In the current work, TiO 2 /Al 2 O 3 binary oxide photocatalysts were synthesized via two different sol-gel protocols (P1 and P2), where various TiO 2 to Al 2 O 3 mole ratios (0.5 and 1.0) and calcination temperatures (150-1000 • C) were utilized in the synthesis. Structural characterization of the synthesized binary oxide photocatalysts was also performed via BET surface area analysis, X-ray diffraction (XRD) and Raman spectroscopy. The photocatalytic NO(g) oxidation performances of these binary oxides were measured under UVA irradiation in a comparative fashion to that of a Degussa P25 industrial benchmark. TiO 2 /Al 2 O 3 binary oxide photocatalysts demonstrate a novel approach which is essentially a fusion of NSR (NO x storage reduction) and PCO (photocatalytic oxidation) technologies. In this approach, rather than attempting to perform complete NO x reduction, NO(g) is oxidized on a photocatalyst surface and stored in the solid state. Current results suggest that alumina domains can be utilized as active NO x capturing sites that can significantly eliminate the release of toxic NO 2 (g) into the atmosphere. Using either (P1) or (P2) protocols, structurally different binary oxide systems can be synthesized enabling much superior photocatalytic total NO x removal (i.e. up to 176% higher) than Degussa P25. Furthermore, such binary oxides can also simultaneously decrease the toxic NO 2 (g) emission to the atmosphere by 75% with respect to that of Degussa P25. There is a complex interplay between calcination temperature, crystal structure, composition and specific surface area, which dictate the ultimate photocatalytic activity in a coordinative manner. Two structurally different photocatalysts prepared via different preparation protocols reveal comparably high photocatalytic activities implying that the active sites responsible for the photocatalytic NO(g) oxidation and storage have a non-trivial nature.