The effect of phosphorus content and preparation methods is studied in this present investigation. Three different methods are employed for preparation of catalysts. The catalysts are characterized by pore size distribution, X-ray diffractogram and temperature programmed reduction. Thiophene hydrodesulfurization (HDS), cumene hydrocracking (HQ, gas oil HDS and Maya heavy crude HDS and hydrodemetallization (HDM) activities are performed. It is found that specific surface area gradually decreases with P loading. The addition of phosphorus increases the formation of polymolybdate species which are more active for hydrotreating reaction. It is also observed that reducibility of these species also increases with P loading. However, at higher P loading the crystalline MoO3 is formed at the expense of these multilayer polymeric molybdates. The increment in the activity is more in the catalyst prepared by co-impregnation method. The activity increases with P loading up to 1 wt% P content. At higher loading the activity decreases. It is also noted that P inhibits coke formation on the catalyst during hydrotreating of heavy crude oil. Phosphorus can also modify the Bronsted acidity of the catalyst and hence cumene hydrocracking activity slightly increases. (C) 2007 Elsevier B.V. All rights reserved.