Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results
Dynamic Nuclear Polarization (DNP) experiments transfer polarization from electron spins to nuclear spins with microwave irradiation of the electron spins for enhanced sensitivity in nuclear magnetic resonance (NMR) spectroscopy. Design and testing of a spectrometer for magic angle spinning (MAS) DN...
| Main Authors: | , , , , , , , , , , , , |
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| Other Authors: | |
| Format: | Article |
| Language: | en_US |
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Royal Society of Chemistry
2012
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| Online Access: | http://hdl.handle.net/1721.1/74583 https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 |
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| author | Rosay, Melanie Tometich, Leo Pawsey, Shane Bater, Reto Schauwecker, Robert Blank, Monica Borchard, Philipp M. Cauffman, Stephen R. Felch, Kevin L. Weber, Ralph T. Griffin, Robert Guy Maas, Werner Temkin, Richard J |
| author2 | Massachusetts Institute of Technology. Department of Chemistry |
| author_facet | Massachusetts Institute of Technology. Department of Chemistry Rosay, Melanie Tometich, Leo Pawsey, Shane Bater, Reto Schauwecker, Robert Blank, Monica Borchard, Philipp M. Cauffman, Stephen R. Felch, Kevin L. Weber, Ralph T. Griffin, Robert Guy Maas, Werner Temkin, Richard J |
| author_sort | Rosay, Melanie |
| collection | MIT |
| description | Dynamic Nuclear Polarization (DNP) experiments transfer polarization from electron spins to nuclear spins with microwave irradiation of the electron spins for enhanced sensitivity in nuclear magnetic resonance (NMR) spectroscopy. Design and testing of a spectrometer for magic angle spinning (MAS) DNP experiments at 263 GHz microwave frequency, 400 MHz 1H frequency is described. Microwaves are generated by a novel continuous-wave gyrotron, transmitted to the NMR probe via a transmission line, and irradiated on a 3.2 mm rotor for MAS DNP experiments. DNP signal enhancements of up to 80 have been measured at 95 K on urea and proline in water–glycerol with the biradical polarizing agent TOTAPOL. We characterize the experimental parameters affecting the DNP efficiency: the magnetic field dependence, temperature dependence and polarization build-up times, microwave power dependence, sample heating effects, and spinning frequency dependence of the DNP signal enhancement. Stable system operation, including DNP performance, is also demonstrated over a 36 h period. |
| first_indexed | 2024-09-23T10:46:08Z |
| format | Article |
| id | mit-1721.1/74583 |
| institution | Massachusetts Institute of Technology |
| language | en_US |
| last_indexed | 2024-09-23T10:46:08Z |
| publishDate | 2012 |
| publisher | Royal Society of Chemistry |
| record_format | dspace |
| spelling | mit-1721.1/745832022-09-30T22:51:32Z Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results Rosay, Melanie Tometich, Leo Pawsey, Shane Bater, Reto Schauwecker, Robert Blank, Monica Borchard, Philipp M. Cauffman, Stephen R. Felch, Kevin L. Weber, Ralph T. Griffin, Robert Guy Maas, Werner Temkin, Richard J Massachusetts Institute of Technology. Department of Chemistry Massachusetts Institute of Technology. Department of Physics Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology) Griffin, Robert Guy Griffin, Robert Guy Temkin, Richard J. Dynamic Nuclear Polarization (DNP) experiments transfer polarization from electron spins to nuclear spins with microwave irradiation of the electron spins for enhanced sensitivity in nuclear magnetic resonance (NMR) spectroscopy. Design and testing of a spectrometer for magic angle spinning (MAS) DNP experiments at 263 GHz microwave frequency, 400 MHz 1H frequency is described. Microwaves are generated by a novel continuous-wave gyrotron, transmitted to the NMR probe via a transmission line, and irradiated on a 3.2 mm rotor for MAS DNP experiments. DNP signal enhancements of up to 80 have been measured at 95 K on urea and proline in water–glycerol with the biradical polarizing agent TOTAPOL. We characterize the experimental parameters affecting the DNP efficiency: the magnetic field dependence, temperature dependence and polarization build-up times, microwave power dependence, sample heating effects, and spinning frequency dependence of the DNP signal enhancement. Stable system operation, including DNP performance, is also demonstrated over a 36 h period. National Institutes of Health (U.S.) (NIH grant EB-002804) National Institutes of Health (U.S.) (NIH grant EB-002026) 2012-11-06T22:34:19Z 2012-11-06T22:34:19Z 2010-05 2010-02 Article http://purl.org/eprint/type/JournalArticle 1463-9076 1463-9084 http://hdl.handle.net/1721.1/74583 Rosay, Melanie et al. “Solid-state Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results.” Physical Chemistry Chemical Physics 12.22 (2010): 5850. Web. https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 en_US http://dx.doi.org/10.1039/c003685b Physical Chemistry Chemical Physics Creative Commons Attribution-Noncommercial-Share Alike 3.0 http://creativecommons.org/licenses/by-nc-sa/3.0/ application/pdf Royal Society of Chemistry Prof. Griffin via Erja Kajosalo |
| spellingShingle | Rosay, Melanie Tometich, Leo Pawsey, Shane Bater, Reto Schauwecker, Robert Blank, Monica Borchard, Philipp M. Cauffman, Stephen R. Felch, Kevin L. Weber, Ralph T. Griffin, Robert Guy Maas, Werner Temkin, Richard J Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results |
| title | Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results |
| title_full | Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results |
| title_fullStr | Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results |
| title_full_unstemmed | Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results |
| title_short | Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results |
| title_sort | solid state dynamic nuclear polarization at 263 ghz spectrometer design and experimental results |
| url | http://hdl.handle.net/1721.1/74583 https://orcid.org/0000-0003-1589-832X https://orcid.org/0000-0001-9813-0177 |
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