A new method for the determination of the herbicide diuron, using a flow injection manifold and photoinduced chemiluminescence detection, is presented. The pesticide, in basic medium, was irradiated on-line with UV light (254 nm) for 53 s. A short discussion about the possible irradiation products is included. The chemiluminescent response of the photoproducts was induced by oxidation with potassium ferricyanide in phosphate buffer at pH 11.5. The method permitted the quantification of diuron over the 0.1 -4.0 mg L -1 range, with a detection limit (S/N = 3) of 20 μg L -1 when the method was applied directly. However, the use of solid phase extraction (SPE) performed with C18 cartridges allowed us to achieve a limit of detection of 0.4 μg L -1 and a 1.5 -30 μg L -1 dynamic range. The method was successfully applied to the diuron determination in samples of water from different sources (spring, ground, mineral, irrigation, sea and tap waters) with a low consumption of reagents.