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倪哲明等用 BPHA 的氯仿溶液在盐酸介质中萃取微量锆与700倍的钍分离,但尚不能满足测定硝酸钍中 Zr/Th=10~(-6)的要求。本文研究了以 N-苯甲酰苯胲(以下简称 BPHA)的二甲苯溶液在盐酸介质中萃取硝酸钍中微量锆,用二甲酚橙钠盐的乙醇(0.1N 盐酸)溶液为显色剂在有机相中直接显色,形成 BPHA-锆-二甲酚橙络合物,最大吸收峰在545(?)m。在10毫升显色液中(5毫升0.2%BPHA 和5毫升0.1%二甲酚橙)含0～24微克锆时遵从比尔定律。有机相用稀盐酸萃洗后,基体钍不干扰,钍中常见杂质离子如:比锆高百倍的钛、磷及千倍的铀、镧(稀土)、铁和大量的硫酸根、硝酸根等均不干扰。提出了硝酸钍中微量锆的分析方法。方法下限:10~(-4)%.锆回收率大于98%,相对标准偏差<±5%。
Ni Zhezhe BPHA chloroform solution with hydrochloric acid extraction of trace zirconium and 700 times the separation of thorium, but can not meet the determination of thorium nitrate Zr / Th = 10 ~ (-6) requirements. In this paper, we studied the extraction of trace zirconium in thorium nitrate by using xylene solution of N-benzoylbenzene (BPHA) in hydrochloric acid medium. Using the solution of xylenol orange sodium salt in ethanol (0.1N hydrochloric acid) Direct color development in the organic phase, the formation of BPHA-zirconium - xylenol orange complex, the maximum absorption peak at 545 (?) M. Beer’s law is obeyed in 10 ml of color developing solution (5 ml of 0.2% BPHA and 5 ml of 0.1% xylenol orange) containing 0 to 24 μg of zirconium. After the organic phase is extracted with dilute hydrochloric acid, the substrate thorium does not interfere with the common impurity ions in thorium such as titanium, phosphorus and thousands of times higher than zirconium, lanthanum (rare earth), iron and a large amount of sulfate, nitrate and the like Do not interfere. A method for the determination of trace zirconium in thorium nitrate is proposed. The lower limit of the method is 10 ~ (-4)%. The recovery of zirconium is more than 98% with relative standard deviation <± 5%.