Journal of Polymer Science Part A: Polymer Chemistry, Vol.39, No.19, 3239-3245, 2001
Analysis of ethylene oxide sequences of the acetal copolymer from trioxane and ethylene oxide
An NMR method for the analysis of the ethylene oxide sequence of the acetal copolymer from trioxane and ethylene oxide has not yet been established. We found three novel cyclic compounds composed of 1 mol of ethyelene oxide and 1 mol of trioxane, 2 mol of ethylene oxide and 1 mol of trioxane, and 3 mol of ethylene oxide and 1 mol of trioxane. These compounds gave only one consecutive oxyethylene unit, two consecutive oxyethylene units, and three consecutive oxyethylene units in three consecutive oxymethylene units, respectively, and gave different H-1 NMR spectra for each oxyethylene unit. Considering these data, we synthesized three polymeric model compounds that have one consecutive oxyethylene sequence, two consecutive oxyethylene sequences, and three consecutive oxyethylene sequences in an oxymethylene main chain. By a linear combination of the H-1 NMR spectrum of each oxyethylene unit of the three polymeric model compounds, we succeeded in determining the ethylene oxide sequence by the H-1 NMR method for the copolymer from trioxane and ethylene oxide. Good agreement was observed between the H-1 NMR method and the hydrolysis method for the analysis of the ethylene oxide sequences.