低于GeCl4挥发温度的密闭消解-ICP-AES法测定AuGe2合金中Ge

摘要

A new technology of sealed digestion AuGe2 alloy at the temperature lower than GeCl4 volatilization temperature was proposed. Conditions for microwave sealed digestion and room temperature dissolution of samples by microwave sealed digestion were studied. At the same time, conditions for reduction of Au( III ) 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 digested or room temperature dissolution completely by 9 mL HC1 and 3 mL H2O2 solution when working parameters of microwave oven or microwave sealed digestion are as following: power 600 W, temperature 70 -80℃ , 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( III ) was reduced to Au(0) at room temperature by hydration hydrazine with 15% HCI. 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% , detection 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 satisfactorily results.%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600W,温度70～ 80℃,压力3238 ～ 3652 kPa,升温5 min,恒温1～2h或室温4～6h时,9 mL HCl-3 mL H2O2能完全消解或室温溶解0.10g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1～506 μg/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.