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提要偶氮氯膦Ⅲ(CPAⅢ),是显色反应的灵敏试剂之一.国内已有不少应用.熊孝先和潘教麦用于铀的测定,刘绍璞和永康拖拉机厂等先后拟定了测定不同材料中稀土总量的方法.但测定钍的详细研究,尤其钍络合物的萃取性能,似未见报导.为此,本文研究了在1.2N的盐酸中,氯化物存在下,钍-CPAⅢ络合物的萃取行为.实验证明,此络合物可为N-263的甲苯溶液萃取,且络合物在有机相至少稳定24小时;萃取后最大吸收波长位于700nm,而试剂本身在此波长下吸收很弱.络合物组成为Th: CAPⅢ:N-263=1:2:2;除浓缩外,选择性比水相有明显提高;用“饱和法”测得摩尔吸光系数达5.0×10~4,Sandell灵敏度为0.0046μg/cm~2;在5毫升有机相中,钍量在0～20微克内服从比尔定律;所制定的方法用于独居石中钍的测定,获得了令人满意的结果.
Abstract Chlorophosphonazo Ⅲ (CPAⅢ) is one of the sensitive reagents for color reaction. There are many applications in China. Xiong Xiaoxian and Pan Jiaomai were used for the determination of uranium. Liu Shaopu and Yongkang Tractor Factory successively developed the method of determination of different materials However, the determination of thorium in detail, especially the extraction performance of thorium complexes seems to have not been reported.Therefore, in this paper, 1.2N hydrochloric acid, the presence of chloride, thorium-CPA Ⅲ network The results show that the complex can be extracted with toluene solution of N-263, and the complex is stable in organic phase for at least 24 hours. The maximum absorption wavelength after extraction is at 700 nm, and the reagent itself is at this wavelength The absorption is very weak.The composition of the complex is Th: CAPⅢ: N-263 = 1: 2: 2, the selectivity is obviously higher than that of the aqueous phase except for concentration; the molar extinction coefficient is 5.0 × 10 ~ 4, Sandell’s sensitivity is 0.0046μg / cm ~ 2; in 5ml organic phase, the thorium content is within 0 ~ 20μg obey Beer’s law; the method is used for the determination of thorium in monazite, Satisfied with the results.