Small angle X-ray scattering experiments have been performed to study the microstructure of messoporous silica meterials prepared by condensation of tetraethylorthosilicate using nonionic alkylpolyethyleneoxide(AEO9) and ionic cetyltrimethylammonium bromide (CTAB) surfactant as templates.It is the pores within the nanometre range that produce the main cattering.The scattering of the pure silica systems obey Porod’s law.This may be because the templates produce some additional scattering background and then make the scattering of pores distorted.The results show that the full removal of templates from the pores of the materials by Soxhlet extraction is very easy for AEO9,but it is difficult for CTAB.The positive deviation correction is also perfromed.