The combination of small-angle X-ray scattering and qualitative porosimetry
is applied to the puzzling phenomenon of overly large specific surface are
as in some mesoporous silicas. Geometrical calculations, considering the re
lationship between structure, lattice parameter, and specific surface area,
reveal the latter to be at least 1 order of magnitude smaller than experim
ental values obtained from sorption experiments, indicating the presence of
micropores. Selective investigation of the mesopore system reveals that up
to 63% of the specific surface area is due to microporosity. A relationshi
p between the undirected creation of porosity and supramolecular templating
is discussed.