Polyamide nanocomposite films were prepared from nanometer sized silica particles and trimesoyl chloride–m-phenylene diamine based polyamides. The type of silica nanoparticles used is commercial LUDOX® HS-40 and the particle size characterized by the radius of gyration (R_g) is about 66 Å. The immediately prepared films were easily broken into particles to form colloidal-like dilute suspension of the silica–polyamide composite particles in D₂O–H₂O solutions for SANS measurements, that in this dilute system SANS data the complication of scattering data from the interacting particles is minimized. At about 60% D₂O of the sample solution, the silica is contrasted out, therefore the SANS profiles are predominantly from the organic polyamide scattering. The SANS profile of the sample solutions measured at 90% D₂O clearly indicates scattering from both silica and polymer. The scattering heterogeneities for two-phase system were evident from the validity of the Debye–Bueche expression in case of the nanocomposite with high silica loading. At limited silica loading of the nanocomposite, interaction between the silica and polymer chains forming core–shell morphology was observed. The transport properties of the membranes made from the nanocomposite films were measured on a batch type test kit with an aqueous solution of 500 ppm dioxane concentration at pressures ranging from 50 to 200 psig, and correlated to their composite structure.