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Helium-cooling and -spinning dynamic nuclear polarization for sensitivity-enhanced solid-state NMR at 14 T and 30 K

Authors
Journal
Journal of Magnetic Resonance
1090-7807
Publisher
Elsevier
Volume
225
Identifiers
DOI: 10.1016/j.jmr.2012.09.008
Keywords
  • Dynamic Nuclear Polarization
  • Solid-State Nmr
  • High Field Condition
  • Cryogenic Mas Using Helium Gas
Disciplines
  • Biology

Abstract

Abstract We describe a 1H polarization enhancement via dynamic nuclear polarization (DNP) at very low sample temperature T≈30K under magic-angle spinning (MAS) conditions for sensitivity-enhanced solid-state NMR measurement. Experiments were conducted at a high external field strength of 14.1T. For MAS DNP experiments at T≪90K, a new probe system using cold helium gas for both sample-cooling and -spinning was developed. The novel system can sustain a low sample temperature between 30 and 90K for a period of time >10h under MAS at νR≈3kHz with liquid He consumption of ≈6L/h. As a microwave source, we employed a high-power, continuously frequency-tunable gyrotron. At T≈34K, 1H DNP enhancement factors of 47 and 23 were observed with and without MAS, respectively. On the basis of these observations, a discussion on the total NMR sensitivity that takes into account the effect of sample temperature and external field strength used in DNP experiments is presented. It was determined that the use of low sample temperature and high external field is generally rewarding for the total sensitivity, in spite of the slower polarization buildup at lower temperature and lower DNP efficiency at higher field. These findings highlight the potential of the current continuous-wave DNP technique also at very high field conditions suitable to analyze large and complex systems, such as biological macromolecules.

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