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探讨了盐酸羟胺-钼(Ⅴ)-EDTA络合物掩蔽钼,硫脲-铼-氯化亚锡分光光度法选择性测定含钼粗铼酸钾中铼含量的方法。对盐酸羟胺-钼(Ⅴ)-EDTA掩蔽钼的体系及对硫脲-铼(Ⅱ)-氯化亚锡络合物显色的条件进行了优化。结果表明:于弱盐酸介质中,80℃水浴35min条件下,4mL EDTA溶液和3mL盐酸羟胺溶液能够掩蔽3.0mg钼,且络合掩蔽体系对显色络合物无影响;于3.0mol/L盐酸介质中,在吸收波长λ440nm处,铼质量浓度在0~20μg/mL范围内符合比尔定律,检出限为1.91×10-8μg/mL。方法用于含钼40%~50%的粗铼酸钾样品中10%~20%的铼含量测定,相对标准偏差(RSD,n=7)为0.15%~0.25%,回收率为100%。
A method for the selective determination of rhenium in molybdenum-containing rhenium rhenium with molylamine, thiourea-rhenium-stannous chloride by hydroxylamine-molybdenum (Ⅴ) -EDTA complex masked with molybdate and thiourea-rhenium-stannous chloride was discussed. The system of hydroxylamine-molybdenum (Ⅴ) -EDTA masked molybdenum and the conditions of thiourea-rhenium (Ⅱ) -tin chloride complex were optimized. The results showed that under the condition of 80 ℃ water bath for 35min, 4mL EDTA solution and 3mL hydroxylamine hydrochloride solution could mask 3.0mg molybdenum in weak hydrochloric acid medium, and the complexing masking system had no effect on the color complex. In 3.0mol / L hydrochloric acid In the medium, Beer ’s law was obeyed at the absorbance wavelength of 440 nm with the concentration of rhenium in the range of 0 ~ 20 μg / mL with the detection limit of 1.91 × 10-8 μg / mL. The method has been applied to the determination of rhenium in 10% ~ 20% potassium Rheninate from 40% ~ 50% molybdenum with the relative standard deviation (RSD, n = 7) of 0.15% ~ 0.25% and the recovery of 100%.