The addition of 8-hydroxy quinoline (Oxine) to vanadium and nickel in oil product sample from Saudi Arabia has increased the efficiency of the extraction. An inductively coupled plasma mass spectrometer (ICP/MS) and standard addition method were used for determining concentrations of vanadium and nickel. Recoveries of added vanadium and nickel as oil soluble salts were made and found to be at (98–102%) and (98–104%) ranges, respectively, and the % relative standard deviation for five replicate samples were less than 4% in all cases.