C. Doremieuxmorin et al., STUDY OF THE CONSTITUTIVE SUPERFICIAL WATER OF PRECIPITATED AMORPHOUSSILICAS USING H-1-NMR - BROAD-LINE AT 4 K AND HR MAS AT 300, Journal of the American Chemical Society, 118(51), 1996, pp. 13040-13045
Two silicas obtained by precipitation have been compared using two TH
NMR techniques: broad-line at 4 K with simulation of the spectra and M
AS at room temperature. Previous Si-29 high resolution NMR results hav
e been used to interpret the spectra. Geminal silanols, single silanol
s. water molecules relatively strongly hydrogen-bonded to silanols, an
d water not interacting with OH groups have been characterized and qua
ntified. Differences are found between the two precipitated silicas. S
ilanols, 70% of which can hydrogen-bond a water molecule, occupy all t
he surface of one of them. The other sample surface is not so crowded
with silanols, and only 37% of them hydrogen-bond water molecules, Bot
h geminal and single silanols hydrogen-bond water. Physisorbed water m
olecules not interacting with silanols can be equilibrated on both sam
ple surfaces. Room temperature dehydration of the samples in vacuum is
studied.