Authors: Piotr Konieczka Berit SejerøeOlsen Thomas P J Linsinger Heinz Schimmel
Publish Date: 2007/05/03
Volume: 388, Issue: 4, Pages: 975-978
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 15 ng/g TBT as Sn while the repeatability and intermediate precision as the coefficient of variation were 19 and 32 respectively The expanded uncertainty was 62 coverage factor k = 2 and the accuracy was confirmed by measurement of a certified reference materialThe 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 PK acknowledges a postdoc fellowship from IRMM The authors would like to thank P Conneely IRMM for his assistance with the Karl Fischer titrations
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