船体钢中微痕量锆的ICP-AES法快速测定

Rapid Determination of Trace Zirconium in the Ship Steel by ICP-AES

采用盐酸-硝酸-氢氟酸溶样,加高氯酸冒烟,用盐酸溶解盐类定容后上机测定,研究了船体钢中共存元素对锆的干扰情况,确定了消除干扰的办法,建立了船体钢中微痕量锆的ICP-AES分析方法。分析方法相关系数为0.9996,线性关系良好;检出限为0.004μg/mL,利用本方法对船体钢中的锆进行分析,分析下限可达到0.0005%,是国标方法分析下限0.005%的1/10;本方法相对标准偏差RSD值不大于1%,精密度好;回收率在97%～101%之间,分析误差在国家标准允许误差范围内。

A method was established for rapid determination of trace zirconium in ship steel by inductively coupled plasma atomic emission spectrometry. The working parameters were optimized and proper sample treatment were defined,in which the sample is dissolved with hydrochloric acid,nitric acid and hydrofluoric acid. While perchloric acid is added to smoking and the salt is dissolved with hydrochloric acid before,the solution was determined in inductively coupled plasma atomic emission spectrometry.The interference of coexistent elements on zirconium was analyzed and the measure to eliminate the interference was determined. The Correlation coefficient of the methods is 0. 9996 with a good linear relationship. Analysis limit reaches to 0. 0005%,that is 1 /10 of the lower limit stipulated in national standard method which is 0. 005%. This method is accurate with relative standard deviation( n = 10) less than 1%. The recovery of the method ranged between 97% and 101% and the analysis error is in the national standards allowed range.