The production of gaseous sulfur-containing species during the steam-assisted recovery of heavy oil and bitumen presents problems owing to their toxicity, corrosion properties and odor. In order to quantitatively study aquathermolysis sulfur chemistry during the thermal (steam-assisted) recovery of heavy oils we have subjected a well-characterized and sulfur-rich bitumen core sample to 150 - 325°C and 70 - 1740 psia (0.48 - 12 MPa) conditions in the continued presence of liquid water for 24 hours. The reaction products include gases, oil flotate, oil sinkate, water-soluble products, and water- insoluble residues. All have been studied with a variety of analytical techniques, including FTIR spectroscopy, chromatographic fractionation (SARA analysis), GC-FPD and GC-MS. Moreover, these techniques have been extended to analysis of the asphaltene fractions. Results suggest that some in-situ upgrading of the oil occurs under these conditions; additionally, gaseous hydrogen sulfide is released at temperatures at and above 250 °C. Variations in the relative abundances of solubility classes and chemical fractions imply that the source of sulfur is via the thermal degradation of resins and/or asphaltenes. The experimental methods, results and quantification approach discussed herein will be useful to support the development of models for engineering design of facilities for the steam-assisted recovery of heavy oils and bitumen.