The electrochemical degradation of methylparathion has been investigated by using Ti/Pt as anode, Stainless Steel 304 as cathode, and sodium chloride as electrolyte. The pesticide is rapidly degraded, but full mineralization is not observed. Degradation products have been monitored through gas chromatography and mass spectrometry, and the overall degradation process has been monitored through dissolved and particulate organic carbon, sulfur, and phosphorus measurements. Several intermediates have been identified, and oxalic, formic, and acetic acids as well as tetraphosphorus trisulfide have been recognized as final products of the degradation process. A proposed mechanism of the process is presented.