MRI: Acquisition of a High Temperature and Pressure Solid-state NMR Spectrometer

The award supports the acquisition, installation, and shared research application of a state-of- the-art solid-state nuclear magnetic resonance (ssNMR) spectrometer system in the Nano Research Facility/Jens Molecular and Nanoscale Analysis Laboratory (NRF/Jens Lab) at Washington University in St. Louis, Missouri (WUStL). The ssNMR system is capable of high- temperature and high-pressure sample analysis, thus opening the door to the study of a broad range of critical environmental remediation, biological processing, and fuel/chemical/polymer manufacturing technologies under realistic conditions.

Primary research areas include: (1) homogeneous and heterogeneous catalysis, (2) membrane-based separations, (3) polymeric and biological materials properties, and (4) geochemical and biogeochemical systems (e.g., carbon sequestration). The system will support a broad user base consisting of researchers at multiple universities in the Midwest region surrounding St Louis (including Missouri Science and Technology, Kansas State University, University of Kansas, University of Notre Dame, and the University of Oklahoma).

The NMR system will play a key, connecting role in advancing fundamental knowledge in critical technology areas while promoting diversity and STEM education at multiple educational levels.

The acquired system is a commercial AVANCE NEO 400 MHz NMR spectrometer uniquely designed and equipped to acquire in-situ NMR spectra simultaneously from solid, liquid, and/or gas analytes at high-temperatures (up to 250 °C), high-pressures (up to 400 bar at 20 °C), or high-T,P conditions (up to 225 bar at 250 °C). The greater St. Louis metropolitan region does not have an ssNMR facility with these capabilities.

The spectrometer is designed for magic-angle spinning (MAS) solid-state NMR (ssNMR) across a range of NMR-active species for conventional (ex-situ) NMR studies and for in-situ MAS ssNMR capable of analyzing simultaneously gases, liquids, and solids under such high-T,P conditions. The spectrometer is equipped with a wide- bore magnet; MAS pneumatic and variable temperature (VT) control with heater power booster units; VT-stack for high-T experiments; and high-T MAS probe required for in-situ ssNMR experiments at high-T,P.

Access and administrative support will be provided through the NRF/Jens Lab with instrument management and oversight coordinated and supported by two advisory committees (a Scientific Advisory Committee and an Operations and Management Committee). The instrument will be available to internal and external academic users as well as external corporate users through a web-based scheduling system.

All users will pay hourly usage fees to support the operation and maintenance of the instrument. This broadly accessible ssNMR instrument, with its modern commercial console and high-T,P capabilities, will provide unprecedented opportunities to (1) familiarize students with this technology—important for their training and professional development, (2) advance the specific science and engineering research projects of user groups, and (3) facilitate shared expertise and catalyze new research partnerships and collaborations.

This award reflects NSF's statutory mission and has been deemed worthy of support through evaluation using the Foundation's intellectual merit and broader impacts review criteria.