Abstract: A method of XRFS for the determination of tungsten and tin in ores was proposed in this paper. Sample was blended with avicel and pressed in a mould under a pressure of 32 MPa to form a disc sample with its outside diameter of 40 mm and inside diameter of 32 mm. Values of detection limits found were 4.9 mg·kg-1 for tungsten and 3.8 mg·kg-1 for tin respectively. The proposed method was applied to the analysis of ores, giving values of RSD′s (n=12) 1.7% for tungsten and 0.37% for tin. Results obtained in consistency with the results found by GB methods.