A fast and specific method has been developed for the determination of hydroxyl content in prepolymers that contain hydroxymethylene functional groups. This method involves reaction of the sample with either trifluoroacetic anhydride or hexafluoroacetone to separate the terminal oxymethylene signals in the 'H NMR spectrum from those of the repeating unit and integration against an internal trinitrobenzene standard. This procedure generally requires less than 50 mg of polymer and has been employed in the analysis of prepolymers with number average molecular weights ranging up to 10000. The analysis has been tested using several different prepolymers. Precision of analysis was determined to be within 2.7 percent using a Varian XL-200 spectrometer.
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