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In the paper, bulk property and chemical composition of Kazakhstan vacuum residuum were characterized. Sulfides and thiophenes were selectively isolated from the residuum and characterized by Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS). Molecular weights of the sulfur compounds were varied from 150 to 800 Da and S1 , S2 , O1S1 , O2S1 , N1S1 class species were assigned in the heavy oil derived methylsulfonium. Vanadyl porphyrins characterized by positive-ion electrospray ionization and FT-ICR MS, which showed that etioporphyrins (ETIO) (CnH2n-28N4V1O1 , corresponding to DBE = 17) and deoxophylloerythroetioporphyrins (DPEP) (CnH2n-30N4V1O1, corresponding to DBE = 18). It should be noted that the vanadyl porphyrins were most abundant.