High-throughput (HT) experimentation in heterogeneous catalysis exemplifies a multidisciplinary approach to address in an efficient manner different aspects of catalyst development - from synthesis to testing and characterization. The present work reports on preparation systems for rapid parallel synthesis of well defined heterogeneous catalysts and catalyst screening in olefin metathesis. Metathesis of ethene and but-2-ene to propene was chosen as a test reaction. The influences of various parameters such as rhenium oxide loading, catalyst calcination conditions, catalyst pre-treatment, as well as the reaction temperature and contact time on the catalytic performance are discussed. Sample characterization by UV-vis and FT-IR gave an evidence for the formation of active surface perrhenate species, very sensitive to humidity and pre-treatment conditions applied. (c) 2008 Elsevier B. V. All rights reserved.