MESOPOROUS alumina with narrow pore size  ……...distribution was synthesized using precipitation method. The effect of various synthesis parameters, including reactants molar ratio, type of co-surfactant, aging time and power source (conventional electric heating (CE) and microwave irradiation (MW)) on the structural properties of the resultant alumina samples were examined. The texture and crystalline phase of the prepared samples were characterized using N₂ adsorption-desorption, pyridine adsorption, XRD, TG-DTA, and TEM. The adsorption activity of the prepared samples was examined towards thiophene and dibenzothiophene species.The prepared alumina samples exhibited narrow pore size distribution with high surface area about 262-334 m²/g, and large mesoporous frameworks with ordered worm-like pores. The preliminary results on the adsorption of sulphur compounds showed that the prepared alumina samples using microwave irradiation as power source and i-propanol as co-surfactant showed distinguished adsorption activities. The structural properties obtained are very interesting for potential applications in desulfurization process in petroleum refining.