The repetitive discoloration kinetics of the azo-dye Methyl Orange (taken as a model organic compound) was followed under solar simulated radiation (90 mW/cm 2 ) to assess the performance of the TiO 2 /Tedlar ® composite photocatalyst. The influence of solution parameters on the photo-discoloration process: pH, dye concentration, applied light intensity and concentration of H 2 O 2 were systematically investigated. During the photocatalysis a modification occurs in the TiO 2 /Tedlar ® composite due to the TiO 2 interaction with the Tedlar ® film. Physical insight is given for the stabilization mechanism of the TiO 2 particles in the Tedlar matrix based on the data obtained by X-ray photoelectron spectroscopy (XPS). The F 1s peak of the Tedlar film indicates that the TiO 2 is loaded on the Tedlar fluoro-groups. The loading of TiO 2 on the 75 m thick Tedlar ® film was ∼0.9% (w/w) as determined by atomic absorption spectrophotometry (AAS). Attenuated total reflection infrared spectroscopy (ATRIR) shows no formation of additional bands within the photodiscoloration reaction. This shows that an efficient catalysis taking place on the TiO 2 /Tedlar ® surface. The rugosity (mean square roughness, rms) of the TiO 2 /Tedlar ® film was determined by atomic force microscopy (AFM) to be 19.7 nm. This value remained constant during long-term operation. Transmission electron microscopy (TEM) reports the thickness and coverage of TiO 2 Degussa P-25 on the Tedlar ® surface before and after photocatalysis.