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Intercalation of lithium ions in nanoporous anatase TiO₂ was studied with XPS using a novel electrochemical preparation technique. The electrolyte was 0.5 M LiClO₄ in acetonitrile (not water-free). The electrochemical insertion of lithium ions creates reduced Ti ions (Ti³⁺), which was observed as a new well-resolved state in the Ti 2p core level spectrum shifted 2.1 eV to lower binding energy. The new Ti 2p state was reversible when the electrode was deintercalated. Changes in the O 1s core spectra were also observed and discussed in terms of hydrated lithium ions in the Helmholtz layer, or formation of Li₂O/LiOH.