We report a novel method for synthesizing monodisperse mesoporous TiO(2) spheres (sizes = 0.6-3.1 μm) by hydrolysis of titanium isopropoxide (TIP) in a mixture of C(8)-C(16)n-alkylamine, water, and ethanol. The size increases with decreasing temperature, TIP concentration, and water concentration, and upon purifying TIP. n-Dodecylamine gives the highest monodispersity.