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The paper looks at the development of a technique for determining the qualitative and quantitative phase composition of catalytic systems based on nano-sized iron-containing particles suspended in a hydrocarbon medium, that are active in the Fischer-Tropsch synthesis. In this study, a qualitative X-ray phase analysis was carried out using the identification of crystalline phases based on their inherent values of interplanar distances and the corresponding intensities of the X-ray spectrum lines, and a quantitative phase analysis of samples of iron-containing catalytic suspensions was carried out using corundum number methods and the Rietveld method. Highly crystalline cerium oxide was used as an internal standard. The Jade software was used for calculations by the corundum number method, and the Maud software was used for calculations by the Rietveld method. The results obtained for the concentrations of the internal standard phase by the Rietveld method turned out to be closer to the contents of cerium oxide determined by X-ray fluorescence elemental analysis, which allows us to conclude that the Rietveld method is a priority for quantitative phase analysis of complex multicomponent systems.