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The study focuses on the development of a new procedure for the preparation of reference samples with a given concentration for X-ray fluorescence analysis by adding certain volume of analyzed elements solutions with a known concentration to certified reference rock materials and further fusion with borate fluxes. The presented method of preparing emitters allows not only to obtain samples with the required concentrations for the elements to be determined, but also to preserve the influence that other elements have on the analytical signal. A set of 12 certified reference samples of rocks was used to construct calibration dependencies. The preparation of multicomponent modified reference samples (MRS) was carried out on the basis of certified reference materials (CRM) included in the set for constructing calibration curves. The concentration dependences on the analytical signal were established for the main oxides (SiO