The synthesis of nano-particle Fe, Co and Fe/Co metal catalysts loaded on γ-alumina granules were achieved by a combined sol-gel/oil-drop method using metal ion solutions. Pure metal ion compositions of ion and cobalt, and mixed metal combinations were used. Comparative study of the ferromagnetic component of these reduced and post-reaction catalysts were undertaken to determine the efficiency of catalytic activation process and the subsequent changes in metal centers after the catalytic reactions.