In this paper, anodization of Ti foil was carried out in ethylene glycol (EG) containing 5 wt% NH4F solution and 0 to 1.5 wt% of water at 50 V for 60 min. The pH of the bath was kept constant at ~pH7. The crystal structure was studied by X-Ray Diffraction (XRD) analysis, and the morphology was observed via field emission scanning electron microscopy (FESEM). TiO2 nanotube with aspect ratio of 100 was obtained in EG containing less than 1wt % water. The nanotubes wall was very smooth. Increasing the water content > 1wt % results in short nanotubes of approximately 6.2μm with aspect ratio of 62. As anodized, nanotubes were amorphous and annealed at 400 °C promote 100 % anatase phase. Photocatalytic activity of the nanotubes produced at different water content was also evaluated by the degradation of methyl orange and the detail of the observation was discussed thoroughly in this paper.