低温密闭消解-KIO3电位滴定法测定金合金中常量锗  

Determination of Ge Content with Potassium Iodate Potentiometric Titration in Au Alloys after Low Temperature Sealing Decomposition

作　　者：朱利亚[1] 李光俐[1] 刘文[1] 李勇[1] 贺小塘[1] 谭文进[1] 吴喜龙[1] 韩守礼[1] 管有祥[1] 谢宏潮[1] 安中庆[1] 

机构地区：[1]贵研资源(易门)有限公司,昆明贵金属研究所稀贵金属综合利用新技术国家重点实验室,昆明650106

出　　处：《贵金属》2012年第3期33-38,共6页Precious Metals

基　　金：国家高技术研究发展计划基金(2012AA063203、2012AA063207);昆明贵金属研究所研究与发展基金(GY-08-RD27)资助项目

摘　　要：研究了低于GeCl4挥发温度密闭分解含锗的金合金的技术、KIO3电位滴定常量Ge的方法和提高方法选择性的条件;比较了电位与传统碘淀粉终点指示法对分析结果准确度、精密度,终点稳定性和敏锐度,方法选择性等的影响。结果表明:在优化条件下,控制消解温度不超过75℃时,9mL HCl-2 mL H2O2能完全消解0.10 g样品,且无Ge的损失。经蒸馏分离收集锗,消除Au(Ⅲ)及常见共存离子的影响。电位终点指示法与传统碘淀粉终点指示法对锗滴定结果准确度基本一致,电位终点指示法实用性更强。方法用于AuGe12、AuGeNi12-2、AuAgGe18.8-12.5、AuAgGeNi43.8-6-0.2等系列金锗合金中6%～13%锗含量的测定,标准偏差和相对标准偏差分别为0.0214%～0.0450%和0.304%～0.391%,样品加标回收率99.11%～100.99%。The Au ahoy samples were subjected to decomposition in a sealed vessel at a temperature lower than that of GeCl4 volatilization, followed by the potentiometric titration with KIO3 to determine the content of Ge after distillation separation. The conditions for decomposition and titration were investigated and op- timized. Under the optimized conditions and for the samples containing 6 to 13% Ge, the standard devia- tion and relative standard deviation were found to be 0. 0214% -0. 0450% and 0. 304%-0. 391% , re- spectively, and recoveries of added standard Ge in sample were 99.11% - 100.99% . The established method can be applied to analysis of AuGel2, AuGeNi12-2, AuAgGe18.8-12.5 and AuAgGe Ni43.8.6-0.2.

关 键 词：分析化学 电位滴定 锗 金合金 低温 密闭分解 蒸馏 

分 类 号：O655.2[理学—分析化学]