Abstract: XRFS was applied to the determination of iron, vanadium and silicon in ferrovanadium nitride. It was shown that the sample should be pulverized to pass through sample sieve with bore size of 0.074 mm. Sample for XRFS analysis was prepared by pressing the powdered sample into sample pieces having its thickness between 3 to 5 mm using starch or methyl cellulose as binder. As shown by the testing results, stable fluorescence intensities were obtained with the sample piece thus prepared. Working curves were prepared by the matrix matching method in XRFS determinations. Precision was tested by analyzing a sample for 10 determinations, giving values of RSD′s of 0.27% (for Fe), 0.23% (for V) and 1.51% (for Si). It was proved that the results of the 3 elements found by the proposed method checked quite well with the results obtained by methods of chemical analysis.