The photocatalytic decomposition of the herbicide (4-chloro-2-methylphenoxy)acetic acid (MCPA), C9H9ClO3 in aqueous suspensions containing TiO2 was investigated by following the formation of intermediates via recording proton NMR spectra. One of theoretically possible intermediates, 4-chloro-2-methylphenolmethanoate, was synthesized by a modified esterification procedure. Based on the data obtained a possible reaction mechanism was proposed. The rate of MCPA aromatic ring decomposition was followed by pH changes during illumination. As a result, apparent reaction rate constant was found to be 7.0 x 10(-6) mol dm(-3) min(-1). The complete mineralization was attained after about 15 h of illumination. (C) 2001 Elsevier Science B.V. All rights reserved.