Transition metals such as Ni, V in the heavy residual oil should be eliminated in advance for further upgrading of the oil. The nickel and vanadium metals in the vacuum residue (VR) have been eliminated by the combination of solvent separation process and chealation process. The metal-porphyrins concentrated into the asphalten part and then further eliminated by the adsorption process onto mesoporous adsorbents. The transition metals separation processes have been monitored by various spectroscopic analysis.