The distribution of vanadium and nickel upon hydroconversion of vacuum tower bottoms in the presence of slurried MoS2, Ni7S6, (NH4)0.25 ⋅ WO3, and Fe1 − xS nanoparticles has been studied. The experiments have been performed in an autoclave reactor and in a flow-through hydroconversion unit. It has been shown that the coke yield in hydrocracking reactions increases in the order MoS2, Ni7S6, (NH4)0.25 ⋅ WO3, Fe1 − xS. The proportion of metals in the toluene-insoluble hydroconversion residue increases in the same order. As the hydroconversion temperature increases, the transfer of vanadium and nickel to condensation products increases. According to electron microscopy data for the toluene insolubles, it can be assumed that vanadium and nickel are bonded to carbon, enter into the coke composition, and do not form compounds with the active phase of the MoS2 catalyst.