By a complex of methods we succeeded in determining the phase composition of powders intended for the production of high-speed steel ROM2F3 by the method of powder metallurgy. By chemical differentiation of the carbides and solid solutions (α-Fe, γ-Fe) we established qualitatively the prescribed composition of the carbides MC and M2C, and in monoliths the composition of M6C. The distribution of elements between the carbides MC and M2C was demonstrated, and their quantities and composition determined. The energy spectra obtained from carbide particles showed that in vanadium base MC and in molybdenum M2C a very small amount of iron is dissolved (in the form of impurities). It was the first time that x-ray microspectrometric analysis was used in combination with investigations of carbides in the powders of high-speed steels in the regime of secondary emission and with emission spectroscopy with a plasma source of excitation (in determining some elements).