Cr(CO)(6)/alumina catalysts promoted with Co-2(CO)(8) were prepared in a fluidised bed reactor by vapour phase adsorption of zero valence metal carbonyls. Catalysts were characterised by diffuse reflectance IR spectroscopy. The catalytic activity was tested in thiophene hydrodesulphurisation (HDS) at 370 degrees C in a batch reactor. Promising HDS results were achieved especially with the reduced bimetallic CrCo/alumina catalyst. The degree of sulphidation was determined after the HDS reaction. The reduction of the catalysts was also investigated by temperature programmed reduction (TPR). TPR and sulphidation results are in agreement with HDS experiments.