Useful NMR solvent mixture for polyesters: Trifluoroacetic acid-d/chloroform-d

Summary

NMR spectra of high molecular weight polyesters such as polyglycolide (PG) and poly(ethylene terephthalate) (PET) have not been available because of low solubility in suitable NMR solvents. Although PG is not soluble enough at ambient temperatures for NMR spectra in either chloroform-d or trifluoroacetic acid-d alone, it dissolves readily to over 0.9% in a mixture of the two. At this concentration, ¹H and ¹³C spectra can be obtained on samples where end group signals are visible from which molecular weights can readily be determined. The solutions are stable up to at least four days when moisture is excluded. NMR spectra of PET can likewise be obtained at ambient temperatures in the solvent mixture which dissolves up to at least 0.6% of PET.