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Gel permeation and thin-layer chromatographic characterization and solution properties of butadiene and styrene homopolymers and copolymers

Authors

  • James L. White,

    1. Department of Chemical and Metallurgical Engineering, University of Tennessee, Knoxville, Tennessee 37916
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  • David G. Salladay,

    1. Department of Chemical and Metallurgical Engineering, University of Tennessee, Knoxville, Tennessee 37916
    Current affiliation:
    1. Amoco, Decatur, Alabama
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  • David O. Quisenberry,

    1. Department of Chemical and Metallurgical Engineering, University of Tennessee, Knoxville, Tennessee 37916
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  • Donald L. MacLean

    1. Department of Chemical and Metallurgical Engineering, University of Tennessee, Knoxville, Tennessee 37916
    Current affiliation:
    1. Monsanto Company, Chemstrand Research Center, Durham, North Carolina
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Abstract

Gel permeation chromatographic (GPC) and thin-layer chromatographic (TLC) studies of polystyrene, polybutadienes (BR), and their copolymers (SBR) have been carried out. GPC primarily separates them on the basis of molecular size, and TLC, on the basis of composition. Methods of obtaining absolute molecular weight distributions for BR and SBR based upon variations of the Strasbourg Universal Calibration procedure are described. In particular, [η]–M relationships in both the GPC solvent (THF) and in a second solvent (toluene) were used; in addition, results of statistical mechanical calculations for equation image (based on the assumption of negligible steric hindrance and freely rotating bonds) were applied. An experimental comparison of these methods was carried out, and use of the [η]–M relationships for both solvents was found to give satisfactory results. The predictions of the statistical theory were too low. A detailed study of polymer–solvent–gel interaction in the GPC unit was made through investigation of ternary phase equilibrium in the (polystyrene)–THF–(polymer) system. The polymers studied included BR and SBR with varying styrene contents. Experimental techniques for TLC separations of BR, SBR, and polystyrene according to the composition are described.

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