Vol.
27 No. 6
November-December 2005
Round Robin Test on the Molecular Characterization of Epoxy Resins by Liquid Chromatography
Stepan
Podzimek
International
Journal of Polymer Analysis and Characterization
Vol. 9, No. 5-6, pp. 305-316 (2004)
DOI: 10.1080/10236660490935718
The great importance of epoxy resins originates from the wide range of applications in many industrial areas. However, only relatively primitive analytical tests are commonly used for routine characterization of epoxy resins. The simple characteristics are often unable to discriminate among different samples, to find structure versus properties relations, and to evaluate production reproducibility. Molar mass distribution of epoxy resins affects their application properties and can be also used as a sensitive measure of the reproducibility of the production.
The main objectives of this project were (i) to study the influence of experimental conditions, in particular the type and number of columns and column calibration, on the molar mass averages obtained by size exclusion chromatography (SEC), and (ii) to figure out attainable reproducibility of SEC results generated in different laboratories, and (iii) to compare SEC molar mass averages with those determined by the absolute methods. Since epoxy resins are typical examples of oligomers, most of the conclusions may be generally applicable to the analysis of other oligomers.
Two commercially available epoxy resins based on bisphenol A (2,2-bis(4-hydroxyphenyl)propane) of different molar mass distribution were selected for the Round Robin Test. The samples were characterized by vapor pressure osmometry (VPO), method of end groups (EG), multi-angle light scattering (MALS) in batch mode, and matrix assisted laser desorption ionization mass spectroscopy (MALDI-MS) to allow comparison of chromatographic results with the data from the absolute methods of molar mass determination.
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