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亚砜的测定已有文献介绍。但芳基亚砜的测定方法还不够理想。例如Zn-Hg齐还原、溴酸钾-溴化钾溶液滴定法,由于溴对苯环的取代作用,对芳香族亚砜的测定结果偏高。用HClO_4非水滴定法测定芳香族亚砜,电位突跃的范围小,终点不明显,测定结果偏低。用TiCl_3还原法要求无氧条件(N_2保护),并且手续复杂,一般不易掌握。 KMnO_4容量法,在文献中只介绍过在水溶液介质中对二甲基亚砜的分析,而对其它非水溶性亚砜及其配合物的分析还未见报道。本文介绍在浓乙酸介质中、于H_2SO_4强酸性条件下KMnO_4容量法对若干烷基、芳基亚砜及其稀土配合物的测定及所取得的较好的结果。
Sulfoxide determination has been described in the literature. However, the determination of aryl sulfoxide is not ideal. For example, Zn-Hg reduction, potassium bromate - potassium bromide solution titration, due to the role of bromine on the benzene ring substitution, the determination of aromatic sulfoxide results are high. Determination of aromatic sulfoxide with HClO_4 non-aqueous titration method showed that the range of potential jump was small, the end point was not obvious, and the determination result was low. TiCl_3 reduction method requires anaerobic conditions (N_2 protection), and the procedure is complex, generally not easy to grasp. KMnO_4 volumetric method, in the literature only describes the dimethyl sulfoxide in aqueous media analysis, and other non-water-soluble sulfoxide and its complexes have not been reported. In this paper, the determination of some alkyl, aryl sulfoxide and rare earth complexes by KMnO_4 volumetric method in concentrated acetic acid medium under strong acidic condition of H_2SO_4 and the good results obtained.