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Fractionation of ethylene/1‐pentene copolymers using a combination of SEC‐FTIR and SEC‐HPer DSC
Authors:Nyambeni Luruli  Thijs Pijpers  Robert Brüll  Valérie Grumel  Harald Pasch  Vincent Mathot
Institution:1. Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, 7602 Matieland, South AfricaDepartment of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, 7602 Matieland, South Africa;2. Laboratory of Macromolecular Structural Chemistry, Division of Molecular and Nanomaterials, Department of Chemistry, Katholieke Universiteit Leuven, Celestijnenlaan 200F, 3001 Heverlee, Belgium;3. Deutsches Kunststoff‐Institut (German Institute for Polymers), Schlo?gartenstr. 6, 64289 Darmstadt, Germany;4. Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, 7602 Matieland, South Africa;5. SciTe, Ridder Vosstraat 6, 6162 AX Geleen. The Netherlands
Abstract:The short chain branching distribution (SCBD) and thermal properties of ethylene/1‐pentene copolymers were studied using SEC‐FTIR and SEC‐HPer DSC. The copolymers, synthesized with Cp2ZrCl2/MAO, were fractionated using size exclusion chromatography (SEC). The infrared analysis of the fractions showed that the copolymers had—on average—higher 1‐pentene concentration in the low molecular weight range. Furthermore, the thermal properties of the SEC deposits of these copolymers on a Germanium disc were studied using high performance differential scanning calorimetry (HPer DSC). Single SEC separations were used to accumulate fractions in the microgram range that were directly analyzed with regard to their thermal properties, thus allowing us to study SCBD as well as thermal behavior simultaneously. When these fractions (with masses ranging from 10–80 μg) were analyzed using HPer DSC, good melting and crystallization temperature distributions were obtained, proving that HPer DSC can be used as a complementary method to SEC‐FTIR. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 2956–2965, 2007
Keywords:catalysis  copolymerization  ethylene/1‐pentene copolymers  fractionation of polymers  high performance differential scanning calorimetry (HPer DSC)  melting and crystallization temperatures  SEC‐FTIR  short chain branching distribution  thermal properties
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