Degradation of 2,4-dichlorophenol (2,4-DCP) in aqueous by glow discharge electrolysis (GDE) has been investigated. Ultraviolet (UV) absorption spectra, atomic force microscopy (AFM), high performance liquid chromatography (HPLC) and gas chromatogram-mass spectrum (GOMS) are :used to monitor the degradation process and to identify the major oxidation intermediate products. It has been found that 2,4-DCP undergoes a series of intermediate step, which leads to form a number of intermediate products, mainly isomeric chlorophenols and aliphatic acids. These products are further oxidized, eventually, mineralized into CO2 and Cl-. A degradation pathway for 2,4-DCP is proposed on the basis of detection of intermediate compounds. (c) 2005 Elsevier B.V. All rights reserved.