The present invention relates to the preparation of catalysts for heteroatom removal, particularly sulfur, from petroleum and synthetic fuel feedstocks. The catalyst is comprised of at least one Group VIII metal, and at least one Group VI metal, on a refractory support. The catalyst is prepared by: impregnating an inorganic oxide support material with a Group VI heteropolyacid; treating said impregnated support with an aqueous solution of a reducing agent which is capable of at least partially reducing the Group VI metal of the heteropolyacid; drying said treated support at a temperature from about 20.degree. C. to about 200.degree. C. at about atmospheric pressure; impregnating the treated support with a Group VIII metal salt of an acid having an acidity less than that of the Group VI heteropolyacid; drying said impregnated treated support at a temperature from about 20.degree. C. to about 200.degree. C. at about atmospheric pressure; and sulfiding said impregnated support, thereby forming the catalysts.