Nitrogen sorption at 77 K is a standard technique for the characterization
of mesoporosity, However, it seemed to be unable to detect the full, theore
tically expected pore volume in high-porosity aerogels, Investigating this
problem, we found that if only the sample is sufficiently equilibrated upon
sorption, the full pore volume is detected regardless of its porosity. As
insufficient equilibration also effects the pore size distribution deduced
from the isotherm, highly erroneous results can be avoided if complete equi
libration upon each sorption step is assured. For compliant aerogels the ef
fect of sample deformation during analysis has to be taken into account. (C
) 2001 Academic Press.