1987 Volume 36 Issue 3 Pages 133-137
A gas chromatographic method was studied for the determination of trace amount of tributyltin compounds in seawater and sediment. The reaction of tributyltin compound with hydrochloric acid gives tributyltin chloride (TBTC) quantitatively, which is sensitive to ECD. One ml of 12 M hydrochloric acid was added to a 1000 ml of seawater, and the solution was shaken with two 40 ml portions of hexane. The extract was washed twice with 25 ml portions of 0.06 M hydrochloric acid, dried over anhydrous sodium sulfate, and filtered. The resulted solution was concentrated, if necessary, as the sample for gas chromatographic determination. In case of sediment samples, tributyltin compounds were extracted with 100 ml of methanol and 1 ml of 12 M hydrochloric acid using Soxhlet's extractor (70°C/2 h). The extract was concentrated to 10 ml, and diluted by 100 ml of saturated sodium chloride solution. The resulted solution was shaken with two 30 ml portions of hexane, and the hexane phase was treated in the same way as the case of seawater sample. The GC conditions were as follows : column packing, 10% Thermon-HG on Chromosorb W 6080 mesh; column size, 3 m×3 mm i.d. stainless steel column; column temperature, 160 °C; injection and detector temperature, 300 °C; carrier gas, nitrogen, 60 ml/min; detector, ECD (63Ni). The recoveries of the overall performance of this method were 8491% for seawater samples and 8994% for sediment samples. The detection limits of TBTC were 0.6 μg/l in seawater and 0.03 μg/g in sediment.
