Anionic polymerization techniques have been implemented successfully in a commercial automated synthesizer. The main problems for a successful adaptation of the experimental technique in the automated synthesizer are addressed, as well as some simple potential applications, such as the anionic polymerization of styrene, isoprene, and methyl methacrylate. The obtained results were reproducible and in concordance with literature knowledge. The apparent rate constant of the anionic polymerization of styrene in cyclohexane initiated by sec-butyllithium could be determined at two different concentrations of the monomer and initiator in a temperature range of 10-60 degrees C. All the synthesis and characterization experiments of the polymers were performed within a short time period. Moreover, the syntheses of poly (styrene-b-isoprene) and poly(styrene-b-methyl methacrylate) block copolymers were also successfully carried out within the automated synthesizer. (c) 2005 Wiley Periodicals, Inc.