Insights into the microstructure and interconnectivity of porosity in porous starch by hyperpolarized 129Xe NMR

Abstract

For the first time, hyperpolarized (HP) ¹²⁹Xe NMR measurements are utilized to explore porous structures of porous starch (PS) successfully. Some micropores resided inside the mesopore walls of PS were detected by variable temperature (VT) HP ¹²⁹Xe NMR, and the pore sizes of micropores were also estimated using the empirical relationship. Furthermore, the interconnectivity of pores was investigated in detail by two-dimensional (2D) exchange spectroscopy (EXSY). The exchange process of xenon from microporosity within pore walls to the free gas space was occurred at the mixing time of ≥12 ms at 173 K, which indicated the well interconnectivity between micropores and mesopores. This study not only exhibits a new approach for investigation of pores and hollows of PS, but also provides a better understanding of porous structures for rational design in adsorbing functional compounds.

Keywords: (129)Xe NMR; 2D EXSY; Interconnectivity; Porous starch; Porous structure.