Poly(acrylate)s as well as poly(methaerylate)s were successfully synthesized via reversible addition-fragmentation chain-transfer (RAFT) polymerizations using 2-cyano-2-butyl dithiobenzoate (CBDB) as RAFT-agent. Four different ratios of RAFT to initiator were screened for four acrylates and four methacrylates using automated parallel synthesizer robots. The reactions were monitored by gel permeation chromatography (GPC) and gas chromatography (GC). The knowledge obtained during this screening was used for the designed synthesis of block and random copolymers containing a water- and a non water-soluble monomer. The results obtained from GPC analysis together with H-1 NMR spectroscopy demonstrate the possibility to design and prepare well-defined block and random copolymers. (c) 2005 Wiley Periodicals, Inc.