Sulfur compounds in the gas oil fractions from two bitumens (Athabasca oil sand and Cold Lake deposit), a heavy oil (Lloydminster) from Cretaceous reservoirs along the western Canada sedimentary basin, and a Cretaceous oil from a deep reservoir that may be mature (Medicine River) are investigated. The gas oil distillates were separated to concentrates of different hydrocarbon types on a liquid adsorption chromatographic column. The aromatic hydrocarbon types with their associated sulfur compounds were resolved by gas chromatographic simulated distillation and then by gas solid chromatography. Some sulfur compounds were further characterized by mass spectrometry. The predominant sulfur compounds in these fractions are alkyl-substituted benzo- and dibenzothiophenes with short side chains which have few dominant isomers.