Experimental protocols aiming at the characterisation of glass transition often suffer from ambiguity. The ambition of the present study is to describe the glass transition in a complex, micro heterogeneous system, the dry rice pasta, in a most unambiguous manner, minimising the influence of technique-specific bias. To this end, we apply an unprecedented combination of experimental techniques. Apart from the usually used NMR and DSC, we employ, in a concurrent manner, neutron transmission, diffraction, and Compton scattering. This enables us to investigate the glass transition over a range of spatio-temporal scales that stretches over seven orders of magnitude. The results obtained by neutron diffraction and DSC reveal that dry rice pasta is almost entirely amorphous. Moreover, the glass transition is evidenced by neutron transmission and diffraction data and manifested as a significant decrease of the average sample number density in the temperature range between 40 and 60 °C. At the microscopic level, our NMR, neutron transmission and Compton scattering results provide evidence of changes in the secondary structure of the starch within the dry rice pasta accompanying the glass transition, whereby the long-range order provided by the polymer structure within the starch present in the dry rice pasta is partially lost.
Keywords: DSC; NMR relaxation; average functional group approximation; glass transition; neutron Compton scattering; neutron diffraction; neutron transmission.