Statistically designed experiments determined which steps in the hydrothermal synthesis of TiO2 nanotubes significantly impacted the rate of photocatalytic oxidation of gas-phase methanol. This study investigated the following synthesis steps: sodium hydroxide treatment time, conductivity of the first and second washings, acid treatment time and pH, calcination temperature, and H2O2 post-treatment. The synthesis procedure produced a highly active photocatalyst; the maximum catalyst activity of the TiO2 nanotubes was approximately seven times that of the starting material, Degussa P-25. Characterization with transmission electron microscopy, X-ray diffraction, and temperature-programmed oxidation revealed that the nanotubes were 10-12 nm in diameter with an average length of approximately 100 nm.