The results of the comparative quantitative study of oxygen-containing groups adsorbed on the surface of carbonized sponge scaffold (CSS), highly oriented pyrolytic graphite (HOPG), fullerite C60 and multi-walled carbon nanotubes (MWCNTs) introduced into a high vacuum from the atmosphere without any pre-treatment of the surface are discussed. The studied materials are first tested by XRD and Raman spectroscopy, and then quantitatively characterized by XPS and NEXAFS. The research results showed the presence of carbon oxides and water-dissociation products on the surfaces of materials. It was shown that main source of oxygen content (~2%) on the surface of HOPG, MWCNTs, and C60 powder is water condensed from the atmosphere in the form of an adsorbed water molecule and hydroxyl group. On the CSS surface, oxygen atoms are present in the forms of carbon oxides (4–5%) and adsorbed water molecules and hydroxyl groups (5–6%). The high content of adsorbed water on the CSS surface is due to the strong roughness and high porosity of the surface.