电感耦合等离子体原子发射光谱法测定高纯二氯氧化锆中钙和钡

Determination of calcium and barium in high purity grade zirconium oxychloride by inductively coupled plasma atomic emission spectrometry

用电感耦合等离子体原子发射光谱法（ICP-AES）测定了高纯二氯氧化锆中的杂质元素钙和钡，并对测定条件和高含量锆带来的基体干扰进行了考察。结果表明，大量锆对测定没有干扰，因此无需分离和进行基体匹配。对标准曲线法和标准加入法的测定结果进行了比对，发现两者没有显著性差异，可以通过简单的标准曲线法对二氯氧化锆中的钙和钡进行测定，简化了试验步骤。对加入Ca和Ba为5.0 mg/kg和10 mg/kg的两个浓度水平溶液进行测定，平均回收率在92.6-102%之间，RSD〈8.76%。钙与钡的方法检出限分别为0.06 mg/kg和0.03 mg/kg，可以很好地满足产品中痕量钙和钡的测定要求。

A rapid, accurate and precise method for the simultaneous determination of trace calcium and barium in high purity zirconium oxychloride by ICP-AES has been reported. The matrix influences caused by zirconium on the analytical lines of Ba, Ca have been studied. It was indicated that larger quantities of zirconium do not interfere in the determination. Therefore the method does not need separation of Ca and Ba from Zr or matrix matching. By comparison of the results obtained by standard curve method with those obtained by standard addition method, there were no significant differences between them. The recoveries at tested concentration levels of 5.0 mg/kg and 10 mg/kg were 92. 6%-102% with RSD〈8.76%. The detection limits of Ba and Ca were 0.06mg/kg and 0.03mg/kg, respectively. The proposed method has been successfully applied to the determination of Ba and Ca in high purity zirconium oxychloride.