Facile NMR Relaxation Sensor for Monitoring of Biomass Degradation Products during Conversion to Biogas

Abstract

The chemical and morphological composition of animal biowaste is known to limit the efficiency of methane production by bacterial anaerobic digestion (AD). To better understand these material limitations, we studied degradative changes in cattle manure's organic complex components chemical and morphological composition during its AD to methane. This was achieved using low field 1 H NMR relaxation times domain (TD) spectral mapping combined with T 1 (spin-lattice) and T 2 (spin-spin) TD of cattle manure biomass (CM) peaks assignment, starting from samples of initial freshly collected CM biomass sample followed by several time points sampling during 21 days cycle of the AD process. A T 1-T 2 relaxation TD graph giving a stable reproducible pattern of 12 peaks was generated, and assigned to different domains, whose changes during AD could be observed. These 12 peaks were assigned to TDs of crystalline nano-aggregated complexes of different degrees of crystallinity with low porosity and low hydration rate and a morphological group of amorphous domains with increased pore size, density, and higher hydration. In agreement with models of elementary cellulose fibrils, these domains were designated as three layers of cellulose consisting of interior, subsurface, and surface. The most amorphous TD volume showed good correlation with biogas production and could serve as an indicator for digestibility and cellulose conversion to a glucose intermediate during the AD process. This study demonstrated the facile and versatile usage of 2D 1 H NMR T 1-T 2 sensorial technology in studying complex biowaste systems, with the potential for improving CM biomass conversion efficiency into bio-methane.