Being able to characterize colloids and surfaces is an important part of the optical field. In a given investigation, information can be required on particle size and shape, surface morphology and chemistry, phases present, as well as degree of aggregation. This chapter presents the most important analysis techniques for these applications within microscopy, light scattering and spectroscopy. A popular straightforward characterization method is microscopy. Although they cannot be used easily in all cases, microscopic techniques can be used not only for optical observations of various surfaces and particles but also for precise estimations of dimensions of colloidal particles. The two most popular techniques in this area are scanning electron microscopy (SEM) and transmission electron microscopy (TEM). One of the most popular choices of microscopy is atomic force microscopy (AFM), which is a powerful imaging and surface-force measuring technique that is well-suited for studying complex technical systems.