An optimized sample preparation procedure for organotin speciation in sediment samples has been applied to the analysis of sediments collected in the environment. The method is based on tropolone complexation of the ionic organotins, followed by extraction into a hexane–ethylacetate mixture and derivatization by NaBEt4. The method was applied to the determination of organotin in various harbour, shipyard and dry-dock sediments in Belgium. Butyltin compounds were detected in all samples analyzed, often at high mg kg−1 levels. A limited number of samples showed the presence of phenyltin compounds. Further, the method was adapted to the analysis of river sediments sampled from the vicinity of shipyards. Butyltin concentrations were detected at the µg kg−1 level in the majority of samples.
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