1,2-Dicarboxyethyl-terminated polystyrenes were synthesized by anionic polymerization of styrene initiated by sec-butyllithium, followed by reaction with dimethyl maleate, basic hydrolysis of the ester groups, acidification, and neutralization with sodium hydroxide. The polymers were characterized by size-exclusion chromatography (SEC), Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR), acid-base titration, and light scattering. SEC indicated the absence of undesired coupling reaction as well as the absence of polymerization of dimethyl maleate. FTIR showed that the hydrolysis and the neutralization were complete. The functionality of the polymers was found to be very close to 2 by NMR spectroscopy and acid-base titration. A sodium-neutralized dicarboxylate-terminated polystyrene was found by light scattering measurements to form reverse micelles in cyclohexane, which have an aggregation number of ca. 20 and extremely low critical micelle concentration (cmc), by contrast to a monocarboxylate-terminated polystyrene, which gave an aggregation number of ca. 12 and a cme of ca. 10(-5) M. When dimethyl fumarate was used instead of dimethyl maleate, side reactions occurred and only a low functionality was obtained.