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Analytical and Bioanalytical Chemistry

, Volume 407, Issue 11, pp 3093–3102 | Cite as

Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium

  • Angela Kaltenbach
  • Janine Noordmann
  • Volker Görlitz
  • Carola Pape
  • Silke Richter
  • Heinrich Kipphardt
  • Gernot Kopp
  • Reinhard Jährling
  • Olaf RienitzEmail author
  • Bernd Güttler
Research Paper
Part of the following topical collections:
  1. Reference Materials for Chemical Analysis

Abstract

Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

Keywords

Digestion Rhodium Molybdenum Reference solution Metrological traceability ICP OES MC-ICP-MS 

Notes

Acknowledgments

Financial Support by EMRP (the European Metrology Research Programme) is gratefully acknowledged (EMRP SIB09, “Primary Standards for Challenging Elements”). The EMRP is jointly funded by the EMRP participating countries within EURAMET and the European Union.

References

  1. 1.
    Güttler B, Richter W (2009) Traceability of chemical measurement results. Chimia 63:619–623CrossRefGoogle Scholar
  2. 2.
    Bureau International des Poids et Mesures (2008) International vocabulary of metrology—basic and general concepts and associated terms (VIM). JCGM 200Google Scholar
  3. 3.
    Bureau International des Poids et Mesures (2006) The international system of units (SI), 8th editionGoogle Scholar
  4. 4.
    Kipphardt H, Matschat R, Rienitz O, Schiel D, Gernand W, Oeter D (2006) Traceability system for elemental analysis. Accred Qual Assur 10:633–639CrossRefGoogle Scholar
  5. 5.
    Richter S, Sargent M, Schiel D, Kipphardt H (2013) Known purity—the fundament of element determination by atomic spectrometry. J Anal At Spectrom 28(10):1540–1543CrossRefGoogle Scholar
  6. 6.
    Rienitz O, Schiel D, Görlitz V, Jährling R, Vogl J, Lara-Manzano JV, Zoń A, Fung W, Buzoianu M, Caciano de Sena R, Augusto dos Reis L, Valiente L, Yim Y, Hill S, Champion R, Fisicaro P, Bing W, Turk GC, Winchester MR, Saxby D, Merrick J, Hioki A, Miura T, Suzuki T, Linsky M, Barzev A, Máriássy M, Cankur O, Ari B, Tunç M, Konopelko LA, Kustikov YA, Bezruchko M (2012) CCQM-K87 “Mono-elemental calibration solutions”. Metrologia, Tech Suppl 49:08010Google Scholar
  7. 7.
    Jun W, Hongmei L, Liandi MA (2009) NIM’s role in developing national system of metrology in chemistry for food analysis, IMEKO World congress fundamental and applied metrology, 6–11, Lisbon, Portugal, 2583–2587Google Scholar
  8. 8.
    Kipphardt H, Czerwensky M, Matschat R (2005) ICP-MS analysis of high purity molybdenum used as SI-traceable standard of high metrological quality. J Anal At Spectrom 20:28–34CrossRefGoogle Scholar
  9. 9.
    Felber H, Weber M, Rivier C (2002) Final report on key comparison CCQM-K8 of monoelemental calibration solutions. Metrologia,Tech Suppl 39:08002CrossRefGoogle Scholar
  10. 10.
    Beck CM, Salit ML, Water RL Jr, Butler TA, Wood LJ (1993) Preparation and certification of a rhodium standard reference material solution. Anal Chem 85:2899–2902CrossRefGoogle Scholar
  11. 11.
    Hauswaldt A-L, Rienitz O, Jährling R, Fischer N, Schiel D, Labarraque G, Magnusson B (2012) Uncertainty of standard addition experiments: a novel approach to include the uncertainty associated with the standard in the model equation. Accred Qual Assur 17:129–138CrossRefGoogle Scholar
  12. 12.
    Serapinas P, Labarraque G, Charlet P, Ežerinskis Ž, Juzikienė V (2010) Method of standard additions for arsenic measurements in water by ICP sector field mass spectrometry at accuracy comparable to isotope dilution. J Anal At Spectrom 25:624–630CrossRefGoogle Scholar
  13. 13.
    Salit ML, Turk GC (1998) A drift correction procedure. Anal Chem 70:3184–3190CrossRefGoogle Scholar
  14. 14.
    Salit ML, Turk GC (2005) Traceability of single-element calibration solutions. Anal Chem 77:136 A–141 ACrossRefGoogle Scholar
  15. 15.
    Salit ML, Turk GC, Lindstrom AP, Butler TA, Beck CM II, Norman B (2001) Single-element solution comparisons with a high-performance inductively coupled plasma optical emission spectrometric method. Anal Chem 73:4821–4829CrossRefGoogle Scholar
  16. 16.
    Nater R, Reichmuth A, Schwartz R, Borys M, Zervos P (2009) Dictionary of weighing terms. Springer, BerlinCrossRefGoogle Scholar
  17. 17.
    Spieweck F, Bettin H (1992) Review: solid and liquid density determination. Tech Mess 59:285–292CrossRefGoogle Scholar
  18. 18.
    Bowman HA, Schoonover RM, Jones MW (1967) Procedure for high precision density determinations by hydrostatic weighing. J Res Natl Bur Stand C Eng Instrumen 71C:179–198CrossRefGoogle Scholar
  19. 19.
    Bureau International des Poids et Mesures (2008) Evaluation of measurement data—guide to the expression of uncertainty in measurement, JCGM 100Google Scholar
  20. 20.
    ISO Guide 35:2006, Reference materials—general and statistical principles for certificationGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2014

Authors and Affiliations

  • Angela Kaltenbach
    • 1
  • Janine Noordmann
    • 1
  • Volker Görlitz
    • 1
  • Carola Pape
    • 1
  • Silke Richter
    • 2
  • Heinrich Kipphardt
    • 2
  • Gernot Kopp
    • 3
  • Reinhard Jährling
    • 1
  • Olaf Rienitz
    • 1
    Email author
  • Bernd Güttler
    • 1
  1. 1.Physikalisch-Technische BundesanstaltBraunschweigGermany
  2. 2.BAM Federal Institute for Materials Research and TestingBerlinGermany
  3. 3.MLS GmbHLeutkirchGermany

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