Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization
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 cryo...
| Main Authors: | , , , , , , , , , , , |
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| Other Authors: | |
| Format: | Article |
| Language: | en_US |
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Elsevier
2013
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| Online Access: | http://hdl.handle.net/1721.1/82050 https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 |
| _version_ | 1811090037159231488 |
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| author | 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. Bryant, Jeffrey A. Griffin, Robert Guy |
| author2 | Massachusetts Institute of Technology. Department of Chemistry |
| author_facet | Massachusetts Institute of Technology. Department of Chemistry 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. Bryant, Jeffrey A. Griffin, Robert Guy |
| author_sort | Barnes, Alexander |
| collection | MIT |
| description | 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. |
| first_indexed | 2024-09-23T14:31:02Z |
| format | Article |
| id | mit-1721.1/82050 |
| institution | Massachusetts Institute of Technology |
| language | en_US |
| last_indexed | 2024-09-23T14:31:02Z |
| publishDate | 2013 |
| publisher | Elsevier |
| record_format | dspace |
| spelling | mit-1721.1/820502022-10-01T21:33:14Z Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization 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. Bryant, Jeffrey A. Griffin, Robert Guy 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) Barnes, Alexander Mak-Jurkauskas, Melody L. Matsuki, Yoh Bajaj, Vikram S. van der Wel, Patrick C.A. DeRocher, Ronald C. Bryant, Jeffrey A. Sirigiri, Jagadishwar R. Temkin, Richard J. Griffin, Robert Guy 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. National Institute for Biomedical Imaging and Bioengineering (U.S.) (Grant EB-002804) National Institute for Biomedical Imaging and Bioengineering (U.S.) (Grant EB-001960) National Institute for Biomedical Imaging and Bioengineering (U.S.) (Grant EB-001035) National Institute for Biomedical Imaging and Bioengineering (U.S.) (Grant EB-002026) National Institute for Biomedical Imaging and Bioengineering (U.S.) (Grant EB-003151) National Science Foundation (U.S.). Graduate Research Fellowship Program 2013-11-08T17:44:18Z 2013-11-08T17:44:18Z 2009-03 2009-02 Article http://purl.org/eprint/type/JournalArticle 10907807 1096-0856 http://hdl.handle.net/1721.1/82050 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. https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 en_US http://dx.doi.org/10.1016/j.jmr.2009.03.003 Journal of Magnetic Resonance Creative Commons Attribution-Noncommercial-Share Alike 3.0 http://creativecommons.org/licenses/by-nc-sa/3.0/ application/pdf Elsevier PMC |
| spellingShingle | 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. Bryant, Jeffrey A. Griffin, Robert Guy Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization |
| title | Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization |
| title_full | Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization |
| title_fullStr | Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization |
| title_full_unstemmed | Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization |
| title_short | Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization |
| title_sort | cryogenic sample exchange nmr probe for magic angle spinning dynamic nuclear polarization |
| url | http://hdl.handle.net/1721.1/82050 https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 |
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