A thin-layer chromatography/flame ionization detection (TLC/ FID) method for characterization of petroleum residues and heavy oils is described. The asphaltenes (defined as insolubles in n-pentane) are separated and determined gravimetrically. The resin and deasphalted oil (DAO) fractions are separated by spotting 1 mu of the deasphalted sample onto a quartz rod coated with sintered silica gel, followed by development with an n-heptane:dichloromethane (50:50) mixture. The rod is then pyrolyzed in a TLC analyzer equipped with a flame ionization detector. The analysis yields results comparable to those of the Strieter method (a sequential solvent extraction method) and requires less time.