1987 Volume 36 Issue 3 Pages 143-148
A gas chromatographic method is presented to determine traces of tricyclohexyltin compounds(TCTC) in environmental samples by using a clean-up cartridge packed with moderately sulfonated polystylene beads. The TCTC in water sample were converted to tricyclohexyltin chloride(TCTCl) with hydrochloric acid, and extracted with hexane. The extract was filtered, and the residue was washed with hydrochloric acid-ethanol solution. The TCTCl in the combined filtrates, mixed with water, was extracted with hexane and was concentrated to ca. 0.5 ml, then made up 10 ml with ethanol. The species in sediment were extracted with hydrochloric acid-ethanol solution and the extract was filtered. The filtrate, mixed with 15% of sodium chloride solution, was extracted with hexane. The organic phase was successively washed with 0.5 M sodium hydroxide in water-ethanol(1 : 1, v/v) and water was concentrated and made up in the same way as for the water sample. The TCTCl in the concentrated sample was passed through a cartridge packed with the hydrogen form resin, cleaned up with ethanol and eluted with hydrochloric acid-ethanol solution. TCTCl extracted with 5 ml volume of hexane was hydridized with 2.5% sodium borohydride-ethanol solution. The tricyclohexyltin hydride(TCTH) formed was extracted with hexane and analyzed by a gas chromatograph with 5% Silicone OV-1 column and electron capture detector(ECD). The TCTC in environmental samples were successfully cleaned up with the cartridge and determined by GC-ECD with good selectivity. Recoveries of the TCTC from water samples and sediments were 8697% with 1.45.0% of relative standard deviation, and the detection limit was 0.5 μg/l, 0.02μg/g as hydroxide, respectively.
