Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization

Alexander B Barnes; Melody L Mak-Jurkauskas; Yoh Matsuki; Vikram S Bajaj; Patrick C.A van der Wel; Ronald DeRocher; Jeffrey Bryant; Jagadishwar R Sirigiri; Richard J Temkin; Johan Lugtenburg; Judith Herzfeld; Robert G Griffin

doi:10.1016/j.jmr.2009.03.003

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Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization

Journal article

Peer reviewed

Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization

Alexander B Barnes, Melody L Mak-Jurkauskas, Yoh Matsuki, Vikram S Bajaj, Patrick C.A van der Wel, Ronald DeRocher, Jeffrey Bryant, Jagadishwar R Sirigiri, Richard J Temkin, Johan Lugtenburg, …

Journal of Magnetic Resonance (1997), Vol.198(2), pp.261-270

06/2009

DOI: https://doi.org/10.1016/j.jmr.2009.03.003

PMCID: PMC2957365

PMID: 19356957

Abstract

Instrumentation

Hardware

Dynamic nuclear polarization

Cryogenic MAS

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.

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Title: Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization
Creators: Alexander B Barnes - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Melody L Mak-Jurkauskas - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Yoh Matsuki - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Vikram S Bajaj - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Patrick C.A van der Wel - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Ronald DeRocher - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Jeffrey Bryant - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Jagadishwar R Sirigiri - Plasma Science and Fusion Center, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Richard J Temkin - Plasma Science and Fusion Center, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Johan Lugtenburg - Department of Chemistry, Rijksuniversiteit te Leiden, NL-2300 R A Leiden, The Netherlands
Judith Herzfeld - Department of Chemistry, Brandeis University, Waltham, MA 02454, USA
Robert G Griffin - Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA
Publication Details: Journal of Magnetic Resonance (1997), Vol.198(2), pp.261-270
Publisher: Elsevier Inc
Identifiers: 9923957904701921
Academic Unit: Department of Chemistry
Language: English
Resource Type: Journal article

Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization

Abstract

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