Molybdenum was supported on -Al2O3 and γ-Al2O3-MgO mixed oxides by varying the MgO loadings (5, 10, 15, 20 wt with respect to γ-Al2O3, via wet impregnation method. The physiochemical properties of these Mo catalysts were explored by various analytical techniques such as N2 adsorption-desorption (BET), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Temperature-programmed reduction (TPR) and Transmission electron microscopy (TEM). The results show that the addition of MgO affected the binding energies of various elements and reducibility of the metal oxides formed after calcination due to different metal-support interaction. Moreover, the characterization techniques show that the active metal was uniformly distributed on the surface of support material. © 2013 American Scientific Publishers All rights reserved.