Anatase TiO₂ has attracted a lot of attention due to its applications as a photocatalyst in water and air treatment technologies. However, its large band gap energy (⁓3.2 eV) limits its application only to UV light. Also, anatase TiO₂ suffers from high electron/hole recombination, which diminishes its photocatalytic activity. Therefore, different methods have been employed to decrease its band gap energy and reduce the recombination of the charge carriers. One of the methods is to incorporate impurities as dopants in its crystal lattice. Different metal and non-metal dopants have been studied for this aim. Among the different choices, Fe³⁺ has showed a great potential to improve the photocatalytic activity of TiO₂ under visible light irradiation. Firstly, the d orbitals of Fe³⁺ interact with the 3d orbitals of Ti⁴⁺ generating intermediate band gap energy levels to facilitate excitation of electrons under visible light by a red shift in the absorption of light. Secondly, Fe³⁺ can interact with both electrons and holes to produce Fe²⁺ and Fe⁴⁺ trapping the charge carriers and reducing their recombination rate. Fe²⁺ and Fe⁴⁺ can release the electron and hole and revert back to the Fe³⁺. The released charge carriers migrate to the surface of the nanoparticles to initiate the photocatalytic reactions. However, it was found that the photocatalytic activity of Fe-TiO₂ is not as high as expected. Therefore, in this research study I investigated the cause for its low photocatalytic activity and found methods to improve it. The Fe-TiO₂ was synthesized using a facile sol-gel method and its structure and properties were characterized by different instrumental techniques. Using TEM and HRTEM an amorphous layer was seen on the surface of the nanoparticles. This layer characterized using XPS and EDX was composed of iron oxide layers. This layer was contaminating the surface of the nanoparticles where the photocatalytic reactions take place. Moreover, the contamination layer was acting as a recombination center for the electrons and holes. To the best of our knowledge, no previous study was conducted to investigate the effect of an iron oxide contamination layer on the photocatalytic activity of Fe-TiO₂ nanoparticles. This layer was removed using a concentrated HCl solution confirmed using HRTEM and XPS. Also, using DRS it was shown that its removal does not effect the optical properties of the Fe-TiO₂ confirming that the acid treatment process did not influence the doped Fe³⁺ in the TiO₂ crystal lattice. The degradation of methelyne orange (MO), a representative pollutant, was increased from 25% to 98% under visible light irradiation. Also, in order to achieve the highest performance of the photocatalyst, it was necessary to study the parameters of the photocatalytic activity and the degradation efficiency. Therefore, experiments using a phenol solution, another representative pollutant, were conducted to investigate and optimize the effects of the catalyst load, reaction time, initial concentrating of the pollutant and pH. The degradation efficiency of the phenol solution was found to increase from 31% to 57% by the removal of the contamination layer and by controlling the pH of the solution.