The influence of added short-chain amines, n-butylamine, BA, and n-octylami
ne, OA, on the mesophase formation of surfactant-silicate composite structu
res in a room-temperature synthesis has been investigated in situ by synchr
otron small-angle X-ray scattering. For BA a marked decrease in the d spaci
ng of the hexagonal phase was observed with increasing amine concentration,
while a slight increase in d spacing was initially observed for OA. Howeve
r, the d spacing of the hexagonal phase went through a maximum with increas
ing concentration. Furthermore, two coexisting hexagonal phases or a purely
lamellar phase was observed if the concentration of OA was increased furth
er. The results are discussed in terms of two competing mechanisms of amine
incorporation: solubilization within the CTAB-silicate mesophase and compe
titive adsorption of the amine to the silicate.