title: Characterization of functionalized polyolefins by high-temperature two-dimensional liquid chromatography.
abstract: High-temperature two-dimensional liquid chromatography (HT 2D-LC) was developed for the separation and characterization of functional polyolefins. Therefore, the key experimental parameters, namely the injection volume, the mobile phase composition, the flow rate in SEC and the time and phase of sampling into the second dimension, were systematically varied and their influence on the resolution of separation were studied. The HPLC separation of ethylene-vinylacetate waxes was realized using silica gel as stationary phase and a solvent gradient decalin→cyclohexanone, while SEC separations were realized in the chromatographic system polystyrene divinyl benzene column/1,2,4-trichlorobenzene. By choosing suitable experimental parameters, the run time needed for one complete 2D-LC analysis of a polymer sample was shortened from about 200 min to 100 min. However, the developed method failed to adsorb polypropylene and ethylene/1-butene copolymers grafted with 13 or 3 mol.% of methyl methacrylate respectively. Using porous graphite as a stationary phase and a solvent gradient 1-decanol→1,2,4-trichlorobenzene as mobile phase 2D-LC separations of both grafted polyolefins were realized.
authors.affiliation: Fraunhofer Institute for Structural Durability and System Reliability LBF, Division Plastics, Group Material Analytics, Schlossgartenstr. 6, 64289 Darmstadt, Germany.
authors.forename: Anton
authors.initials: A
authors.lastname: Ginzburg
authors.forename: Tibor
authors.initials: T
authors.lastname: Macko
authors.forename: Frank
authors.initials: F
authors.lastname: Malz
authors.forename: Michael
authors.initials: M
authors.lastname: Schroers
authors.forename: Irene
authors.initials: I
authors.lastname: Troetsch-Schaller
authors.forename: Jan
authors.initials: J
authors.lastname: Strittmatter
authors.forename: Robert
authors.initials: R
authors.lastname: Brüll
mesh_terms: D002850:Chromatography, Gel / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006108:Graphite / Q000737:chemistry; D006358:Hot Temperature; D011090:Polyenes / Q000737:chemistry*; D019904:Polymethyl Methacrylate / Q000737:chemistry; D011145:Polyvinyls / Q000737:chemistry
chemical_list: D011090:Polyenes; D011145:Polyvinyls; C016438:ethylenevinylacetate copolymer; D006108:Graphite; D019904:Polymethyl Methacrylate