The selective reaction of CO oxidation (PROX) was named as the most attractive way to reduce the CO concentration, thereby purifying the hydrogen. The aim of this work is to make the structural and morphologic characterization of the NiFe2O4 spinel synthesized by combustion reaction, using glycine as fuel, and to evaluate as catalyst in the reaction of selective oxidation of carbon monoxide in the presence of hydrogen, oxygen and carbon monoxide. The powder was prepared by using a vitreous silica crucible on a hot plate at 480°C and according to stoichiometry established by theory of propellants and explosive. The powder was characterized by X-ray diffraction (XRD), FTIR, textural analyses, transmission electron microscopy (TEM) and catalytic measurements. The results from XRD show characteristic peaks of spinel phase without presence of secondary phases. The morphologic results show surface area of 3.1 m2/g and particle size calculated by TEM of 21.72 nm. The catalyst was active and selective for O2, reaching 100% of conversion.