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The aim of this paper is to evaluate the effectiveness of photocatalytic treatment with titanium dioxide in the degradation of 44 organic pesticides analyzed systematically in the Ebro river basin (Spain). The effect of the addition of hydrogen peroxide in this treatment is studied, and a monitoring of effectiveness of photocatalytic processes is carried out by measurements of physical-chemical parameters of water. The application of photocatalytic treatment with 1 g L−1 of TiO2 during 30 minutes achieves an average degradation of the studied pesticides of 48%. Chlorine demand, toxicity, and dissolved organic carbon (DOC) concentration of water are reduced. If hydrogen peroxide is added with a concentration of 10 mM, the average degradation of pesticides increases up to 57%, although chlorine demand and toxicity of water increase while DOC concentration remains unchanged with this treatment. The application of either photocatalytic treatments does not produce variations in the physical-chemical parameters of water, such as pH, conductivity, colour, dissolved oxygen, and hardness. The pesticides which are best degraded by photocatalytic treatments are parathion methyl, chlorpyrifos, α-endosulphan, 3,4-dichloroaniline, 4-isopropylaniline, and dicofol while the worst degraded are HCHs, endosulphan-sulphate, heptachlors epoxide, and 4,4′-dichlorobenzophenone.