An experimental work in a well-stirred batch recycling reactor for the photo-Fenton degradation of atrazine in water is presented. A study of the quantum efficiency is performed to assess the effectiveness of the photo-Fenton process on the atrazine degradation and total organic carbon (TOC) mineralization. Apparent and absolute quantum efficiencies of degradation and mineralization of an atrazine-based commercial herbicide are determined under different experimental conditions. Higher apparent efficiencies were found for both atrazine degradation and TOC mineralization when the ferric ion and hydrogen peroxide concentrations are increased. Because of the well known stability of the triazine ring, atrazine was not completely mineralized by the photo-Fenton process. However, a TOC reduction of 40% was achieved, being 62.5% of the maximum value that can be reached.