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, Bi(2-x), Pb(x)Sr2Ca2Cu3O8) 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.

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