Dynamic nuclear polarization at 700 MHz/460 GHz. Barnes, A. B, Markhasin, E., Daviso, E., Michaelis, V. K, Nanni, E. a, Jawla, S. K, Mena, E. L, DeRocher, R., Thakkar, A., Woskov, P. P, Herzfeld, J., Temkin, R. J, & Griffin, R. G Journal of magnetic resonance (San Diego, Calif. : 1997), 224:1–7, November, 2012. Publisher: Elsevier Inc.![Dynamic nuclear polarization at 700 MHz/460 GHz. [link]](https://bibbase.org/img/filetypes/link.svg "link")
Paper doi abstract bibtex We describe the design and implementation of the instrumentation required to perform DNP-NMR at higher field strengths than previously demonstrated, and report the first magic-angle spinning (MAS) DNP-NMR experiments performed at (1)H/e(-) frequencies of 700 MHz/460 GHz. The extension of DNP-NMR to 16.4 T has required the development of probe technology, cryogenics, gyrotrons, and microwave transmission lines. The probe contains a 460 GHz microwave channel, with corrugated waveguide, tapers, and miter-bends that couple microwave power to the sample. Experimental efficiency is increased by a cryogenic exchange system for 3.2 mm rotors within the 89 mm bore. Sample temperatures ≤85 K, resulting in improved DNP enhancements, are achieved by a novel heat exchanger design, stainless steel and brass vacuum jacketed transfer lines, and a bronze probe dewar. In addition, the heat exchanger is preceded with a nitrogen drying and generation system in series with a pre-cooling refrigerator. This reduces liquid nitrogen usage from \textgreater700 l per day to \textless200 l per day and allows for continuous (\textgreater7 days) cryogenic spinning without detrimental frost or ice formation. Initial enhancements, ε=-40, and a strong microwave power dependence suggests the possibility for considerable improvement. Finally, two-dimensional spectra of a model system demonstrate that the higher field provides excellent resolution, even in a glassy, cryoprotecting matrix.
@article{Barnes2012,
title = {Dynamic nuclear polarization at 700 {MHz}/460 {GHz}.},
volume = {224},
issn = {1096-0856},
url = {http://www.ncbi.nlm.nih.gov/pubmed/23000974},
doi = {10.1016/j.jmr.2012.08.002},
abstract = {We describe the design and implementation of the instrumentation required to perform DNP-NMR at higher field strengths than previously demonstrated, and report the first magic-angle spinning (MAS) DNP-NMR experiments performed at (1)H/e(-) frequencies of 700 MHz/460 GHz. The extension of DNP-NMR to 16.4 T has required the development of probe technology, cryogenics, gyrotrons, and microwave transmission lines. The probe contains a 460 GHz microwave channel, with corrugated waveguide, tapers, and miter-bends that couple microwave power to the sample. Experimental efficiency is increased by a cryogenic exchange system for 3.2 mm rotors within the 89 mm bore. Sample temperatures ≤85 K, resulting in improved DNP enhancements, are achieved by a novel heat exchanger design, stainless steel and brass vacuum jacketed transfer lines, and a bronze probe dewar. In addition, the heat exchanger is preceded with a nitrogen drying and generation system in series with a pre-cooling refrigerator. This reduces liquid nitrogen usage from {\textgreater}700 l per day to {\textless}200 l per day and allows for continuous ({\textgreater}7 days) cryogenic spinning without detrimental frost or ice formation. Initial enhancements, ε=-40, and a strong microwave power dependence suggests the possibility for considerable improvement. Finally, two-dimensional spectra of a model system demonstrate that the higher field provides excellent resolution, even in a glassy, cryoprotecting matrix.},
urldate = {2013-12-17},
journal = {Journal of magnetic resonance (San Diego, Calif. : 1997)},
author = {Barnes, Alexander B and Markhasin, Evgeny and Daviso, Eugenio and Michaelis, Vladimir K and Nanni, Emilio a and Jawla, Sudheer K and Mena, Elijah L and DeRocher, Ronald and Thakkar, Ajay and Woskov, Paul P and Herzfeld, Judith and Temkin, Richard J and Griffin, Robert G},
month = nov,
year = {2012},
pmid = {23000974},
note = {Publisher: Elsevier Inc.},
keywords = {Equipment Design, Equipment Failure Analysis, Magnetic Resonance Spectroscopy, Magnetic Resonance Spectroscopy: instrumentation, Refrigeration, Refrigeration: instrumentation, Specimen Handling, Specimen Handling: instrumentation, Transducers},
pages = {1--7},
}
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The extension of DNP-NMR to 16.4 T has required the development of probe technology, cryogenics, gyrotrons, and microwave transmission lines. The probe contains a 460 GHz microwave channel, with corrugated waveguide, tapers, and miter-bends that couple microwave power to the sample. Experimental efficiency is increased by a cryogenic exchange system for 3.2 mm rotors within the 89 mm bore. Sample temperatures ≤85 K, resulting in improved DNP enhancements, are achieved by a novel heat exchanger design, stainless steel and brass vacuum jacketed transfer lines, and a bronze probe dewar. In addition, the heat exchanger is preceded with a nitrogen drying and generation system in series with a pre-cooling refrigerator. This reduces liquid nitrogen usage from \\textgreater700 l per day to \\textless200 l per day and allows for continuous (\\textgreater7 days) cryogenic spinning without detrimental frost or ice formation. Initial enhancements, ε=-40, and a strong microwave power dependence suggests the possibility for considerable improvement. 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