Abstract
Extraction conditions for the determination of tributyltin (TBT) in sediment samples have been developed further. The analytical procedure is based on spiking with isotopically labelled analyte, pressurised liquid extraction (PLE) with a hexane/tropolone mixture, Grignard derivatization and quantification by GC–MS. It was applied to two unknown sediment samples as part of an intercomparison exercise of the Comité Consultatif pour la Quantité de Matière (CCQM). The detection limit was approximately 1.5 ng/g TBT as Sn, while the repeatability and intermediate precision (as the coefficient of variation) were 1.9% and 3.2%, respectively. The expanded uncertainty was 6.2% (coverage factor k = 2), and the accuracy was confirmed by measurement of a certified reference material.
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Acknowledgment
The authors would like to thank Ralph Sturgeon from the NRCC and Raimund Wahlen from the LGC for the provision of the samples, for organizing the intercomparison and for providing the calibration solutions and certified reference materials. P.K. acknowledges a post-doc fellowship from IRMM. The authors would like to thank P. Conneely (IRMM) for his assistance with the Karl Fischer titrations.
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Konieczka, P., Sejerøe-Olsen, B., Linsinger, T.P.J. et al. Determination of tributyltin (TBT) in marine sediment using pressurised liquid extraction–gas chromatography–isotope dilution mass spectrometry (PLE–GC–IDMS) with a hexane–tropolone mixture. Anal Bioanal Chem 388, 975–978 (2007). https://doi.org/10.1007/s00216-007-1285-0
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DOI: https://doi.org/10.1007/s00216-007-1285-0