Alkalimetric determination of halogeno or carboxylato groups in their triaryl- or trialkylantimony (V) derivatives

Abstract

Halogeno or carboxylato groups in their triaryl- or trialkylantimony (V) derivatives have been determined by alkalimetry after their hydrolysis. The standard analytical process is as follows. About 0.2 mmol(70 150 mg) of the sample is taken into a 200 cm3 beaker, and is dissolved into 20 cm3 of acetonitrile. The mixture is boiled if the sample is hardly soluble. After the complete dissolution, it is diluted with 20 cm3 of water, and is kept for several min. The solution is then titrated with 0.1 M sodium hydroxide aqueous solution. Acetone, N, N-dimethylforrnamide, tetrahydrofuran, and dimethylsulfoxide can also be used in place of acetonitrile (N, N-dimethylforma mide solution should not be boiled). Satisfactory results could be obtained for 13 organoantimony compounds, such as dibromotriphenylantimony (V), diacetatotriphenylantimony (V), bis (benzoato) tris (p tolyl) antimony (V), dibromotrimethylantimony (V) etc. (The samples used were over 99.7% in their purity estimated from their carbon analyses). This method is conveniently applicable to check the composition of the samples of these compounds.