Abstract: Residue hydroprocessing catalysts are susceptible to deactivation. One of the causes is metal deposition. Combination utilization of dot, line, and mapping analysis of scanning electron microscope (SEM), second electron (SE) image, back scatted electron (BSE) image, and energy dispersive spectroscope (EDS) can not only qualitatively but also quantitatively analyze the metal deposition to understand the changes of the catalyst properties. The results show that the distribution of Ni is relatively uniform along the cross section of the deactivated catalyst, meanwhile, V and Fe mainly deposite on the outside of the catalyst. Along the flow direction, the amount of deposited Ni and V decrease. Most of the metal deposition is on the demetallization catalyst bed.