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以四苯鏻过氯酸盐、氟钽酸盐为电活性物质,对六种介体溶剂进行比较,选择苯二甲酸二(2-乙基己)酯研制成四苯鏻盐PVC膜电极,线性响应下限可达5×10~(-8)M.以该电极为指示电极,提出四苯溴化鏻作滴定剂电位滴定铌的新方法。滴定5-10mg铌的变异系数为0.26％,大量Fe、Co、Ni、Al、Cu、Ti、Sn、Ge不干扰,可在硫酸、磷酸、盐酸介质中滴定。应用于超导及磁钢材料中铌的测定,不需分离共存元素,远较重量法简单快速,结果亦良好。
Using tetraphenylphosphonium perchlorate and fluorotantalate as electroactive materials, six kinds of mediator solvents were compared. Di (2-ethylhexyl) phthalate was selected to develop into tetraphenylphosphonium salt PVC membrane electrode. The lower limit of linear response is up to 5 × 10 ~ (-8) M. With this electrode as the indicator electrode, a new method of titration of tetrabenzylphosphonium bromide as potentiometric titrator for niobium is proposed. Titration 5-10mg Niobium coefficient of variation of 0.26%, a large number of Fe, Co, Ni, Al, Cu, Ti, Sn, Ge do not interfere, in sulfuric acid, phosphoric acid, hydrochloric acid medium titration. Applied to the determination of niobium in superconducting and magnetic materials, without the need to separate the coexisting elements, the method is far simpler and faster than the gravimetric method and the result is also good.