Using solution technique, sulfur in the sulfide ore was indirectly determined by X-ray fluorescence spectrometry. The sample was dissolved with the mixed solution of B$r_2$ and HN$O_3$, and Si$O_2$, a major constituent, was repelled from the solution by HF treatment several times, B$a^{2+}$ solution was added to the solution to precipitate the S$O^4_{2-}$ ion as BaS$O_4$. Measuring the fluorescent X-ray intensity of excess Ba2+ ion in the filtrate, the content of sulfur in the original ore was back-calculated. Comparing the results by this method with the gravimetric method, the mean difference was ${pm}1.7%$ in the range of 20 to 40% of sulfur content and the method was tolerably reproducible.