新铪试剂间羧基偶氮苦氨酸的合成及其分析性能的研究

Study on the synthesis and analytical characteristics of a new chromogenic reagent for hafnium-pi(?)ramazochrom-m-COOH

间羧基偶氮苦氨酸的合成及纯化方法。研究了此试剂与铪的反应条件。在盐酸介质中.试剂与铪形成1:1的蓝色配合物,在624nm 波长处具有最大吸收,对比度为80nm,摩尔吸光系数为4.08×10~4;在体系中加乳化剂OP 后,试剂与铪形成2:1的蓝色配合物,在638nm 波长处具有最大吸收,对比度为83nm,摩尔吸光系数为7.76×10~4。在两种体系中,铪量在0～40μg/25mL 范围内均符合比尔定律。适量的锆小影响测定。

In this paper,the synthesis and purifica-tion of picramazochrom-m-COOH is de-scribed.The color reaction between the newchromogenic reagent and hafnium has beenstudied.In HCl medium,the reagent reactswith hafnium to form a 1:1 blue complex,having an absorption maximum at 624nm(△λ=80nm)with an apparent molar absorp-tivity of 4.08×10~4L·mol^(-1)·cm^(-1).In thepresence of emulsifier OP,the complex withthe molar composition of 1:2(metal:reagent)is remarkably sensitized.The complex exhibitsa maximum absorption at 638nm(△λ=83nm)with an apparent molar absorptivity of 7.76×10~4L·mol^(-1)·cm^(-1).Beer's law is obeyed for0～40μg of hafnium in 25mL of solution.Zirconium in reasonable amounts does notinterfere with the determination.