The recent introduction of multiangle light-scattering detectors for size-exclusion chromatography has made possible the measurement of the root mean square radius of gyration (Rg) and molecular weight (M) of polymer fractions eluting from a size-exclusion chromatography column. The characterization of the dimensions of a polymer may be accomplished with only a few milligrams. The dimensions of a polyimide precursor prepared by the condensation of the meta-diethyl ester of pyromellitic dianhydride with para-phenylene diamine have been measured with this technique. The dependence of Rg on M across the distribution is compared with that predicted for a freely rotating chain, and with other similar polymers measured with hydrodynamic techniques.