October 9, 2020
Journal Article

High-Temperature and High-Pressure In Situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Abstract

Nuclear magnetic resonance (NMR) spectroscopy represents an important technique to understand the structure and bonding environment of molecules. There exists a drive to conduct characterization experiment under conditions relevant to the chemical process of interest. To address this, in situ high-temperature, high-pressure MAS NMR methods have been developed to enable the observation of chemical interactions over a range of pressures (vacuum to several hundred bar) and temperatures (well below 0°C to 250°C). Further, the chemical identity of the samples can be comprised of solids, liquids, and gases or mixtures of the three. The method incorporates all-zirconia NMR rotors (sample holder for MAS NMR) which can be sealed using a threaded cap to compress an O-ring. This rotor exhibits great chemical resistance, temperature compatibility, low NMR background, and can withstand high pressures. These factors combined enable its use in a wide range of system combinations which permit its use in diverse fields as carbon sequestration, catalysis, material science, geochemistry, and biology. The flexibility of this technique makes it an attractive option for scientists from numerous disciplines.

Revised: January 18, 2021 | Published: October 9, 2020

Citation

Jaegers N.R., W. Hu, Y. Wang, and J.Z. Hu. 2020. High-Temperature and High-Pressure In Situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy. Journal of Visualized Experiments (JoVE). PNNL-SA-153912. doi:10.3791/61794