DETERMINATION OF TRIBUTYLTIN AND TRIPHENYLTIN COMPOUNDS IN INDUSTRIAL-WASTE WATER BY GC

Tributyltin (TBT) and triphenyltin compounds (TPT) in industrial waste water were determined by GC with flame photometric detector (FPD) using tripentyltin chloride (Pe3SnCl) as a surrogate compound. A volume of water sample (1 1) was mixed with 10 ml of hydrochloric acid and 20 g of sodium chloride and then extracted twice with 100 ml of hexane. The extract was dehydrated with anhydrous sodium sulfate and concentrated to a small volume (ca. 5 ml) using a rotary evaporator. The concentrate was propylated with 1 ml of 2 mol/1 n-propylmagnesium bromide/tetrahydrofuran. Reaction product was passed through Sep-pak Florisil cartridge column and eluted with 5(v/v)%-diethylether/hexane. The eluate was concentrated to about 2 ml. Three microliters of the concentrate was analyzed by GC equipped with a capillary column (0.53 mm i.d. X 30 m) coated with 1.5-mu-m of DB-5 and FPD. TBT and TPT in industrial waste water from ship building, paint manufacture, and pharmaceutical factory were analyzed by this method. Recovery of TBT and TPT from these water samples was 96 approximately 104%, 105 approximately 106%, respectively and the relative standard deviations (R.S.D.) were 2.2 approximately 6.8%, 1.8 approximately 7.3%, respectively. The detection limits were 10 ng/1 for TBT (as tributyltin chloride), 30 ng/l for TPT (as triphenyltin chloride). Analysis by GC/MS were also performed. Analytical data by GC/MS agreed well with the data by GC-FPD. R.S.D. by GC/MS were 0.4 approximately 1.7% for TBT, 1.1 approximately 2.5% for TPeT, 1.1 approximately 3.7% for TPT, when standard solution and actual waste water samples were analyzed.