In oxidation of carbon monoxide, the activity of the Cu-Cr-Mn/g-Al-2(3)O catalytic system is correlated with its morphology. The phase composition and valence state of the metal ions in catalysts of different genesis were investigated by x-ray phase analysis (XPA) and diffuse-reflection electron spectroscopy (DRES). The sequence of application of the active components of the system over binary sections affects the catalytic activity. The undesirable copper-chromium combination is excluded by separation of the successively applied combinations of ingredients Cr Cu and Cu-Mn through an interinediate stage.