The chemical structures of fresh and aged Ti-peroxy gels, made from metallic titanium and hydrogen peroxide, were analyzed in the aqueous and solid states by FT-Raman spectroscopy. Fresh transparent gels displayed strong Ti-peroxy vibrations. In gels aged for 3 years in the aqueous state the dried precipitate was rutile. Fresh transparent gels were freeze-dried first, and then aged for 3 years in the dry state, however, displayed Ti-peroxide and anatase vibrations. Accelerated degradation and aging of solids of fresh transparent gels by heat treatment at 200°C gave rise to a white precipitate identified as anatase. Additional heat treatment of the white precipitate at 1050°C showed bands characteristic of rutile. The present study shows that rutile is the main degradation product formed in aging aqueous Ti-peroxy gels. © 1993 Academic Press, Inc.