-Genger, Ute A1 - Ebert, B. A1 - Voigt, Jan A1 - Shigeri, Y. A1 - Vonsky, M.S. A1 - Konopelko, L.A. A1 - Gaigalas, A.K. A1 - Bailey, M. J. A. T1 - An international comparability study to determine the sources of uncertainty associated with a non-competitive sandwich fluorescent ELISA KW - ELISA KW - Fluorescence KW - Interferon KW - Uncertainty KW - Round Robin KW - Immunoassay KW - Quality assurance KW - Fluorescein PY - 2008 SN - 1434-6621 SN - 1437-8523 VL - 46 IS - 7 SP - 1033 EP - 1045 PB - De Gruyter CY - Berlin AN - OPUS4-18283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ma, L. A1 - Feng, L. A1 - Hioki, A. A1 - Cho, K.H. A1 - Vogl, Jochen A1 - Berger, Achim A1 - Turk, G. A1 - Macleod, S. A1 - Labarraque, G. A1 - Tong, W.F. A1 - Schiel, D. A1 - Yafa, C. A1 - Valiente, L. A1 - Konopelko, L.A. A1 - Quetel, C. A1 - Vermaercke, P. A1 - Manzano, J.V.L. A1 - Linsky, M. A1 - Cortés, E. A1 - Tangpitayakul, S. A1 - Plangsangmas, L. A1 - Bergamaschi, L. A1 - Hearn, R. T1 - International comparison of the determination of the mass fraction of cadmium, chromium, mercury and lead in polypropylene: the Comité Consultatif pour la quantité de matière pilot study CCQM-P106 KW - Cadmium KW - Chromium KW - Mercury KW - Lead KW - Polypropylene KW - CCQM PY - 2010 U6 - https://doi.org/10.1007/s00769-009-0574-z SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 1 SP - 39 EP - 44 PB - Springer CY - Berlin AN - OPUS4-20787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Vogl, Jochen A1 - Gusarova, Tamara A1 - Czerwensky, Michael A1 - Heinrich, Hans-Joachim A1 - Hioki, A. A1 - Konopelko, L.A. A1 - Methven, B. A1 - Miura, T. A1 - Petersen, O. A1 - Riebe, Gundel A1 - Sturgeon, R. A1 - Turk, G.C. A1 - Yu, L. L. T1 - Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability N2 - Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established. KW - Interlaboratory comparison KW - Purity analysis KW - High purity metals KW - CCQM-P107 KW - Zinc PY - 2010 U6 - https://doi.org/10.1007/s00769-009-0557-0 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 1 SP - 29 EP - 37 PB - Springer CY - Berlin AN - OPUS4-20767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hioki, A. A1 - Nonose, N. A1 - Liandi, M. A1 - Jingbo, C. A1 - Liuxing, F. A1 - Chao, W. A1 - Cho, K.H. A1 - Suh, J.K. A1 - Min, H.S. A1 - Lim, Y. A1 - Recknagel, Sebastian A1 - Koenig, Maren A1 - Vogl, Jochen A1 - De Sena, R.C. A1 - Dos Reis, L.A. A1 - Borinsky, M. A1 - Puelles, M. A1 - Hatamleh, N. A1 - Acosta, O. A1 - Turk, G. A1 - Rabb, S. A1 - Sturgeon, R. A1 - Methven, B. A1 - Rienitz, O. A1 - Jaehrling, R. A1 - Konopelko, L.A. A1 - Kustikov, Y.A. A1 - Kozyreva, S.B. A1 - Korzh, A.A. T1 - Final report of the key coamparison CCQM-K88: Determination of lead in lead-free solder containing silver and copper N2 - The CCQM-K88 key comparison was organized by the Inorganic Analysis Working Group of CCQM to test the abilities of the national metrology institutes to measure the mass fraction of lead in lead-free solder containing silver and copper. National Metrology Institute of Japan (NMIJ), National Institute of Metrology of China (NIM) and Korea Research Institute of Standards and Science (KRISS) acted as the coordinating laboratories. The participants used different measurement methods, though most of them used inductively coupled plasma optical emission spectrometry (ICP-OES) or isotope-dilution inductively coupled plasma mass spectrometry (ID-ICP-MS). Accounting for relative expanded uncertainty, comparability of measurement results was successfully demonstrated by the participating NMIs for the measurement of the mass fraction of lead in lead-free solder at the level of 200 mg/kg. It is expected that metals at mass fractions greater than approximately 100 mg/kg in lead-free solder containing silver and copper can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. KW - CCQM KW - Metrology KW - IDMS PY - 2013 U6 - https://doi.org/10.1088/0026-1394/50/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 50 IS - 08002, 1A (Technical Supplement 2013) SP - 1 EP - 19 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-30457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Wielgosz, R. A1 - Davies, S. A1 - Moad, M. A1 - Chan, B. A1 - Munoz, A. A1 - Conneely, P. A1 - Ricci, M. A1 - Do Rego, E.C.P. A1 - Garrido, B.C. A1 - Violante, F.G.M. A1 - Windust, A. A1 - Dai, X. A1 - Huang, T. A1 - Zhang, W. A1 - Su, F. A1 - Quan, C. A1 - Wang, H. A1 - Lo, M. A1 - Wong, W. A1 - Gantois, F. A1 - Lalerle, B. A1 - Dorgerloh, Ute A1 - Koch, Matthias A1 - Klyk-Seitz, Urszula-Anna A1 - Pfeifer, Dietmar A1 - Philipp, Rosemarie A1 - Piechotta, Christian A1 - Recknagel, Sebastian A1 - Rothe, Robert A1 - Yamazaki, T. A1 - Zakaria, O. B. A1 - Castro, E. A1 - Balderas, M. A1 - González, N. A1 - Salazar, C. A1 - Regalado, L. A1 - Valle, E. A1 - Rodríguez, L. A1 - Laguna, L.