A method is described for the determination of chromium in a nickel base B-Cr-Fe-Si alloy powder. The existing technique began with the melting of as received powder samples in an electric button furnace, and analysis of the solid sample by x-ray fluorescence. The procedure gave erratic quantitative results for high chromium alloys because of the segregation associated with the precipitation of chromium borides. Dilution of the as received powders with 30% nickel before melting solved the problem of chrome boride segregation, as evidenced by the concurrence of results obtained by both x-ray fluorescence and wet chemical results for chromium percentage in the alloys.