Abstract: | Solid‐state NMR characterization of hybrid aluminosilicate xerogels, by 17O magic angle spinning (MAS) and triple quantum magic angle spinning (MQMAS) techniques, evidences Si—O—Si and Si—O—Al oxygen sites, spectrally separated in MQMAS experiments. Inversion of the MQMAS spectra allows the measurement of quadrupolar parameters, isotropic chemical shifts, distribution of chemical shift and discussion of the mobility of the structural units. Copyright © 2003 John Wiley & Sons, Ltd. |