膦系化合物中磷含量的测定方法研究

Study on the Determination Method of Phosphorus Content in Phosphine Compounds

膦系化合物中磷含量的快速测定有重要的意义。传统的有机磷含量测定的消解方法用于对膦系化合物的消解有诸多不足。本文以甲基膦酸二甲酯为试样,用不同组合的氧化剂对其消解,以磷钼酸铵重量法作为测定方法,研究了膦类化合物的消解方案。结果表明,分批加入KMnO4,每2 h加入0.5 g,在120℃反应10 h消解甲基膦酸二甲酯的方法最佳。该方法具有回收率高、准确度高、操作简单的优点。

The rapid determination of phosphorus content in phosphine compounds is of great significance.The traditional digestion method for determination of organic phosphorus content has many shortcomings for the digestion of phosphine compounds.In this paper,dimethyl methylphosphonate is used as a sample,and different combinations of oxidants are used to digest it,and the ammonium phosphomolybdate gravimetric method is used as the determination method to study the digestion scheme of phosphine compounds.The results show that adding KMnO4 in batches,adding 0.5 g every 2 h,and reacting at 120℃for 10 h is the best method for digestion of dimethyl methylphosphonate.The method has the advantages of high recovery rate,high accuracy and simple operation.