Á.. A1 - Ramírez, P. A1 - Avila, M. A1 - Ibarra, J. A1 - Valle, L. A1 - Arce, M. A1 - Mitani, Y. A1 - Konopelko, L. A1 - Krylov, A. A1 - Lopushanskaya, E. A1 - Lin, T.T. A1 - Liu, Q. A1 - Kooi, L.T. A1 - Fernandes-Whaley, M. A1 - Prevoo-Franzsen, D. A1 - Nhlapo, N. A1 - Visser, R. A1 - Kim, B. A1 - Lee, H. A1 - Kankaew, P. A1 - Pookrod, P. A1 - Sudsiri, N. A1 - Shearman, K. A1 - Gören, A.C. A1 - Bilsel, G. A1 - Yilmaz, H. A1 - Bilsel, M. A1 - Cergel, M. A1 - Coskun, F.G. A1 - Uysal, E. A1 - Gündüz, S. A1 - Ün, I. A1 - Warren, J. A1 - Bearden, D.W. A1 - Bedner, M. A1 - Duewer, D.L. A1 - Lang, B.E. A1 - Lippa, K.A. A1 - Schantz, M.M. A1 - Sieber, J.R. T1 - Final report on key comparison CCQM-K55.c (L-(+)-Valine): Characterization of organic substances for chemical purity N2 - KEY COMPARISON Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.c, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2012. Twenty National Measurement Institutes or Designated Institutes and the BIPM participated. Participants were required to assign the mass fraction of valine present as the main component in the comparison sample for CCQM-K55.c. The comparison samples were prepared from analytical grade L-valine purchased from a commercial supplier and used as provided without further treatment or purification. Valine was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of low structural complexity [molecular weight range 100–300] and high polarity (pKOW > –2). The KCRV for the valine content of the material was 992.0 mg/g with a combined standard uncertainty of 0.3 mg/g. The key comparison reference value (KCRV) was assigned by combination of KCRVs assigned from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 1 mg/g to 6 mg/g when using mass balance based approaches alone, 2 mg/g to 7 mg/g using quantitative 1H NMR (qNMR) based approaches and from 1 mg/g to 2.5 mg/g when a result obtained by a mass balance method was combined with a separate qNMR result. The material provided several analytical challenges. In addition to the need to identify and quantify various related amino acid impurities including leucine, isoleucine, alanine and a-amino butyrate, care was required to select appropriate conditions for performing Karl Fischer titration assay for water content to avoid bias due to in situ formation of water by self-condensation under the assay conditions. It also proved to be a challenging compound for purity assignment by qNMR techniques. There was overall excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content, residual solvent and total non-volatile content of the sample. Appropriate technical justifications were developed to rationalise observed discrepancies in the limited cases where methodology differences led to inconsistent results. The comparison demonstrated that to perform a qNMR purity assignment the selection of appropriate parameters and an understanding of their potential influence on the assigned value is critical for reliable implementation of the method, particularly when one or more of the peaks to be quantified consist of complex multiplet signals. PY - 2014 U6 - https://doi.org/10.1088/0026-1394/51/1A/08010 SN - 0026-1394 SN - 1681-7575 VL - 51 SP - 08010, 1 EP - 44 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-31072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Schiel, D. A1 - Görlitz, V. A1 - Jährling, R. A1 - Vogl, Jochen A1 - Lara-Manzano, J.V. A1 - Zon, A. A1 - Fung, W.-H. A1 - Buzoianu, M. A1 - De Sena, R.C. A1 - Dos Reis, L.A. A1 - Valiente, L. A1 - Yim, Y.