Abstract
An improved method was proposed for the gasliquid chromatographic determination of n-butyl-, n-octyl- and phenyl-tin halogenides, which were treated with Grignard reagents before injection into a gas-liquid chromatograph equipped with a thermal conductivity detector. Grignard reagents and gasliquid chromatographic conditions used in this procedure were as follows.
Butyl-tin compounds: Grignard reagent-n-propyl magnesium bromide; column-3 mm × 0.75 m, stainless steel packed with 25 wt.% silicone DC 550 on 80-to 100-mesh Celite 545; temperature -190°C; carrier gas-helium 50 ml per min. flow rate; internal standard-n-octadecane.
Octyl-tin compounds : Grignard reagent-n-amyl magnesium bromide; column-3 mm × 0.75 m, stainless steel packed with 25 wt.% silicone DC HV grease on 80- to 100-mesh Celite 545; temperature -280°C; carrier gas-helium 90 ml per min. flow rate; internal standard-trioctylpropyl-tin.
Phenyl-tin compounds: Grignard reagent-n-amyl magnesium bromide; column-3 mm × 0.75m, stainless steel packed with 25 wt.% silicone DC HV grease on 80- to 100-mesh Celite 545; temperature -260°C; carrier gas-helium 50 ml per min. flow rate; internal standard-triphenylbutyl-tin.
