“…To quantify chemically the number of non-hydrogen bonded Q 3 SiOH sites per gram, we bind a probe molecule, (3,3,3-trifluoropropyl) dimethylchlorosilane (TFS), to reactive hydroxyl groups and quantify the number of attached TFS molecules with 19 F solid-state nuclear magnetic resonance (NMR) spectroscopy. The TFS molecule is an ideal probe for quantifying reactive hydroxyl groups; not only do chlorosilanes selectively attach to non-hydrogen-bonded Q 3 SiOH groups (Lochmuller and Kersey, 1988;Vandervoort et al, 1990;Kawai and Tsutsumi, 1998;Zhao and Lu, 1998;Washton et al, 2008), but each TFS molecule contains three fluorine atoms, of which the fluorine-19 isotope is NMR active and 100% abundant. To quantify the number of chemisorbed TFS molecules, 19 F magic angle spinning (MAS) NMR is utilized via a comparison of integrated peak intensities of TFS-treated samples with a 19 F-containing reference having a known concentration of spins.…”