Utilyzing the solution prepared for the sulfur determination, the amounts of iron, copper and cobalt in the sulfide ore were determined by X-ray fluorescence spectrometry. The samples were dissolved with the mixed solutions of ,$Br_2;and;HNO_3$ and a major constituent of $SiO_2$was repelled from the solution by HF treatment several times. The analytical results agreed with the data obtained by conventional methods within ${pm}$1.5% for Fe of the range of 20 to 50%, ${pm}$1.0% for Cu of 10 to 15%, and ${pm}$0.4% for Co of 1 to 5%. The present method was tolerably found to be reproducible.