Mesoporous molecular sieves of MCM-48 type were prepared by conventional hy
drothermal and novel room temperature syntheses. Scanning electron microsco
py (SEM) studies have shown that nonagglomerated uniform spheres of size ca
. 0.5 mu m were obtained by the room temperature method. Internal pore stru
cture was studied by X-ray diffraction (XRD), transmission electron microsc
opy (TEM), and high-resolution nitrogen and argon adsorption. Pore size dis
tributions were calculated from low-temperature nitrogen and argon adsorpti
on isotherms by the nonlocal density functional theory (NLDFT) method. A no
vel approach to calculating the pore wall thickness of MCM-48 from XRD and
gas adsorption isotherms was employed. The approach utilizes intrinsic symm
etry of MCM-48 pore structure, cubic Ia3d space group, revealed by XRD and
combines the results of the pore size distribution analysis with general ge
ometrical relations between structural parameters of the gyroid minimal sur
face. The pore wall thickness of MCM-48 calculated from both nitrogen and a
rgon adsorption data was found to be ca. 8-10 Angstrom, in good agreement w
ith the estimates obtained from TEM.