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In this study, we investigate the thermal reduction of graphene oxide using high-temperature annealing in various gas atmospheres: Argon, 10% CO in Argon, and 10% CH4 in Argon. Graphene oxide was synthesized, chemically pre-reduced, and dried before undergoing reduction in these controlled atmospheres. To evaluate the impact of different gases on the reduction process, we conducted a series of characterizations, including combustion analysis for C/O ratio, Raman spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, Brunauer–Emmett–Teller surface area measurements, and electrical conductivity testing. The results demonstrated that the presence of methane during annealing notably increased the reduction rate and induced other changes in the material properties, whereas the use of CO had no significant impact on the final material.