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Macromolecular Division (IV)


Number: 1999-021-1-400

Title: Round Robin Test on the Molecular Characterization of Epoxy Resins by Liquid Chromatography

Task Group
S. Podzimek

Members: D. Berek, J. Chmelik, S. Clarke, Z. Dobkowski, S. Fugmann, H. Geerts, D. Held, A. Herod, H. Jordi, M. Kaska, S. Kok, N. Marheineke, S. Matsuyama, E. Meehan, P. Mena, J. Minnee, M. Netopilik, T.Q. Nguyen, H.J.A. Philipsen, J. Pulda, S. Rumbelow, G. Saunders, H. Tomizawa, G. Verreyt, and M. Zigon

Completion Date: 2005 - project completed

Standardization of the experimental conditions for the characterization of epoxy resins based on bisphenol A by liquid chromatography.

The broad interest in epoxy resins originates from the extremely wide range of applications in many important industrial areas. So far only relatively primitive analytical tests are used for routine characterization of epoxy resins. The simple characteristics are often unable to discriminate between different samples and to find structure vs. properties relations. Liquid-chromatographic characterization of epoxy resins has been reported in the literature, but no standard procedure has been established yet. Molar mass distribution of epoxy resins affects their application properties and can be used as a sensitive measure of the reproducibility of the manufacture. Two different samples of solid bisphenol A based epoxy resins are intended to be analysed by conventional size exclusion chromatography (SEC), SEC coupled with a light scattering detector or a viscometer and high performance liquid chromatography (HPLC). The project should show the influence of the experimental conditions, namely the type and number of SEC columns and column calibration on the molar mass averages, and type of HPLC column and mobile phase composition on the resolution of epoxy oligomers. The samples shall be analysed by the above mentioned techniques in two rounds. In the first one the participants will be free to choose experimental conditions, in the second one the recommendation of experimental conditions will be provided based on the data from the first round robin test. The information obtained during the test should result in establishment of appropriate experimental conditions for the analysis of bisphenol A based epoxies by SEC and HPLC. Participants can choose only one of the mentioned chromatographic techniques or to employ more of them.

Till Feb 2002, 26 scientists from 23 organizations joined the project. Some of them have already measured and sent the results, some just asked for samples expressing interest to measure. Most participants used conventional SEC with column calibration. However, several scientists applied light scattering or viscometric detectors as well. Only one participant employed gradient elution reversed phase chromatography. In addition, the samples have been carefully measured by vapor phase osmometry, method of end groups, and static light scattering to allow comparison of chromatographic results with the data from the absolute methods of molar mass determination.

Preliminary results were presented during the 16th Bratislava International Meeting on Polymers, see: "Repeatability and apparent Reproducibility of Molar Mass Values for Commercial Polymers Determined with Size Exclusion Chromatography", by D. Berek, R. Bruessau, D. Lilge, I. Mingozzi, S. Podzimek, E. Robert, Proc. 16th International Bratislava Meeting on Polymers, Coupled, Hyphenated and Multidimensional Liquid Chromatographic Procedures for Separation of Macromolecules, Bratislava, Sept 9-13, 2001, p. 57.

As of Feb 2004, all 17 participants who worked under freely chosen experimental conditions analyzed two bisphenol A based epoxy resins by means of SEC. Some of the participants used more types of detection and/or column sets. The obtained results were statistically evaluated and compared with the data from the absolute methods of molar mass determination, namely vapor pressure osmometry, end group analysis, light scattering, and matrix assisted laser desorption ionization mass spectroscopy. The presentation of the results and their discussion as well as some general remarks on the characterization of oligomers shall be given at the 17th ISPAC Meeting (Heidelberg, 6-9 June 2004). The final publication will be submitted to the International Journal of Polymer Analysis and Characterization, Vol 9, No 5-6, pp. 305-316 (2004)
DOI 10.1080/10236660490935718

Project completed

Last update: 21 July 2005

<project announcement published in Chem. Int. 22(5) 2000>


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