トリアリール-及びトリアルキルアンチモン(V)誘導体中のハロゲン又はカルボキシラト基のアルカリ滴定

概要

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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 cm^3 beaker, and is dissolved into 20 cm^3 of acetonitrile. The mixture is boiled if the sample is hardly soluble. After the complete dissolution, it is diluted with 20 cm^3 of water, and is kept for several min. The solution is then titrated with 0.1 M sodium hydroxide aqueous solution. Acetone, N, N-dimethylformamide, 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.
社団法人日本分析化学会の論文
1980-05-05