A CoMo/gamma-Al2O3 catalyst, prepared by depositing on the Al2O3 carrier first the Mo species via equilibrium deposition filtration (EDF) and then the Co species by dry impregnation, was compared to three CoMo/gamma-Al2O3 samples prepared using various conventional impregnation methods. All samples had the same composition, cot-responding to an atomic ratio Co/(Co + Mo) equal to 0.3. The above samples were characterized using various physicochemical techniques (AAS, BET, DRS, LRS, XPS, TPR, and NO chemisorption), and their catalytic activity was determined using the hydrodesulfurization (HDS) of thiophene as a probe reaction. The EDF-prepared catalyst was about 30-43% more active in HDS than those prepared with the conventional impregnation techniques at all reaction temperatures studied. In contrast, the EDF catalyst exhibited the lowest hydrogenation activity. The higher HDS activity of the EDF sample is attributed to the higher number of active HDS sites formed on its surface. It is concluded that the increased number of active sites is due to the fact that the deposition of the Mo species by EDF results to a higher coverage of the support surface by supported molybdenum phase, which in turn, inhibits the formation of the catalytically inactive CoAl2O4 and favors the dispersion of octahedral cobalt on its surface. (C) 2003 Elsevier Inc. All rights reserved.