低于GeCl_4挥发温度的密闭消解-ICP-AES法测定AuGe_2合金中Ge  

Sealed Digestion-ICP-AES Determination of Germanium in AuGe_2 Alloy at the Temperature Lower Then GeCl_4 Volatilization

作　　者：周建[1] 朱利亚[1] 李光俐[1] 赵青[1] 管有祥[1] 谢宏潮[1] 陈登权[1] 陈亮维[2] 安中庆[1] 王应进[1] 

机构地区：[1]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 [2]昆明理工大学,昆明650224

出　　处：《贵金属》2012年第1期59-64,共6页Precious Metals

基　　金：昆明贵金属研究所研究与发展基金资助项目(GY-08-RD27)

摘　　要：提出了低于GeCl4挥发温度密闭消解AuGe2合金的新技术,研究了微波密闭消解和微波密闭消化罐室温溶解样品的条件,以及水合肼室温还原Au(Ⅲ)为Au(0)和电感耦合等离子体发射光谱法测定Ge的条件。结果表明:当功率600 W,温度70～80℃,压力3238～3652 kPa,升温5 min,恒温1～2 h或室温4～6 h时,9 mL HCl-3 mL H2O2能完全消解或室温溶解0.10 g样品,且Ge无损失。于约15%HCl介质中,水合肼室温能完全还原Au(Ⅲ)为Au(0)。当分析波长为209.426nm时,测定AuGe2合金中Ge的相对标准偏差0.882%和0.833%,样品加标回收率99.32%～100.71%,检出限0.0049μg/mL和线性范围1～506μg/mL。方法结果准确、分析快速、操作简便,已用于实际的样品分析,结果满意。A new technology of sealed digestion AuGe2 alloy at the temperature lower than GeC14 volatili- zation temperature was proposed. Conditions for microwave sealed digestion and room temperature dissolu- tion of samples by microwave sealed digestion were studied. At the same time, conditions for reduction of Au（ HI ） to Au （0） at room temperature by hydration hydrazine and determination of Ge by inductively coupled plasma atomic emission spectrometry were studied. Results indicate that the sample of 0.1 g is di- gested or room temperature dissolution completely by 9 mL HC1 and 3 mL H202 solution when working pa- rameters of microwave oven or microwave sealed digestion are as following ： power 600 W, temperature 70 80~C , pressure 3238 -3652 kPa, ramp 5 min and holding time 1 -2 h or room temperature 4 -6 h. None of Ge is lost. Au （ HI ） was reduced to Au （0） at room temperature by hydration hydrazine with 15 % HC1. The relative standard deviations of determination of Ge in AuGe2 alloy were 0. 882% and 0. 833% when analytical line was 209. 426 nm, recoveries of added standard Ge were 99.32% - 100.71% , detec- tion limit of Ge was 0. 0049 μg/mL and linear range of Ge was 1 - 506 μg/mL. The proposed method was accuracy, rapid, convenient and has been applied to determination of Ge in actual sample with satisfacto- rily results.

关 键 词：分析化学 密闭消解 低于GeCl4挥发温度 ICP-AES 合金 锗 

分 类 号：O657.31[理学—分析化学]