The development of high-throughput liquid chromatographic techniques for the analysis of styrene-butyl acrylate (SBA) copolymers is discussed. The analysis time in size-exclusion chromatography (SEC) can be reduced to about 3 min per sample when high-throughput SEC columns and high flow rates are used. In gradient HPLC, small columns with improved separation efficiencies can be applied. The time requirements can be decreased to less than 2 min per sample. Using the high-throughput HPLC technique, the chemical composition distribution of high-conversion SBA copolymers can be analyzed in a fast and efficient way. The calibration of HPLC separation is conducted by coupling the HPLC system with FTIR through the LC-transform interface. A comparison of the chemical compositions of the copolymers obtained by 1H NMR, off-line FTIR and coupled HPLCFTIR verifies the accuracy of the high-throughput copolymer analysis approach.

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.

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