Molybdenum catalysts supported on γ-Al 2O 3 and γ-Al 2O 3-MgO mixed oxide with varying loading of MgO (5, 10, 15, 20 wt with respect to γ-Al 2O 3) were prepared successfully by wet impregnation method. The physiochemical properties of these synthesized Mo catalysts were studied by various analytical techniques such as N 2 adsorption-desorption (BET), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Temperature-programmed reduction (TPR).The results showed that the addition of MgO into the support affected the binding energies of the elements and reducibility of the metal oxides formed after calcination of catalyst samples due to change in metal-support interaction. Further, the characterization techniques showed that the active metal was well dispersed on the surface of support material. © (2012) Trans Tech Publications.