Vanadium-titanium-hydroquinone oxide bronze, V1.67Ti0.33O5±δ /HQ (HQ-hydroquinone), was synthesized by using the sol–gel method. Vanadium pentoxide powder, titanium dihydride, hydrogen peroxide and hydroquinone were used as the starting materials to produce bronze. The composition of the synthesized compound was compared with V1.67Ti0.33O5±δ∙nH2O/HQ xerogel data. The xerogel and bronze were investigated by means of the XPS method. Analysis of the V–O region of XPS spectra showed that vanadium ions in xerogel ocurr in V5+ and V4+ states. In bronze, these ions are in a stable V5+ state. The oxygen in xerogel can be associated with O2- ions, hydroxide grouping and water. Oxygen only exists in bronze in the form of O2- ions and hydroxyl groups. Titanium ions in both cases are in a stable Ti4+ state.