Chemical analysis of spent Co/Mo/gamma Al2O3 catalyst revealed the presence of carbon, molybdenum, sulfur, vanadium and cobalt at levels of 16.0, 10.9, 7.3, 4.6 and 4.0 wt.%, respectively. It was found that calcination at 500 degreesC provides an effective solution for the removal of carbon and sulfur and this generates the oxide form of the heavy metals. The removal of these heavy metals can be achieved through a two-stage leaching process. During the first stage, in which concentrated ammonia is used and it has been found that this process can be successful in removing as much as 83% (w/v) Mo. In a second stage, it was found that using 10% (v/v) of sulfuric acid, it was possible to account for up to 77% (w/v) Co and 4% (w/v) Mo removal. Leaching test results indicated that the vanadium present in the heated spent catalyst was almost stabilized but the molybdenum and cobalt were not. The combination of two solid wastes, ladle furnace slag (LFS) and treated residue of spent catalyst, could be used for making a high value-added anorthite glass-ceramic materials. Further leaching tests showed that ceramic glass materials provided a very effective method of Co, Mo and V heavy metals stabilization resulting in a product with a possible commercial value.