痕量磷的苯芴酮-钼间接比色法—用于三氯氢硅和四氯化硅中痕量磷的测定

• 作 者: 陶光仪 李从 倪哲明 王顺荣
• 机 构: 中国科学院化学研究所,中国科学院化学研究所,中国科学院化学研究所,中国科学院化学研究所,
• 出 处: 分析化学
• 发表日期: 1973年04期
• 关键词: 四氯化硅 三氯氢硅 芴酮 间接比色法 磷的测定 乙酸正丁酯 硫酸介质 定磷法 氢氟酸 杂质

本工作提出一个快速、灵敏、简便的测定三氯氢硅、四氯化硅中杂质磷的方法——苯芴酮测钼间接定磷法。样品水解后以氢氟酸赶去硅,在0.5M高氯酸介质中以乙酸正丁酯萃取形成的磷钼杂多酸,用0.5M高氯酸洗去残余的钼酸铵,并用水反萃取磷钼酸,在硫酸介质中测定钼—苯芴酮的红色络合物。测定的最低量为5×10~(-9)克,当取样量为1毫升时,可测磷含量为3×10~(-7)％。

This work proposed a rapid, sensitive and simple method for the determination of trichlorosilane, silicon tetrachloride impurity phosphorus - phenyl fluorenone measured molybdenum indirect phosphorus method. The sample was hydrofluoric acid after the rush to silicon, in 0.5M perchloric acid medium with n-butyl acetate extraction of the resulting molybdenum phosphomolybdic acid with 0.5M perchloric acid to remove residual ammonium molybdate, Phosphomolybdic acid is extracted and the red complex of molybdenum-phenylfluorenone is measured in a sulfuric acid medium. The minimum amount of 5 × 10 ~ (-9) g was determined. When the sample volume was 1 ml, the measurable phosphorus content was 3 × 10 ~ (-7)%.