A combinatorial approach was developed for the synthesis and the screening of a large variety of conjugated polymers. The parallel synthesis of 96 polyaryleneethynylene derivatives was performed on a 12 x 8 format from diethynyl and dibromoaryl building blocks, via a palladium-catalyzed carbon-carbon coupling reaction. The qualitative distinction between fluorescent and nonfluorescent polymers as well as between the different emission colors were obtained from a simple visual test or via a 96-well plate reader spectrofluorimeter. New solid-state blue-emitting polymers were detected.