Abstract: The morphology of nickel and vanadium compounds in the asphaltenes were investigated via hydropyrolysis with the help of inductively coupled plasma mass spectrometer (ICP-MS), ultraviolet-visible (UV-Vis), high-temperature gas chromatography atomic emission detection (HT GC-AED), and positive-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (+ESI FT-ICR MS). The results showed that the toluene soluble yields of products decreased from 64% to 19% as the hydropyrolysis temperature increased from 330 to 410 ℃, while the abundance of nickel and vanadium compounds detected by GC-AED increased significantly. The molecular composition distribution of nickel and vanadyl porphyrins showed rhythmic changes with different temperatures in the hydropyrolysis of asphaltenes.