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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 technology of airtightly decomposing germanium-containing gold alloy below the volatilization temperature of GeCl4, the method of KIO3 titration constant Ge, and the method of increasing the selectivity of the method were studied. The comparison between the potential and the traditional method of iodine starch endpoint indication on the analysis accuracy, precision , Endpoint stability and acuity, method selectivity and the like. The results showed that 9 mL HCl-2 mL H2O2 can completely dissolve 0.10 g sample without any loss of Ge under optimal conditions when the control digestion temperature does not exceed 75 ℃. The germanium is collected by distillation to eliminate the influence of Au (Ⅲ) and common coexisting ions. Potential endpoint indication method is consistent with the traditional iodate starch endpoint indication method to the accuracy of germanium titration result, and the end potential indication method is more practical. The method has been applied to the determination of 6% ~ 13% germanium in AuGe12, AuGeNi12-2, AuAgGe18.8-12.5, AuAgGeNi43.8-6-0.2 series. The standard deviation and relative standard deviation are 0.0214% ~ 0.0450 % And 0.304% ~ 0.391% respectively. The spiked recoveries of the samples ranged from 99.11% to 100.99%.