The applicability of energy dispersive X-ray fluorescence spectrometry as an analytical technique for the determination of a few metallic impurities such as Ca, Cr, Cu, Fe, Mn, Pb, and Zn in alumina (Al 2 O 3 ) matrix was investigated. A series of Al 2 O 3 standards containing the elements of interest in the range 10-1000 ppm was prepared and the spectrometer conditions were optimized to obtain calibration plots for the various analytes that could be further used for the analysis of actual samples. The present method serves as an alternative to currently used AES method for analytes expected in the concentration range 50-1000 ppm.