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根据高酸度溶液中偶氮砷Ⅲ优先和H~+络合的原理,以偶氮胂Ⅲ为显色剂,2.0 mol/L盐酸为溶剂,建立了高浓度La~(3+)(La~(3+)和Zr~(4+)的浓度比大于1.5)共存条件下Zr~(4+)的分光光度测试方法。结果显示,在高质量浓度La~(3+)存在下,以大于0.3 mol/L盐酸为溶剂,可实现对La~(3+)的屏蔽;且当盐酸浓度为2.0 mol/L时,灵敏度最大。在最佳的实验条件下,锆离子的工作曲线方程式为:A=0.101 14C-0.001 17,相关性系数R=0.999 7,线性范围为0.4~2.4μg/m L。该方法简单易行,准确度高。
According to the principle of arsenic Ⅲ and H ~ + complexation in high acidity solution, arsenazo Ⅲ was used as the chromogenic reagent and 2.0 mol / L hydrochloric acid was used as the solvent to establish a high concentration of La ~ (3 +) (La ~ (3+) and Zr 4+ concentration ratio greater than 1.5) under the coexistence of Zr ~ (4 +) spectrophotometric method. The results show that the shielding of La 3+ can be achieved with higher concentration of 0.3 mol / L hydrochloric acid in the presence of high concentration of La 3+. When the concentration of hydrochloric acid is 2.0 mol / L, the sensitivity maximum. Under the optimal experimental conditions, the equation of the working curve of zirconium ion is: A = 0.101 14C-0.001 17, the correlation coefficient R = 0.999 7, the linear range of 0.4 ~ 2.4μg / m L. The method is simple and easy to operate with high accuracy.