Abstract: A method for the determination of SiO2, Al2O3, Fe2O3, TiO2, CaO and MgO in magnesiumbased refractory materials by X-ay fluorescence spectrometry with powder pellet sample preparation was developed. The instrument operating parameters were optimized and a series of standard reference materials were used for the calibration. The matrix effect was corrected by using empirical coefficient method. The analytical precision of the method for major and minor components were less than 5% RSD（n=10）. The method has been applied to the determination of these six components in magnesiumbased refractory materials with satisfactory results.