Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source
In this communication, we report enhancements of nuclear spin polarization by dynamic nuclear polarization (DNP) in static and spinning solids at a magnetic field strength of 9 T (250 GHz for g = 2 electrons, 380 MHz for [superscript 1]H). In these experiments, [superscript 1]H enhancements of up to...
| Main Authors: | , , , , , , , , , |
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| Other Authors: | |
| Format: | Article |
| Language: | en_US |
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Elsevier
2015
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| Online Access: | http://hdl.handle.net/1721.1/99503 https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 |
| _version_ | 1826203592230436864 |
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| author | Bajaj, Vikram S. Farrar, C. T. Hornstein, Melissa K. Mastovsky, Ivan Vieregg, Jeffrey Bryant, Jeffrey A. Elena, B. Kreischer, K. E. Griffin, Robert Guy Temkin, Richard J |
| author2 | Massachusetts Institute of Technology. Department of Chemistry |
| author_facet | Massachusetts Institute of Technology. Department of Chemistry Bajaj, Vikram S. Farrar, C. T. Hornstein, Melissa K. Mastovsky, Ivan Vieregg, Jeffrey Bryant, Jeffrey A. Elena, B. Kreischer, K. E. Griffin, Robert Guy Temkin, Richard J |
| author_sort | Bajaj, Vikram S. |
| collection | MIT |
| description | In this communication, we report enhancements of nuclear spin polarization by dynamic nuclear polarization (DNP) in static and spinning solids at a magnetic field strength of 9 T (250 GHz for g = 2 electrons, 380 MHz for [superscript 1]H). In these experiments, [superscript 1]H enhancements of up to 170 ± 50 have been observed in 1-[superscript 13]C-glycine dispersed in a 60:40 glycerol/water matrix at temperatures of 20 K; in addition, we have observed significant enhancements in [superscript 15]N spectra of unoriented pf1-bacteriophage. Finally, enhancements of ~17 have been obtained in two-dimensional [superscript 13]C–[superscript 13]C chemical shift correlation spectra of the amino acid U–[superscript 13]C, [superscript 15]N-proline during magic angle spinning (MAS), demonstrating the stability of the DNP experiment for sustained acquisition and for quantitative experiments incorporating dipolar recoupling. In all cases, we have exploited the thermal mixing DNP mechanism with the nitroxide radical 4-amino-TEMPO as the paramagnetic dopant. These are the highest frequency DNP experiments performed to date and indicate that significant signal enhancements can be realized using the thermal mixing mechanism even at elevated magnetic fields. In large measure, this is due to the high microwave power output of the 250 GHz gyrotron oscillator used in these experiments. |
| first_indexed | 2024-09-23T12:39:44Z |
| format | Article |
| id | mit-1721.1/99503 |
| institution | Massachusetts Institute of Technology |
| language | en_US |
| last_indexed | 2024-09-23T12:39:44Z |
| publishDate | 2015 |
| publisher | Elsevier |
| record_format | dspace |
| spelling | mit-1721.1/995032022-10-01T10:19:52Z Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source Bajaj, Vikram S. Farrar, C. T. Hornstein, Melissa K. Mastovsky, Ivan Vieregg, Jeffrey Bryant, Jeffrey A. Elena, B. Kreischer, K. E. Griffin, Robert Guy Temkin, Richard J 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) Bajaj, Vikram S. Farrar, C. T. Hornstein, Melissa K. Mastovsky, Ivan Vieregg, Jeffrey Bryant, Jeffrey A. Elena, B. Kreischer, K. E. Temkin, Richard J. Griffin, Robert Guy In this communication, we report enhancements of nuclear spin polarization by dynamic nuclear polarization (DNP) in static and spinning solids at a magnetic field strength of 9 T (250 GHz for g = 2 electrons, 380 MHz for [superscript 1]H). In these experiments, [superscript 1]H enhancements of up to 170 ± 50 have been observed in 1-[superscript 13]C-glycine dispersed in a 60:40 glycerol/water matrix at temperatures of 20 K; in addition, we have observed significant enhancements in [superscript 15]N spectra of unoriented pf1-bacteriophage. Finally, enhancements of ~17 have been obtained in two-dimensional [superscript 13]C–[superscript 13]C chemical shift correlation spectra of the amino acid U–[superscript 13]C, [superscript 15]N-proline during magic angle spinning (MAS), demonstrating the stability of the DNP experiment for sustained acquisition and for quantitative experiments incorporating dipolar recoupling. In all cases, we have exploited the thermal mixing DNP mechanism with the nitroxide radical 4-amino-TEMPO as the paramagnetic dopant. These are the highest frequency DNP experiments performed to date and indicate that significant signal enhancements can be realized using the thermal mixing mechanism even at elevated magnetic fields. In large measure, this is due to the high microwave power output of the 250 GHz gyrotron oscillator used in these experiments. Natural Sciences and Engineering Research Council of Canada (Postgraduate Scholarship Fellowship) National Institutes of Health (U.S.) (Grant GM-35382) National Institutes of Health (U.S.) (Grant GM-55327) National Institutes of Health (U.S.) (Grant RR-00995) 2015-10-29T16:33:43Z 2015-10-29T16:33:43Z 2011-12 2002-12 Article http://purl.org/eprint/type/JournalArticle 10907807 1096-0856 http://hdl.handle.net/1721.1/99503 Bajaj, V.S., C.T. Farrar, M.K. Hornstein, I. Mastovsky, J. Vieregg, J. Bryant, B. Eléna, K.E. Kreischer, R.J. Temkin, and R.G. Griffin. “Dynamic Nuclear Polarization at 9T Using a Novel 250GHz Gyrotron Microwave Source.” Journal of Magnetic Resonance 213, no. 2 (December 2011): 404–409. https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 en_US http://dx.doi.org/10.1016/j.jmr.2011.09.010 Journal of Magnetic Resonance Creative Commons Attribution-Noncommercial-NoDerivatives http://creativecommons.org/licenses/by-nc-nd/4.0/ application/pdf Elsevier PMC |
| spellingShingle | Bajaj, Vikram S. Farrar, C. T. Hornstein, Melissa K. Mastovsky, Ivan Vieregg, Jeffrey Bryant, Jeffrey A. Elena, B. Kreischer, K. E. Griffin, Robert Guy Temkin, Richard J Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source |
| title | Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source |
| title_full | Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source |
| title_fullStr | Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source |
| title_full_unstemmed | Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source |
| title_short | Dynamic nuclear polarization at 9 T using a novel 250 GHz gyrotron microwave source |
| title_sort | dynamic nuclear polarization at 9 t using a novel 250 ghz gyrotron microwave source |
| url | http://hdl.handle.net/1721.1/99503 https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 |
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