Treated silica xerogels with controlled porosity and surface area were prep
ared by the in situ treatment of hydrogels with hexamethyldisiloxane or alk
ylchlorosilanes in the presence of isopropyl alcohol. The resulting hydroge
ls were hydrophobic and readily transferred to nonpolar organic solvents up
on contact. The surface area and porosity of the xerogel were controlled by
varying the pH, time, and temperature used to polymerize the hydrogel prio
r to treatment. In general, the surface area decreased with increases in ag
ing time or temperature, whereas the total pore volume and pore size increa
sed. Silylation of the hydrogel in the aqueous phase retains the structure
of the hydrogel and permits isolation with minimum structure collapse. By u
sing this technique, silylated xerogels with surface areas ranging from 200
to >700 m(2)/g and pore volumes of 1.5 to 3.8 cm(3)/g were obtained.