The titania nanospheres were synthesized from the controlled hydrolysis of a mixture of titanium(IV) isopropoxide and the precursor, [Ti(OPr i)3(Kry)]n in supercritical carbon dioxide. The use of sc-CO2 in the reaction , eliminates the need for organic solvents, optimizes manufacturing efficiency and produces materials with tailored properties. Simultaneous thermal analysis (STA) data for the nanospheres was carried out from room temperature (RT) to 800°C. The X-ray powder diffraction (XRD) pattern of the heat treated powder (600° C in air), reveals only phase anatase (TiO2).