The influence of the processing parameters on the properties of zirconia, alumina and silica MCM-41 has been investigated. Digestion of the precursors leads to zirconia, alumina and silica MCM-41 with higher surface area and better thermal stability. The effects of digestion are attributed to increased dehydroxylation, strengthening of the network between primary particles, and to a decrease in the number of surface defects. In the case of zirconia and alumina, digestion also increased the surface acidity. This may be due to the smaller crystallites which expose low-coordinated sites at the surface. Al-MCM-41 prepared by post-synthesis grafting of aluminum is compared with MCM-41 prepared by direct incorporation of aluminum during synthesis. The surface Si/Al ratio was determined using XPS and correlated to the catalytic activity of the Al-MCM-41 for the synthesis of jasminaldehyde.