The electronic structure and functional composition of products of the graphite oxide (GO) interaction with concentrated sulfuric acid (H2SO4) are studied, depending on the oxygen content in the precursor and the treatment temperature. X-ray photoelectron spectroscopy, near-edge X-ray absorption fine structure (NEXAFS) measured at the CK edge, and infrared spectroscopy are used to show the recovery of the π electron system of graphene planes at a temperature of 200 °C. Aggregation of functional groups in GO containing more than 40% of oxygen causes the formation of vacancy defects in the planes with treatment. When the GO treatment temperature rises to 280 °C, the oxidation of the basal plane π-regions occurs. The results can underlie the control of the functional composition, vacancy number, and size in graphite materials.