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Synthesis and characterization of random copolymers by spectroscopic and chromatographic techniques are normally slow and expensive because most measurements are conducted consecutively and no high-throughput techniques are used. In the present work parallel synthesis and high-throughput analytical techniques for random styrene-ethyl acrylate copolymers were developed. With combinatorial methods, high-throughput instruments and a better design of experiments, the molar mass and chemical composition analyses were carried out simultaneously with time savings of more than 90% as compared to conventional set-ups. The chemical heterogeneity of high-conversion styrene-ethyl acrylate copolymers was determined successfully by fast gradient HPLC. Determination of the average composition was carried out via selective UV detection in size exclusion chromatography. The results were verified by  1 H NMR and calculations based on the copolymerisation parameters. Differential scanning calorimetry and optical microscopy techniques were used for determination of the phase separation behaviour of the copolymers and correlated with the chemical heterogeneity.

Determination of chemical composition and molar mass distribution of random styrene-ethyl acrylate copolymers by high-throughput liquid chromatography