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Published: Journal of Chromatographic Science, Volume 33, Number 3, March 1995, pp. 89-97.

Simultaneous Speciation of Butyl-, Phenyl-, and Cyclohexyltin Compounds in Aqueous Matrices Using Ethylation Followed by Solid-Phase Trace Enrichment, SFE, and GC Determination
Yong Cai and Josep M. Bayona

A method for the simultaneous determination of butyl-, phenyl-, and cyclohexyltin compounds in aqueous environmental matrices is developed. The analytical procedure involves ethylation of ionic organotins by sodium tetraethylborate, trace enrichment of the derivatized organotins on a C18 disk, and then extraction with supercritical CO2. The extract recovered is analyzed by gas chromatography–flame photometric detection without any additional cleanup step. Both aqueous ethylation and supercritical fluid extraction procedures are optimized by simplex and experimental design, respectively. The recoveries of organotins from spiked seawater are studied at two concentration levels. The recoveries range from 82–104% at the higher spiked level (121–441 ng/L as tin) and 79–115% (55% for monobutyltin) at the lower level (12.1–44.1 ng/L as tin). The relative standard deviations are 4–8.5% and 3.1–11% for high and low spiked levels, respectively. The procedure is successfully applied to the determination of organotin compounds in harbor and river water samples.

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