ICP-AES分析超导粉中杂质元素的干扰系数矩阵校正法

利用ICP-AES法测定了铋系超导前驱粉(BSCCO)中Fe,Cr,Ni,Si,Al和Ba等微量杂质元素,优化了仪器测定参数并研究了酸的种类及浓度对测定结果的影响。系统研究了BSCCO基体元素Bi,Sr,Pb,Ca和Cu对微量杂质元素测定的干扰,分别测定了每个基体元素对测定元素的校正系数并组成交互干扰校正矩阵,采用全选主元高斯消去法计算出基体元素产生的背景等效浓度,再计算出样品的真实浓度。用此方法对合成标样中的上述微量杂质元素进行了测定,分析结果的回收率99.5%~100.5%,测定了实际样品中的杂质元素,并与ICP-MS法进行了对比,二者结果一致。

Correction of Spectral Interferences with Mutual Interference Coefficient Matrix for Determination of Impurities in Bi-Based Superconductor Powder by Inductively Coupled Plasma Emission Spectrometry

In the present paper a method was proposed for the determination of Fe,Cr,Ni,Si,Al and Ba in Bi-based superconductor powder(BSCCO,Bi2-xPbxSr2Ca2Cu3O8) by inductively coupled plasma atomic emission spectrometry(ICP-AES).The operation parameters for ICP-AES were optimized,and the influences of acid kind and concentration were examined.The interferences of matrix elements Bi,Sr,Pb,Ca and Cu in Bi-based superconductor powder on the determination of impurities were studied systematically.The interference coefficients of Bi,Sr,Pb,Ca and Cu were obtained for each target elements respectively,and the mutual interferences matrix was constituted with the above coefficients.The equated concentrations of background from matrix elements were calculated by interferences coefficients matrix and concentrations of Bi,Sr,Pb,Ca and Cu using Gaussian elimination with full pivoting method.Then the concentrations of impurities were obtained by calculation of differences.By means of the mutual interference coefficients matrix,the artificial sample was determined for the target elements with the recovery coefficient of 99.5%-100.5%.The superconductor powers were analysed with satisfactory results also,and the results were identical with the reference values from ICP-MS.