Thermal evacuation of a surfactant template from pure siliceous MCM-41 and MCM-41 containing aluminium in hydrogen flow was
investigated. Micelle templated MCM-41 were prepared using hexadecyltrimethylammonium bromide (CTAB). The products of thermal
surfactant degradation outside and inside pores were identified at various temperatures using 13C solid-state nuclear magnetic resonance (NMR) spectroscopy, gas chromatography coupled with mass spectrometer (GC-MS) and
temperature programmed desorption coupled with mass spectrometer (TPD-MS). The GC-MS and 13C MAS NMR results obtained from this study provide an insight into the mechanism of surfactant transformation during MCM-41
synthesis on molecular level.