A new titanium(IV) oxide–hectorite nanofilm photocatalyst was prepared on quartz slides. It was evaluated in the photooxidation of dibenzothiophene (DBT) in nonpolar organic solution (tetradecane), as a model for diesel fuel. A removal regimen was developed consisting of catalytic photooxidation followed by adsorption of products on silica gel. Photooxidation of DBT was performed with and without catalyst, at 254 and 300 nm. Comparison was made with a commercially available TiO 2 catalyst, Degussa P25. The catalyst was analyzed by nitrogen adsorption, XRD, SEM, and TGA-DTA. DBT concentrations were measured by HPLC and UV spectrophotometry. Preliminary qualititative analysis of products was performed by UV and HPLC. Results indicated that the outlined process was effective in reducing sulfur levels to below 10 ppm sulfur.