Analytical and Bioanalytical Chemistry

, Volume 376, Issue 6, pp 780–787 | Cite as

Determination of tributyltin in marine sediment: Comité Consultatif pour la Quantité de Matière (CCQM) pilot study P-18 international intercomparison

  • R. E. Sturgeon
  • R. Wahlen
  • T. Brandsch
  • B. Fairman
  • C. Wolf-Briche
  • J. I. Garcia Alonso
  • P. Rodriguez González
  • J. Ruiz Encinar
  • A. Sanz-Medel
  • K. Inagaki
  • A. Takatsu
  • B. Lalere
  • M. Monperrus
  • O. Zuloaga
  • E. Krupp
  • D. Amouroux
  • O. F. X. Donard
  • H. Schimmel
  • B. Sejerøe-Olsen
  • P. Konieczka
  • P. Schultze
  • P. Taylor
  • R. Hearn
  • L. Mackay
  • R. Myors
  • T. Win
  • A. Liebich
  • R. Philipp
  • L. Yang
  • S. Willie
Paper in Forefront

Abstract

The capabilities of National Metrology Institutes (NMIs—those which are members of the Comité Consultatif pour la Quantité de Matière (CCQM)of the CIPM) and selected outside "expert" laboratories to quantitate (C4H9)3Sn+ (TBT) in a prepared marine sediment were assessed. This exercise was sanctioned by the 7th CCQM meeting, April 4–6, 2001, as an activity of the Inorganic Analysis Working Group and was jointly piloted by the Institute for National Measurement Standards of the National Research Council of Canada (NRC) and the Laboratory of the Government Chemist (LGC), UK. A total of 11 laboratories submitted results (7 NMIs, and 4 external labs). Two external laboratories utilized a standard calibration approach based on a natural abundance TBT standard, whereas all NMIs relied upon isotope dilution mass spectrometry for quantitation. For this purpose, a species specific 117Sn-enriched TBT standard was supplied by the LGC. No sample preparation methodology was prescribed by the piloting laboratories and, by consequence, a variety of approaches was adopted by the participants, including mechanical shaking, sonication, accelerated solvent extraction, microwave assisted extraction and heating in combination with Grignard derivatization, ethylation and direct sampling. Detection techniques included ICP–MS (with GC and HPLC sample introduction), GC–MS, GC–AED and GC–FPD. Recovery of TBT from a control standard (NRCC CRM PACS-2 marine sediment) averaged 93.5±2.4% (n=14). Results for the pilot material averaged 0.680±0.015 µmol kg−1 (n=14; 80.7±1.8 µg kg−1) with a median value of 0.676 µmol kg−1. Overall, performance was substantially better than state-of-the-art expectations and the satisfactory agreement amongst participants permitted scheduling of a follow-up Key comparison for TBT (K-28), a Pilot intercomparison for DBT (P-43), and certification of the test sediment for TBT content and its release as a new Certified Reference Material (HIPA-1) with a TBT content of 0.679±0.089 µmol kg−1 (expanded uncertainty, k=2, as Sn) (80.5±10.6 µg kg−1).

Keywords

Tributyltin Marine sediment International intercomparison 

Notes

Acknowledgements

The authors thank V. Boyko for preparation of the pilot sediment, V. Clancy for help with their distribution, and Z. Mester and P. Maxwell for preliminary analysis of the pilot material for TBT content.

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Copyright information

© Springer-Verlag 2003

Authors and Affiliations

  • R. E. Sturgeon
    • 1
  • R. Wahlen
    • 2
  • T. Brandsch
    • 3
  • B. Fairman
    • 2
  • C. Wolf-Briche
    • 2
  • J. I. Garcia Alonso
    • 4
  • P. Rodriguez González
    • 4
  • J. Ruiz Encinar
    • 4
  • A. Sanz-Medel
    • 4
  • K. Inagaki
    • 5
  • A. Takatsu
    • 5
  • B. Lalere
    • 6
  • M. Monperrus
    • 7
  • O. Zuloaga
    • 7
  • E. Krupp
    • 7
  • D. Amouroux
    • 7
  • O. F. X. Donard
    • 7
  • H. Schimmel
    • 8
  • B. Sejerøe-Olsen
    • 8
  • P. Konieczka
    • 8
  • P. Schultze
    • 9
  • P. Taylor
    • 10
  • R. Hearn
    • 10
  • L. Mackay
    • 10
  • R. Myors
    • 10
  • T. Win
    • 11
  • A. Liebich
    • 11
  • R. Philipp
    • 11
  • L. Yang
    • 1
  • S. Willie
    • 1
  1. 1.Institute for National Measurement StandardsNational Research Council of CanadaOttawaCanada
  2. 2.Laboratory of the Government ChemistTeddingtonUK
  3. 3.Limnologisches Institut Dr NowakOttersbergGermany
  4. 4.Department of Physical and Analytical ChemistryUniversity of OviedoOviedoSpain
  5. 5.National Metrology Institute of JapanTsukubaJapan
  6. 6.LNEParisFrance
  7. 7.Laboratoire de Chimie Analytique Bioinorganique et Environnment, UMR 034Université de Pau et des Pays de l'AdourPauFrance
  8. 8.European Commission, Joint Research CentreInstitute for Reference Materials and MeasurementsGeelBelgium
  9. 9.Crompton GmbH, Research AnalyticGermany
  10. 10.National Analytical Reference LaboratoryPymbleAustralia
  11. 11.Bundesanstalt für Materialforschung und-prüfungFederal Institute for Materials' Research and TestingGermany

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