This article describes the photolytic and photocatalytic removal of the insecticide methomyl at low concentration from different types of water, upon UV, visible or natural solar light radiation, in the presence of TiO2 and ZnO, as well as using Fe-ZSM-5 zeolite and AlFe-pillared montmorillonite (photo-Fenton process). The rate of photodecomposition of methomyl was measured using UV spectrometry and HPLC, while its mineralization was investigated by ion chromatography (IC) and total organic carbon (TOC) analysis. The photochemical removal of methomyl is a natural and applicable model for the purification of water.