Jv. Oglesby et Jf. Stebbins, Si-29 CPMAS NMR investigations of silanol-group minerals and hydrous aluminosilicate glasses, AM MINERAL, 85(5-6), 2000, pp. 722-731
One-pulse magic angle spinning (MAS) Si-29 and H-1-Si-29 cross-polarization
(CP) MAS nuclear magnetic resonance (NMR) spectroscopy was performed on mi
nerals with OH groups and on hydrous aluminosilicate glass samples. The sil
anol-group samples used were krauskopfite, rosenhahnite, thaumasite, ussing
ite, and KHSi2O5 with known Si to H distances and ellenbergerite, the proto
n positions of which are not as well defined. The Si-H distances from the m
inerals can he compared with the cross-polarization time constants (tau(S,H
)) and the proton spin-relaxation times in the rotating frame [tau(1p)(H)],
and a rough correspondence exists between a mineral's shortest Si-H distan
ce and its rsi, value. Also, fast [tau(1p)(H)] values correspond to large b
ulk Ii densities. The CP spectra of the hydrous aluminosilicate glass sampl
es were fitted with two peaks, representing two different Si environments w
ithin the glass structure. The contact-time curves of the higher frequency
peak imply tau(SiH) similar to the mineral samples with short Si-H distance
s, and this suggests that the glasses could contain a large fraction of eit
her Si-OH groups or protonated bridging O atoms.