Аннотация:In the course of synthesis and studies of properties of nanomatherials based on layered molybdenum disulfide, it becomes nesessary to perform rapid elemental analysis and to retern the matherial to customer promptly.In some cases, to improve catalytic or magnetic properties, it is reguired to modify nanoparticles of molybdenum disulfide by metal compounds. A procedure is proposed for rapid X-ray fluorescence determination of molybdenum and cobalt in the content range of 10-50% in similar compounds by a bulk method without dilution. Analytical signals have been measured at the wavelengths of the MoKa and CoKa lines, using a VRA-30 spectrometer (Carl Zeiss, Germany, X-ray tube with Rh anode). The content of the metals has been calculated using the derived equations of interrelations. The error of determination is 2,7%(abs.) for Mo and 1,4%(abs.) for Co. Correctness of the procedure has been confirmed for a batch of synthesized compounds by comparison with XRF results with dilution. The rapid method makes it possible to simplify the procedure and to reduce the time of analysis by more than 4 times; here, the sample is retained and can be used for further research.