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Transition metal (Cr, Cu, Fe, Co and Ni) oxides supported on γ-alumina were characterized with respect to their textural parameters and reducibility and used as catalysts in decomposition of nitrous oxide and ethylbenzene (EB) dehydrogenation as well as coupling of both processes. High activity of γ-Al2O3 in N2O decomposition coupled with EB dehydrogenation has been found. An increase in EB and N2O conversion was observed when transition-metal-containing catalysts were used. The activity of catalysts depended on their reducibility. Maximum N2O efficiency was observed for the Cr/γ-Al2O3 sample, whereas γ-Al2O3-supported Cu and Fe oxide systems showed about 50% efficiency of N2O in the reaction. An influence of the molar ratio of N2O/EB on activity and selectivity of the catalysts was found. An excess of N2O resulted in an increase in CO2 formation at nearly constant styrene yield.