The formation of silica-surfactant mesophases that are precursors to the mesoporous materials MCM-41 and FSM-16 were followed in real time using a synchrotron X-ray facility developed by our research group at the Daresbury SRS, UK. The facility has been designed to record powder diffraction data of the phases as they form in situ, from solns., gels or via intercalation processes. The technique is a direct method of following the formation processes and can therefore provide a means of elucidating the mechanisms involved. A wide range of temps. and hydrothermal conditions are possible. The prepn. of Keggin cluster tungsten (VI) oxide and molybdenum (VI) oxide mesophases using quaternary ammonium salts, altered pH and ammonium metatungstate or molybdate resp. produced lamellar and hexagonal phases that could be obsd. using this technique. A review of the study will be presented. [on SciFinder(R)]