Quantitative Characterization of Solid Epoxy Resins Using Comprehensive Two Dimensional Liquid Chromatography Coupled with Electrospray Ionization-Time of Flight Mass Spectrometry

被引:31
作者
Julka, Samir [1 ]
Cortes, Hernan [1 ]
Harfmann, Robert [1 ]
Bell, Bruce [1 ]
Schweizer-Theobaldt, Andreas [2 ]
Pursch, Matthias [2 ]
Mondello, Luigi [3 ]
Maynard, Shawn [4 ]
West, David [4 ]
机构
[1] Dow Chem Co USA, Analyt Sci, Midland, MI 48667 USA
[2] Dow Deutschland Anlagengesell mbH, Analyt Sci, Rheinmunster, Germany
[3] Univ Messina, Dipartimento Farmacochim, Fac Farm, I-98168 Messina, Italy
[4] Dow Chem Co USA, Epoxy R&D, Freeport, TX 77541 USA
关键词
HYPHENATED TECHNIQUES; SEPARATION; ADSORPTION; FUNCTIONALITY; COPOLYMERS; PROTEIN; SYSTEM;
D O I
10.1021/ac9001047
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A comprehensive multidimensional liquid chromatography system coupled to Electrospray Ionization-Mass Spectrometry (LCxLC-ESI-MS) was developed for detailed characterization and quantitation of solid epoxy resin components. The two orthogonal modes of separation selected were size exclusion chromatography (SEC) in the first dimension and liquid chromatography at critical conditions (LCCC) in the second dimension. Different components present in the solid epoxy resins were separated and quantitated for the first time based on the functional groups and molecular weight heterogeneity. Coupling LCxLC separations with mass spectrometry enabled the identification of components resolved in the two-dimensional space. Several different functional group families of compounds were separated and identified, including epoxy-epoxy and epoxy-alpha-glycol functional oligomers, and their individual molecular weight ranges were determined. Repeatability obtained ranged from 0.5% for the main product to 21% for oligomers at the 0.4% concentration level.
引用
收藏
页码:4271 / 4279
页数:9
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