-H. A1 - Hill, S. A1 - Champion, R. A1 - Fisicaro, P. A1 - Bing, W. A1 - Turk, G.C. A1 - Winchester, M. R. A1 - Saxby, D. A1 - Merrick, J. A1 - Hioki, A. A1 - Miura, T. A1 - Suzuki, T. A1 - Linsky, M. A1 - Barzev, A. A1 - Máriássy, M. A1 - Cankur, O. A1 - Ari, B. A1 - Tunc, M. A1 - Konopelko, L.A. A1 - Kustikov, Y.A. A1 - Bezruchko, M. T1 - Final report on CCQM-K87: Mono-elemental calibration solutions N2 - The aim of this comparison was to demonstrate the capability of national metrology institutes to measure elemental mass fractions at a level of w(E) ≈ 1 g/kg as found in almost all mono-elemental calibration solutions. These calibration solutions represent an important link in traceability systems in inorganic analysis. Virtually all traceable routine measurements are linked to the SI through these calibration solutions. Every participant was provided with three solutions of each of the three selected elements chromium, cobalt and lead. This comparison was a joint activity of the Inorganic Analysis Working Group (IAWG) and the Electrochemical Analysis Working Group (EAWG) of the CCQM and was piloted by the Physikalisch-Technische Bundesanstalt (PTB, Braunschweig, Germany) with the help of the Bundesanstalt für Materialforschung und -prüfung (BAM, Berlin, Germany), the Centro Nacional de Metrología (CENAM, Querétaro, Mexico) and the National Institute of Standards and Technology (NIST, Gaithersburg, USA). A small majority of participants applied inductively coupled plasma optical emission spectrometry (ICP OES) in combination with a variety of calibration strategies (one-point-calibration, bracketing, calibration curve, each with and without an internal standard). But also IDMS techniques were carried out on quadrupole, high resolution and multicollector ICP-MS machines as well as a TIMS machine. Several participants applied titrimetry. FAAS as well as ICP-MS combined with non-IDMS calibration strategies were used by at least one participant. The key comparison reference values (KCRV) were agreed upon during the IAWG/EAWG meeting in November 2011 held in Sydney as the added element content calculated from the gravimetric sample preparation. Accordingly the degrees of equivalence were calculated. Despite the large variety of methods applied no superior method could be identified. The relative deviation of the median of the participants' results from the gravimetric reference value was equal or smaller than 0.1% (with an average of 0.05%) in the case of all three elements. KW - CCQM KW - Metrology KW - IDMS PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08010 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 08010, 1A (Technical Supplement 2012) SP - 1 EP - 104 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-30458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konopelko, L.A. A1 - Kolobova, A.V. A1 - Rozhnov, M.S. A1 - Melnyk, D.M. A1 - Petryshyn, P.V. A1 - Shpilnyi, S.A. A1 - Iakubov, S.E. A1 - Bakovec, N. V. A1 - Kluchits, A.S. A1 - Kipphardt, Heinrich A1 - Aleksandrov, V. V. T1 - COOMET.QM-S5 (COOMET project № 576/RU/12) : “Supplementary comparison of national standards in the field of analysis of gas mixtures containing СО2, СО, С3Н8 in nitrogen (“automotive” gas mixtures)” N2 - The relevance of the COOMET.QM-S5 comparison is founded on tightening of requirements to a control of automobile emissions (realization of environmental standards of EURO 4, EURO-5). Participating laboratories: VNIIM, BAM, BelGIM, Ukrmetrteststandart, KazInMetr. This comparison was carried out in 2013-2014. This supplementary comparison supports CMC claims for: CO2 in the range (4–16) 10⁻² mol/mol; CO in the range (0.5–5) 10⁻² mol/mol; C3H8 in the range (0.01–0.3) 10⁻² mol/mol. Results: Component CO: All laboratories identified the values of carbon monoxide mole fraction in the gas mixture within ±0.9134%. Component CO2: All laboratories identified the values of carbon dioxide mole fraction in the gas mixture within ±0.3042%. Component C3H8: All laboratories identified the values of propane mole fraction in the gas mixture within ±0.443%. KW - COOMET.QM-S5 KW - Gas analysis PY - 2016 UR - http://kcdb.bipm.org/appendixB/KCDB_ApB_info.asp?cmp_idy=1401&cmp_cod=COOMET.QM-S5&prov=exalead SN - 1681-7575 SN - 0026-1394 VL - 53 IS - Technical Supplement SP - Article 08004, 1 EP - 33 PB - IOP publishing AN - OPUS4-40015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ricci, M. A1 - Shegunova, P. A1 - Conneely, P. A1 - Becker, Roland A1 - Torres, M. M. A1 - Osuna, M. A. A1 - On, T.P. A1 - Man, L.H. A1 - Baek, S.