硫脲光度法测定粗铼酸钾中铼时钼干扰的消除  

Elimination of the interference of molybdenum in determination of rhenium in raw potassium rhenate by thiourea spectrophotometry

作　　者：周煜[1] 谭艳山[1] 朱利亚[1,2] 牛春林[1] 汤云正[1] 李玉仙[1] 李美菊[1] 万仲建[1] 王前会[1] 

机构地区：[1]云南铜业股份有限公司,云南大理675600 [2]贵研资源(易门)有限公司,稀贵金属综合利用新技术国家重点实验室,云南昆明650106

出　　处：《冶金分析》2013年第9期57-60,共4页Metallurgical Analysis

基　　金：昆明贵研资源(易门)有限公司横向合作基金资助项目(GYZY-2012-001)

摘　　要：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，4mLEDTA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O～20ug／mL范围内符合比尔定律，检出限为1．91×10μg／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 selective determination of rhenium in raw potassium rhenate containing molyb- denum was proposed by thiourea-rhenium（ II ）-stannous chloride spectrophotometry after masking mo- lybdenum with hydroxylamine hydrochloride-molybdenum （V）-EDTA complex. The conditions for masking molybdenum with hydroxylamine hydrochloride-molybdenum （ V ）-EDTA and the coloring conditions for thiourea-rhenium （ II ）-stannous chloride were optimized. The results showed that, in weak hydrochloric acid, 3.0 mg of molybdenum could be masked with 4 mL of EDTA solution and 3 mL of hydroxylamine hydrochloride solution in water bath at 80 ℃ for 35 min. Moreover, the compl- exation masking system had no influence on the coloring complex. In 3.0 mol/L hydrochloric acid me- dium, the Beer＇s law was obeyed for mass concentration of rhenium in range of 0-20 μg/mL at A440 nm. The detection limit was 1.91× 10 8 μg/mL. The proposed method was applied to the determina- tion of rhenium （10%-20%） in raw potassium rhenate sample containing molybdenum （40%-50%）, The relative standard deviation （RSD, n=7） was 0.15%-0.25%, and the recoveries were 100%.

关 键 词：铼 粗铼酸钾 硫脲光度法 钼 

分 类 号：O657.32[理学—分析化学]