New technology is reported here for the synthesis of an effective weak acid-cation exchanger for ion chromatography. Monodisperse macroporous poly(ethylvinylbenzene-co-divinylbezene) (PEVB-DVB) beads of 5m diameter were prepared by a two-step swelling and polymerization method. Then carboxyl groups were introduced by polymerization of maleic anhydride with unreacted vinyl groups on the resin beads, followed by hydrolysis of the maleic anhydride groups. A column packed with the carboxylate beads was used to separate alkali and alkaline earth metal ions in a single isocratic run. Separations were found to be better than those with similar resin particles that are simply coated with maleic acid. The columns containing the new particles were 100% compatible with solvents commonly used for HPLC. Additionally, the prepared column was stable and could be used for a long time in a wide range of pH. The column gave good resolution, low detection limits and good repeatability for the separation of common cations. Satisfactory results were also obtained for separations of organic amines and of common cations in rainwater.