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Development and validation of a fast size exclusion chromatographic method for at-line determination of the conversion of a polymerization reaction

By H. A. Lousberg, H. C. J. Hoefsloot, H. F. M. Boelens, P. Schoenmakers and A. K. Smilde

Abstract

A fast, convenient and accurate method for the determination of conversion of styrene polymerization reactions was developed and validated. Polymer samples were diluted and analyzed with size exclusion chromatography (SEC). Calibration experiments revealed that there is an excellent correlation between the conversion and the observed fractional peak area of the polymer in the chromatogram. Calibration was performed using orthogonal polynomial regression. Validation experiments showed that the predicted conversion is not sensitive to the molar mass distribution of the investigated polystyrene. Furthermore, the stability of the chromatographic system was thoroughly tested. The limit of quantification of the proposed method is approximately 0.008. The precision at higher conversion (similar to 0.30) is better than 0.003. A comparison of the SEC method with conventional gravimetry showed that this SEC method is faster, less laborious and more accurate. The total analysis time of this SEC method is about 20 min. For the gravimetric method this time is about 32

Year: 2002
DOI identifier: 10.1080/10236660214592
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Provided by: NARCIS
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