基体分离-电感耦合等离子体发射光谱法测定高纯银中21种杂质元素

Determination of 21 impurity elements in high purity silver by matrix separation-inductively coupled plasma optical emission spectrometry

建立了基体分离-电感耦合等离子体发射光谱法测试高纯银中21种杂质元素的分析方法。采用硫氰酸钾作为沉淀剂分离银基体,滤液经定容后,用电感耦合等离子体发射光谱进行测试。21种杂质元素的质量浓度在0~4.0μg/mL范围内与光谱强度呈良好的线性关系,线性相关系数均大于0.992,检出限为0.0001~0.0214 mg/L。加标量为0.5、1.0、2.0 mg/L时,测定结果的相对标准偏差(n=6)分别为0.35%~1.96%、0.41%~2.54%、0.32%~2.07%,平均加标回收率分别为81.5%~109.6%、80.0%~108.6%、81.2%~116.8%。该方法适用于高纯银中21种杂质元素的测定。

A matrix separation-inductively coupled plasma optical emission spectrometry(ICP-OES)method for the determination of 21 kinds of impurity elements in high purity silver was established.Silver matrix was separated by potassium thiocyanate as precipitant,the filtrate was tested by ICP-OES after constant volume.The mass concentration of 21 kinds of elements had good linear relationships with spectral intensity in the linear range of 0-4.0μg/mL with correlative coefficients were more than 0.992,the detection limits were 0.0001-0.0214 mg/L.Under the 3 spiked levels of 0.5,1.0,2.0 mg/L,the relative standard deviations(n=6)were 0.35%-1.96%,0.41%-2.54%,0.32%-2.07%,respectively,the average recoveries were 81.5%-109.6%,80.0%-108.6%,81.2%-116.8%,respectively.The method was suitable for the determination of 21 kinds of elements in high purity silver.