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The effect of the substitution of cobalt into the GdFeO3 perovskite structure on the selective hydrogenation of CO was investigated. A series of GdCoxFe1−xO3 (x = 0; 0.2; 0.5; 0.8; 1) samples were synthesized by sol-gel technology and characterized by XRD, BET specific area, DSC, TG, EDX and XPS. The experimental data made it possible to reveal a correlation between the state of iron and cobalt atoms, the fractions of surface and lattice oxygen, and catalytic characteristics. It has been found that varying the composition of GdCoxFe1−xO3 complex oxides leads to a change in the oxygen-metal binding energy in Gd-O-Me, the ratio of metals in various oxidation states, and the amount of surface and lattice oxygen, which affects the adsorption and catalytic characteristics of complex oxides.