The removal of hazardous organic compounds from water has become an issue of serious concern.[1-3] Efficient wastewater treatment is essential in the face of increasing population, industrial activity, and decreasing energy resources. Currently used methods for the removal of organic compounds from wastewater include biological, physical, and chemical treatment. However, traditional wastewater treatment methods have several disadvantages. [3,4] Photooxidation is an attractive alternative method for wastewater treatment because it utilizes solar energy (free and inexhaustible), does not produce secondary product waste since the organic waste is decomposed to harmless chemicals during process, [3] and can eliminate toxic, bioresistant, and inorganic compounds from wastewater.[4]The photocatalyst TiO 2 is a wide-bandgap semiconductor that can be used to readily degrade organic compounds, [2,5,6] and is found in three different crystalline phases: anatase, rutile, and brookite. Most titania photocatalyst studies have utilized the anatase crystalline phase, which can be synthesized in large quantities by aerosol flame reactors using vapor-phase titanium-organic or titanium-chloride precursors. [7,8] Recently, however, it has been demonstrated that brookite is more electrochemically active than anatase. [9,10] Both titania particles [3,5,11,12] and films [6,[13][14][15][16] have been used in photocatalyis. Studies of the photocatalytic activity of titania particles have shown that photocatalytic activity is largely size dependent, and the optimum particle size is in the nanoparticle size range.[12] However, such nanoparticles are somewhat impractical for industrial applications because downstream nanoparticle removal processes are typically expensive.[11] Implementation of titania films in large-scale industrial processes is also difficult. Methods for circumventing the problems associated with titania photocatalysts have been suggested by several research groups. [5,[15][16][17] The preparation of macroporous and mesoporous films [15][16][17][18][19][20] and particles [21,22] has been proposed as a method to increase the effective surface area of titania photocatalysts, which would allow for increased light absorption and improve photocatalytic performance. Macroporous and mesoporous structures would presumably have a photocatalytic activity similar to nanoparticles but would not require the high maintenance costs associated with nanoparticles. However, there are some unresolved issues with the preparation and photocatalytic activity of porous photocatalysts. Heat treatment and UV irradiation of porous materials usually induces collapse of the porous structure, [16] and surfactant from the synthesis process is not always removed completely, [15] which deters photocatalytic performance. The purpose of this study was to develop a method for the preparation of macroporous titania particles and demonstrate that they have improved photocatalytic performance over nonporous titania particles. In light of recent studies, [9] ...