Characterization of functionalized polyolefins by high-temperature two-dimensional liquid chromatography

被引:8
作者
Ginzburg, Anton [1 ]
Macko, Tibor [1 ]
Malz, Frank [1 ]
Schroers, Michael [2 ]
Troetsch-Schaller, Irene [2 ]
Strittmatter, Jan [2 ]
Bruell, Robert [1 ]
机构
[1] Fraunhofer Inst Struct Durabil & Syst Reliabil LB, Div Plast, Grp Mat Analyt, D-64289 Darmstadt, Germany
[2] BASF SE, D-67056 Ludwigshafen, Germany
关键词
Two-dimensional liquid chromatography; Functionalized polyolefins; Porous graphite; Ethylene-vinylacetate waxes; VINYL ACETATE COPOLYMERS; CRYSTALLIZATION ANALYSIS FRACTIONATION; CHEMICAL-COMPOSITION DISTRIBUTION; ELUTION FRACTIONATION; ETHYLENE COPOLYMERS; SEC-FTIR; SEPARATION; POLYETHYLENE; CRYSTAF; TREF;
D O I
10.1016/j.chroma.2013.01.067
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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. (C) 2013 Elsevier B.V. All rights reserved.
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页码:40 / 47
页数:8
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