Price, Lauren E., Nicholas Alaniva, Marthe Millen, Till Epprecht, Michael Urban, Alexander Däpp, and Alexander B. Barnes. “Cryogenic-Compatible Spherical Rotors and Stators for Magic Angle Spinning Dynamic Nuclear Polarization.” Preprint. Solid-state NMR/▪ probe development, May 8, 2023.
https://doi.org/10.5194/mr-2023-6.
Cryogenic magic-angle spinning (MAS) is a standard technique utilized for Dynamic Nuclear Polarization (DNP) in solid state nuclear magnetic resonance (NMR). Here we describe the optimization and implementation of a stator for cryogenic MAS with spherical rotors, allowing for DNP experiments on large sample volumes. Designs of the stator and rotor 10 for cryogenic MAS build on recent advancements of MAS spheres, and take a step further to incorporate sample-insert/eject and temperature-independent spinning stability of +/- 1 Hz. At a field of 7 T and spinning at 2.0 kHz with a sample temperature of 105-107 K, DNP enhancements of 256 and 200 were observed for 124 μL and 223 μL sample volumes, respectively, each consisting of 4 M 13C, 15N-labelled urea and 20 mM AMUPol in a glycerol-water glassy matrix.