Automotive catalysts generally lose-agtivity during vehicle operation due to several well-known deactivation mechanisms. To gain a more fundamental understanding of catalyst deactivation, the microscopic details of fresh and vehicle-aged commercial pelleted automotive exhaust catalysts containing Pt, Pd and Rh were studied by employing Analytical Electron Microscopy (AEM). Two different vehicle-aged samples containing similar poison levels but having different catalytic activities (denoted better and poorer) were selected for this study.The general microstructure of the supports and the noble metal particles of the two catalysts looks similar; the noble metal particles were generally found to be spherical and often faceted. However, the average noble metal particle size on the poorer catalyst (21 nm) was larger than that on the better catalyst (16 nm). These sizes represent a significant increase over that found on the fresh catalyst (8 nm). The activity of these catalysts decreases as the observed particle size increases.