The Nanolayered TiO2 photocatalysts were prepared by thermal treatment of metallic titanium chips. Photocatalytic activity for methyl ethyl ketone (MEK) and toluene was investigated using a closed circulating system. The photocatalysts were characterized by SEM and XRD. Surface of the Ti chips changed to be rough with increase of treatment temperature, and severe oxidation over 900 degrees C resulted in TiO2 powder. Uniform TiO2 nanolayer was formed as a rutile type on the metallic chip. Photocatalytic decomposition of MEK over the TiO2 photocatalysts occurred efficiently by UV-C irradiation. The maximum activity for MEK was obtained over Ti Chip treated at 700 degrees C. It was known that the prepared photocatalyts could be applied to remove various VOCs.