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Nuclear magnetic resonance has been used to investigate relaxation in the methyl ester precursor of a perfluorocarboxylate ionomer. Whereas the findings are broadly consistent with earlier interpretations of dynamic mechanical relaxation, minor interpretative changes are indicated, principally a revision of the assignment of the 'Y relaxation peak in the DMA data. Further insight is also obtained into the way in which even quite small amounts of water can influence in an important way the overall relaxation response of the system.