We demonstrate the preparation and catalytic testing of nanocatalysts composed of TiO2 synthesized in aerogel using a supercritical drying process with Pt nanoparticles deposited on the mesopore oxide surface. By controlling the aging time, we found conditions that led to TiO2 with a surface area among the highest ever reported for a TiO2 material in aerogel form (similar to 685 m(2) g(- 1)). The chosen synthesis route also features good control over the pore volume and pore size. Even though our aerogel TiO2 support showed an amorphous structure before calcination, 90.2% anatase and 9.8% rutile phases co-existed after calcination at 500 A degrees C for 2 h with an average particle size of about 17 nm based on XRD results. The as-synthesized TiO2 and Pt/TiO2 were both used as catalysts for the CO oxidation reaction. Uncalcined Pt/TiO2 showed 100% conversion at 300 A degrees C. After calcination, Pt/TiO2 exhibited a significantly higher catalytic activity, showing 100% conversion at 125 A degrees C and an activation energy of only 13.4 kcal mol(- 1). We show that TiO2 synthesized by the aerogel method can be an excellent support material for nanocatalysis because of its high surface area and facile and scalable synthesis. [GRAPHICS] .