Nitrogen adsorption at -195 degrees C serves as routine method for the
measurement of surface area of porous materials derived by sol-gel pr
ocedures. In a systematic study of the simultaneous effect of the pH a
nd water-silane ratio of the starting solutions of preparation of SiO2
xerogels on their surface areas, it was found that conditions of high
acidity and low water/silane ratio result in microporous materials, t
he surface of which cannot be accessed by N-2 at -195 degrees C, withi
n a realistic time scale, but only by CO2 at 0 degrees C. In a typical
result for TMOS/water/methanol = 1/2/3 at pH = 1.0, the apparent N-2-
area was zero, while the CO2-area was 414 m(2)/gr. It is recommended t
o recheck apparent N-2-low surface areas of sol-gel materials by CO2 a
dsorption. The behavior of pyrene-doped xerogels of this type is in ag
reement with the structural characterization by adsorption.