电感耦合等离子体原子发射光谱法测定锡锗中间合金中锗
ICP-AES Determination of Germanium in Sn-Ge Intermediate Alloy
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摘要: 锡锗中间合金溶解于硝酸(1+1)及盐酸(1+4)中,溶解温度应在60 ℃以下,所得溶液中锗含量用电感耦合等离子体原子发射光谱法(ICP-AES)测定,对测定条件作了试验并予以优化.最后选择载气流量为0.6 L·min-1,试样溶液的介质及酸度为约2 mol·L-1盐酸溶液,分析谱线为265.118 nm.基体元素锡对锗的分析信号有增强作用,明显影响了锗测定结果的准确性.为克服此基体效应,在制备标准曲线时应用了基体匹配法.经试验,方法的回收率在96.0%~103.6%之间,测定结果的相对标准偏差(n=6)为0.53%.Abstract: Intermediate alloy of tin and germanium was dissolved in HNO3 (1+1) and HCl (1+4) at temperature below 60 ℃,and its germanium content was determined by ICP-AES.Conditions for AES determination were tested and optimized.Flow-rate of carrying gas of 0.6 L·min-1,acidity of ca.2 mol·L-1 HCl of the sample solution,and analytical spectral line of 265.118 nm were selected.Accuracy of analytical results of germanium was affected remarkably by the matrix element of tin due to its enhancement on the analytical signals.The matrix effect of tin was overcome by applying the matrix-matching method in preparation of standard curve.Precision and recovery of the method were tested,giving results of recovery in the range of 96.0%-103.6%,and value of RSD (n=6) of 0.53%.