AbstractTo maximize polycarbonate (PC) stability, it is extremely important that the polycarbonate manufacturing process be operated in such a way as to minimize uncapped polymer chain‐ends. Insurance of complete end‐capping during manufacture would require constant process monitoring using a fast and accurate phenolic end‐group analysis technique for samples typically having > 5% uncapped chain‐ends. Published end‐group analysis techniques are inaccurate if the polymer samples are contaminated with monomer or other small phenolic molecules. Accuracy can be improved by purifying the polymer before analysis, but this procedure is sometimes tedious. This article describes the development of a facile gel permeation chromatography‐ultraviolet (GPC–UV) technique for quantitative determination of low levels of phenolic uncapped chain‐ends in PC. This technique improves accuracy because monomers and other small molecule impurities are separated and excluded from the PC during the analysis.