Solid State ¹³C Nuclear Magnetic Resonance Study of Morphology and Molecular Mobility in Quenched Poly(3-hydroxybutyrate)

Single pulse magic angle spinning ¹³C NMR spectra and the carbon spin-lattice relaxation times T₁(¹³C) were used for the study of morphology and molecular mobility in poly(3-hydroxybutyrate) quenched in cold water after melting in a twin-screw extruder. The crystallinity of the quenched sample was found to be comparable with that of virgin material, and the decrease in dimensions of the crystallites grown after quenching was deduced from the single pulse magic angle spinning ¹³C NMR spectra. The spin-lattice relaxation curves for the carbons of the CO, CH, CH₂ and CH₃ groups were found to be bi-exponential, which enables the molecular mobility within crystalline and amorphous domains to be studied. The spin-lattice relaxation times T₁(¹³C) estimated for the carbons of the CO, CH, CH₂ groups show the chain mobility enhancement within crystalline domains of the quenched sample, but the influence of the quenching on the CH₃ group rotation and on the main chain motion within amorphous regions was not observed