Solid-state 13C NMR and SAXS characterization of the amorphous phase in low-molecular weight poly(ethylene oxide)s

Low-molecular weight poly(ethylene oxide)s (PEO) with extended, once or twice folded chains (as characterized by SAXS), were investigated by solid-state 13C NMR spectra measured under conditions to detect only the signal of the narrow line component. The direct detection and integrated intensities of the signals from hydroxy-terminated chain-end units in these spectra confirm that the narrow line component corresponds to the noncrystalline (amorphous) phase. The NMR line of PEO carbons adjacent to the hydroxy end-groups was used as an intensity standard to obtain information on the mean number of carbons per chain contributing to the amorphous phase. Assuming that amorphous phase is formed by chain ends (cilia) and folds it follows from the spectra that the length of folds is 6–7 monomer units; cilia are 2–3 monomer units long.