Zerovalent carbonyl precursor based W/Al2O3 and CoW/Al2O3 catalysts were prepared by controlled and gradual gas phase adsorption in a fluidized bed reactor. The preparation process was followed by diffuse reflectance Fourier transform IR spectroscopy (DRIFT) and temperature programmed desorption (TPD). The catalytic activity of the catalysts was tested in thiophene hydrodesulfurization (HDS), acid the reduction behavior was determined by temperature programmed reduction (TPR), promising activities were achieved, especially with the bimetallic tungsten cobalt catalyst. TPR profiles were in agreement with the observed activity trends. The activity and reduction measurements suggest that preparation method applied together with zerovalent precursors, leads to adsorbed surface species that are more easily activated by sulfur or reduced than traditional tungsten oxide catalysts.