Sulfur compounds in bitumen-derived gas oil undergo selective oxidation using a titanium-derived catalyst, resulting in the formation of sulfones and sulfoxide species. Using caustic solution, the sulfones and sulfoxide species are then chemically converted to hydrocarbon compounds by replacing C-S fragments with C-H fragments. In this study, we provide detailed chemical and structural hydrocarbon-type information for the hydrocarbon streams. The results presented in this paper consist of data obtained using elemental analysis, saturate-aromatic-resin-asphaltene (SARA) separation, and comprehensive two-dimensional gas chromatography (GC x GC) with both flame ionization/sulfur chemiluminescence detectors (FID/SCD) and time-of-flight mass spectrometry detector (TOFMS). These techniques were used to track elemental composition, the speciation of sulfur-containing hydrocarbons, and their respective oxidized and desulfurized counterparts in three bitumen-derived gas oil samples. Based on the compositional data presented in this study, 87.5% of the sulfur compounds were converted to sulfone/sulfoxides compared to the original gas oil feed, followed by 72.5% of the sulfone/sulfoxide conversion to sulfur-free hydrocarbons, resulting in a 63% reduction of the sulfur originally present in the sample. This work is the first known attempt to identify the broad range of species appearing during the oxidative desulfurization (ODS) process of bitumen-derived gas oil feed with the use of GC x GC-TOFMS/SCD/FID techniques. The comprehensive characterization results of SARA fractions provide evidence of the existence of species from two consecutive stages of ODS reactions, oxidation, and desulfurization, which is beneficial to further technology and process development.