Organizations & People
Title: Round Robin Test on the Molecular Characterization of
Epoxy Resins by Liquid Chromatography
Chairman: 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.
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)
Last update: 21 July 2005
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