High-speed experimentation (HSE) techniques are newly developed methods that, allowing the fast preparation and analysis of large numbers of parallel experiments, enable to screen an extensive parameter space. These techniques are particularly useful to investigate chemical systems for which a precise knowledge of the overall reaction or formation mechanism is not available. Here, we report the application of HSE techniques to the study of the synthesis of two families of siloxane compounds: zeolites and silsesquioxanes. Zeolites are well known crystalline microporous materials with broad applications as heterogeneous catalysts. Silsesquioxanes are small, discrete siloxane cages used both as homogeneous catalysts and as model compounds for silica surfaces and zeolites. With our HSE approach we were able to investigate the synthesis of alummium-rich zeolite beta (Si/Al ratio from 2.5 to 5) and to identify a new and fast way to synthesise silsesquioxane precursors for Ti-catalysts active in the epoxidation of alkenes. (C) 2002 Elsevier Science B.V. All rights reserved.