Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization
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Griffin_Cryogenic sample.pdf
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1.9 MB
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Author(s)
Barnes, Alexander
Mak-Jurkauskas, Melody L.
Matsuki, Yoh
Bajaj, Vikram S.
van der Wel, Patrick C.A.
Sirigiri, Jagadishwar R.
Temkin, Richard J.
Lugtenburg, Johan
Herzfeld, Judith
DeRocher, Ronald C.
Date Issued
March 2009
Journal
Journal of Magnetic Resonance
Publisher
Elsevier
Citation
Barnes, Alexander B., Melody L. Mak-Jurkauskas, Yoh Matsuki, Vikram S. Bajaj, Patrick C.A. van der Wel, Ronald DeRocher, Jeffrey Bryant, et al. “Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization.” Journal of Magnetic Resonance 198, no. 2 (June 2009): 261-270.
Version
Author's final manuscript
Abstract
We describe a cryogenic sample exchange system that dramatically improves the efficiency of magic angle spinning (MAS) dynamic nuclear polarization (DNP) experiments by reducing the time required to change samples and by improving long-term instrument stability. Changing samples in conventional cryogenic MAS DNP/NMR experiments involves warming the probe to room temperature, detaching all cryogenic, RF, and microwave connections, removing the probe from the magnet, replacing the sample, and reversing all the previous steps, with the entire cycle requiring a few hours. The sample exchange system described here—which relies on an eject pipe attached to the front of the MAS stator and a vacuum jacketed dewar with a bellowed hole—circumvents these procedures. To demonstrate the excellent sensitivity, resolution, and stability achieved with this quadruple resonance sample exchange probe, we have performed high precision distance measurements on the active site of the membrane protein bacteriorhodopsin. We also include a spectrum of the tripeptide N-f-MLF-OH at 100 K which shows 30 Hz linewidths.
MIT Department
Massachusetts Institute of Technology. Department of Chemistry
Massachusetts Institute of Technology. Department of Physics
Massachusetts Institute of Technology. Plasma Science and Fusion Center
Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology)
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Creative Commons Attribution-Noncommercial-Share Alike 3.0
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DOI of Published Version
https://doi.org/10.1016/j.jmr.2009.03.003
