Abstract: A method for the determination of 9 trace and associated elements(Cu, Pb, Zn, As, Co, Ni, W, Ba, S) in antimony ore powder pellets by X-ray fluorescence spectrometry was developed.The national standard material and synthetic standard reference materials were used to build the calibration curve, the matrix effect and overlapping interference of elements were corrected by an experiential coefficient method and internal standard of scattered lines. The detection limit of the method and precision(RSD, n=12) is less than 5%. Comparing with the chemical method, the method is simple and fast in operation, with a higher accuracy and good precision, the method effectively solve the problems of complicated operation and serious interference to the associated and harmful trace component, in antimony ores using the chemical method.