-Y. A1 - Kim, B. A1 - Hopley, C. A1 - Liscio, C. A1 - Warren, J. A1 - Le Diouron, V. A1 - Lardy-Fontan, S. A1 - Lalere, B. A1 - Mingwu, S. A1 - Kucklick, J. A1 - Vamathevan, V. A1 - Matsuyama, S. A1 - Numata, M. A1 - Brits, M. A1 - Quinn, L. A1 - Fernandes-Whaley, M. A1 - Gören, A.C. A1 - Binici, B. A1 - Konopelko, L. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K102: Polybrominated diphenyl ethers in sediment N2 - The key comparison CCQM-K102: Polybrominated diphenyl ethers in sediment was coordinated by the JRC, Directorate F - Health, Consumers & Reference Materials, Geel (Belgium) under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM). Thirteen National Metrology institutes or Designated Institutes and the JRC participated. Participants were requested to report the mass fraction (on a dry mass basis) of BDE 47, 99 and 153 in the freshwater sediment study material. The sediment originated from a river in Belgium and contained PBDEs (and other pollutants) at levels commonly found in environmental samples. The comparison was designed to demonstrate participants' capability of analysing non-polar organic molecules in abiotic dried matrices (approximate range of molecular weights: 100 to 800 g/mol, polarity corresponding to pKow < −2, range of mass fraction: 1–1000 μg/kg). All participants (except one using ultrasonic extraction) applied Pressurised Liquid Extraction or Soxhlet, while the instrumental analysis was performed with GC-MS/MS, GC-MS or GC-HRMS. Isotope Dilution Mass Spectrometry approach was used for quantification (except in one case). The assigned Key Comparison Reference Values (KCRVs) were the medians of thirteen results for BDE 47 and eleven results for BDE 99 and 153, respectively. BDE 47 was assigned a KCRV of 15.60 μg/kg with a combined standard uncertainty of 0.41 μg/kg, BDE 99 was assigned a KCRV of 33.69 μg/kg with a combined standard uncertainty of 0.81 μg/kg and BDE 153 was assigned a KCRV of 6.28 μg/kg with a combined standard uncertainty of 0.28 μg/kg. The k-factor for the estimation of the expanded uncertainty of the KCRVs was chosen as k = 2. KW - Intercomparison KW - Traceability KW - Nation metrology institutes PY - 2017 U6 - https://doi.org/10.1088/0026-1394/54/1A/08026 SN - 0026-1394 SN - 1681-7575 VL - 54 SP - 08026, 1 EP - 82 AN - OPUS4-41998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, Z. A1 - Han, Q. A1 - Wang, D. A1 - Macé, T. A1 - Kipphardt, Heinrich A1 - Maiwald, Michael A1 - Tuma, Dirk A1 - Uehara, S. A1 - Akima, D. A1 - Shimosaka, T. A1 - Jung, J. A1 - Oh, S.-H. A1 - van der Veen, A. A1 - van Wijk, J.I.T. A1 - Ziel, P. R. A1 - Konopelko, L. A1 - Valkova, M. A1 - Mogale, D.M. A1 - Botha, A. A1 - Brewer, P. A1 - Murugan, A. A1 - Minnaro, M.D. A1 - Miller, M. A1 - Guenther, F. A1 - Kelly, M.E. T1 - CCQM K101 Final report international comparison CCQM-K101:Oxygen in nitrogen-a track B comparison and that the matrix contains argon N2 - This key comparison aims to assess the capabilities of the participants to determine the amount-of-substance fraction oxygen in nitrogen. The GAWG has classified this as a track B comparison, due to the unexpected 50 μmol/mol argon mole fraction content of the transfer standards, which effects the achievable performance of some measurement techniques such a GC-TCD. The separation of oxygen and argon is challenging, and not all systems in use are equally well designed for it. As this analytical challenge due to a substantial fraction of argon in the transfer standards became a reality, the Gas Analysis Working Group (GAWG) decided to qualify this key comparison as a regular key comparison and not as a core comparison, which may be used to support calibration and measurement capabilities (CMCs) for oxygen in nitrogen, or for oxygen in nitrogen mixtures containing argon only (see also the section on support to CMCs). KW - CCQM-K101 KW - Gas analysis PY - 2016 UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08013 SN - 1681-7575 SN - 0026-1394 VL - 53 IS - Techn Suppl SP - 08013, 1 EP - 71 PB - IOP publishing AN - OPUS4-40013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -