Accelerating Nuclear Magnetic Resonance (NMR) Analysis of Soil Organic Matter with Dynamic Nuclear Polarization (DNP) Enhancement

Tuesday, 16 December 2014
Anna Evangeline Normand1, Adam N Smith2, Joanna R Long3 and K. Ramesh Reddy1, (1)University of Florida, Soil and Water Science, Ft Walton Beach, FL, United States, (2)University of Florida, Chemistry, Ft Walton Beach, FL, United States, (3)University of Florida, Biochemistry and Molecular Biology, Ft Walton Beach, FL, United States
13C magic angle spinning (MAS) solid state Nuclear Magnetic Resonance (ssNMR) has become an essential tool for discerning the chemical composition of soil organic matter (SOM). However, the technique is limited due to the inherent insensitivity of NMR resulting in long acquisition times, especially for low carbon (C) soil. The pursuits of higher magnetic fields or concentrating C with hydrofluoric acid are limited solutions for signal improvement. Recent advances in dynamic nuclear polarization (DNP) have addressed the insensitivity of NMR. DNP utilizes the greater polarization of an unpaired electron in a given magnetic field and transfers that polarization to an NMR active nucleus of interest via microwave irradiation. Signal enhancements of up to a few orders of magnitude have been achieved for various DNP experiments. In this novel study, we conduct DNP 13C cross-polarization (CP) MAS ssNMR experiments of SOM varying in soil C content and chemical composition. DNP signal enhancements reduce the experiment run time allowing samples with low C to be analyzed in hours rather than days. We compare 13C CP MAS ssNMR of SOM with multiple magnetic field strengths, hydrofluoric acid treatment, and novel DNP approaches. We also explore DNP surface enhanced NMR Spectroscopy (SENP) to determine the surface chemistry of SOM. The presented results and future DNP MAS ssNMR advances will lead to further understanding of the nature and processes of SOM.