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As an increasingly important structural-characterization technique, grazing-incidence small-angle scattering (GISAXS) finds vast applications in nanostructures and nanocomposites at surfaces and interfaces for in situ and real-time studies because of its probing q-range (10-3 – 1 nm-1) and temporal resolution (10-3 – 1 s). At the Advanced Photon Source (APS), GISAXS techniques under thin-film waveguide-based resonance conditions were developed to study the diffusion phenomena in nanoparticle/polymer nanocomposites. Also, the kinematics of nanoparticle crystal formation at air/liquid interfaces has been obtained by the similar method in real time during the liquid droplet evaporation. To meet the strong demand from the nanoscience community, a dedicated GISAXS beamline has been designed and constructed as a part of the 8-ID-E beamline at the APS. This dedicated GISAXS setup was developed based on a 4-circle diffractometer so that precise reflectivity of the sample can be measured to complement the GISAXS analysis under the dynamical refection conditions. © 2007 American Institute of Physics [ABSTRACT FROM AUTHOR]