Two groups of samples were studied for the aromatization of methane over Mo-Fe/ZSM-5 catalysts. The first group contains fixed loading (5 wt%) and variable Mo/Fe ratio. The second group was prepared with fixed Mo/Fe ratio and variable loading. The samples were characterized by TGA, S (BET), XRD, NH3-TPD and TPO analysis. NH3-TPD results indicate that the strength of strong acid sites increases when Mo/Fe ratio decreases for samples with fixed loading. The amount of strong sites decreases and new intermediate acid sites appear on samples containing both Mo and Fe. XRD results show the presence of iron molybdate for samples impregnated with both Mo and Fe. The catalytic properties of these samples were related not only to the amount and strength of acid sites but also to the iron molybdate phase.