The catalytic properties in n-hexane total oxidation of perovskite type mixed oxides, LaCo(1-x)FexO3 prepared by a new technique designated as reactive grinding, are investigated. All catalysts were found significantly more active than a reference sample prepared by conventional synthesis using amorphous citrate complexes. The activity per unit surface area was found to depend on grinding conditions and calcination temperature. These enhanced activities are associated with both the high surface area and high defect density reached by the reactive grinding synthesis method. Cobalt rich perovskites were shown more active per unit surface area than iron perovskites calcined at the same temperature.