Abstract: X-ray fluorescence spectrometry (XRFS) with sample preparation by pressure powder molding was applied to the determination of 8 chemical components (including SiO₂, CaO, TiO₂ etc.) in high-titanium blast furnace slag. Powdered slag sample with granular size <0.125 mm was taken and pressed under 25 MPa for 30 s to give sample tablet for use in XRFS analysis. A higher working voltage of 50 kV and lower current of 40 mA were chosen for the X-ray tube, to solve the problem of dificulty in separation of analytical signals from interfering noise caused by the high-bearing elements of Si, Ca and Ti. Good precision and accuracy were shown by the results obtained in analysis of slag samples of high, medium and low contents of the analytes by the proposed method. As compared with the results found by XRFS with the fusion sample preparation, values of relative errors obtained were within the allowable limits.