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 - Vogl, Jochen A1 - Kipphardt, Heinrich A1 - del Rocío Arvizu Torres, M. A1 - Manzano, J.V.L. A1 - Rodrigues, J.M. A1 - de Sena, R.C. A1 - Yim, Y.-H. A1 - Heo, S.W. A1 - Zhou, T. A1 - Turk, G.C. A1 - Winchester, M. A1 - Yu, L. L. A1 - Miura, T. A1 - Methven, B. A1 - Sturgeon, R. A1 - Jährling, R. A1 - Rienitz, O. A1 - Tunc, M. A1 - Can, S.Z. T1 - Final report of the key comparison CCQM-K72: Purity of zinc with respect to six defined metallic analytes N2 - KEY COMPARISON High purity elements can serve as a realization of the SI unit amount of substance for the specific element. Solutions prepared from high purity metals by applying gravimetric preparation and the concept of molar mass are used as 'calibration' solutions in many fields of analytical chemistry and provide the metrological basis in elemental analysis. Since ideal purity does not exist for real materials, the actual purity of the high purity material must be known with a specified uncertainty. As required uncertainties around 10-4 relative on the purity statement are not accessible in almost all cases by a direct measurement of the element in itself, the indirect approach is followed, where all elements excepting the matrix element itself are measured and their sum is subtracted from the value for ideal purity, which is 1 kg/kg. It was the aim of this comparison to demonstrate the capability of national metrology institutes and designated institutes to determine the purity of pure elements. In order to limit the effort within this comparison, only six metallic impurities (Ag, Al, Cd, Cr, Ni, Tl) in the low mg/kg range are considered in a zinc matrix. It has to be underlined here that the task was to measure the purity of zinc based on the determination of six analytes. The task is not trace analysis of specific analytes in zinc. This subtle distinction defines different measurands. The sample, pure Zn, was cut in pieces of cubic geometry for wet chemical analysis or of pin geometry for GDMS analysis and was sent to the participants. The comparison was run under the auspices of the Inorganic analysis Working Group (IAWG) of the CCQM and was piloted by the BAM Federal Institute for Materials Research and Testing, Berlin, Germany. The majority of the participants applied ICP-MS techniques and only two participants used additionally atomic absorption spectrometry. GDMS was used only by one participant. The observed spreads for the measurement results reported by the participants were significantly lower than those of the preceding study CCQM-P107 and were well below the target uncertainty of 30% relative. As a consequence, comparability within the participating laboratories is demonstrated to be established. The individual measurement results, mean values and medians derived were in all cases very consistent with the reference values obtained by IDMS and so the accuracy of the measurement results for the participating laboratories is as well demonstrated to be established. Especially with the results of CCQM-P62 and CCQM-P107 in mind, the outcome of CCQM-K72 can be considered as a big step forward in the community. CCQM is aware of the difference between a characterization based on only six analytes and a complete characterization. Therefore, the pilot study CCQM-P149 has been initiated and already started, which focuses on the fit-for-purpose approaches for the purity determination of metals (here: zinc) to be used as primary standards in elemental analysis. Another follow-up in the form of a pilot study on non-metal impurities is mandatory, because non-metal impurities such as oxygen, nitrogen and sulfur often make up the largest contributions. 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 (CIPM MRA). KW - CCQM KW - Metrology KW - Purity PY - 2014 U6 - https://doi.org/10.1088/0026-1394/51/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 51 IS - 1A (Tech.Suppl. 2014) SP - 08008, 1 EP - 40 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-30772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H. A1 - Malinowskiy, D. A1 - Ren, T. A1 - Wang, J. A1 - Vocke Jr., R.D. A1 - Murphy, K. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. A1 - Näykki, T. A1 - Sara-Aho, T. A1 - Ari, B. A1 - Cankur, O. T1 - Final report of the key comparison CCQM-K98: Pb isotope amount ratios in bronze KW - CCQM KW - Metrology KW - Isotope amount ratios KW - Lead PY - 2014 UR - http://www.bipm.org/utils/common/pdf/final_reports/QM/K98/CCQM-K98.pdf U6 - https://doi.org/10.1088/0026-1394/51/1A/08017 SN - 0026-1394 SN - 1681-7575 VL - 51 IS - 1A Tech. Suppl. SP - 08017-1 EP - 08017-47 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-31929 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 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-496080 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sargent, M A1 - Goenaga-Infante, H A1 - Inagaki, K A1 - Ma, L A1 - Meija, J A1 - Pramann, A A1 - Rienitz, O A1 - Sturgeon, R A1 - Vogl, Jochen A1 - Wang, J A1 - Yang, L T1 - The role of ICP-MS in inorganic chemical metrology N2 - ICP-MS has played a key role in inorganic chemical metrology for 25 years, from the 1993 CIPM feasibility study which led to establishment of the CCQM. Since that time, the Inorganic Analysis Working Group of the CCQM has organised 56 international comparisons involving measurements by ICP-MS and, in a recent comparison, 16 different national institutes submitted their results using the technique. Metrological applications of ICP-MS currently address an enormous range of measurements using a wide variety of instrumentation, calibration strategies and methodologies. This review provides an overview of the ICP-MS field with an emphasis on developments which are of particular relevance to chemical metrology. Examples from CCQM comparisons and the services available from the participants are used to illustrate how the capability and scope of ICP-MS methods have expanded far beyond the expectations of 1993. This is due in part to the research and development Programmes of the national institutes which participate in the CCQM. They have played a key role in advancing new instrumentation and applications for elemental analysis, isotope dilution mass spectrometry, determination of isotopic ratio or composition, and speciation of organometallic compounds. These developments are continuing today, as demonstrated by work in new fields such as heteroatom quantitation of proteins, characterisation and counting of nanoparticles using spICP-MS, and LA-ICP-MS analysis of solid materials. KW - CCQM KW - Metrology KW - Interlaboratory comparison KW - ICP-MS KW - Mass spectrometry KW - Hyphenated KW - Isotope ratio PY - 2019 U6 - https://doi.org/10.1088/1681-7575/ab0eac VL - 56 IS - 3 SP - 034005 PB - IOP Publishing AN - OPUS4-47929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -