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Multicomponent and multiphase oxide catalysts with a uniform composition Mo 1 V 0.3 Te 0.23 Nb 12 but different phase contents were studied in the oxidative conversion of ethane to ethylene and characterized by X ray diffraction analysis. The phase composition of the samples was varied by modifying such conditions of catalyst preparation as the pH of raw precursor, the drying of the wet precursor, and the conditions of solid precur sor calcination. The content of the detected phase is determined via Rietveld refinement. The catalytic activity of MoVTeNb oxide catalysts studied in the oxidative conversion of ethane was found to be determined by the content of the orthorhombic M1 phase (the layered four component compound (TeO) 0.23 (Mo,V,Nb) 5 O 14 ).