Final report on CCQM-K87: Mono-elemental calibration solutions

Autor: Reinhard Jährling, Lindomar Augusto dos Reis, David Saxby, Murat Tunç, Agnieszka Zon, Alex Barzev, Gregory C. Turk, Sarah Hill, Wai-hong Fung, Judith Velina Lara-Manzano, Oktay Cankur, Paola Fisicaro, Rodrigo Caciano de Sena, Jeffrey Merrick, Yu. A. Kustikov, Liliana Valiente, Jochen Vogl, Marina Bezruchko, Mirella Buzoianu, Volker Görlitz, Michael R. Winchester, Akiharu Hioki, Yong-Hyeon Yim, Leonid Konopelko, Toshihiro Suzuki, Wu Bing, Rachel Champion, Maré Linsky, Betül Ari, Tsutomu Miura, Olaf Rienitz, Michal Máriássy, Detlef Schiel
Rok vydání: 2012
Předmět:
Zdroj: Metrologia. 49:08010-08010
ISSN: 1681-7575
0026-1394
Popis: 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 fur Materialforschung und -prufung (BAM, Berlin, Germany), the Centro Nacional de Metrologia (CENAM, Queretaro, 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. 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).
Databáze: OpenAIRE