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Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results
Open accessAbstract
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 (1)H 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.
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Cited by
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
Lesage, A., Lelli, M., Gajan, D., Caporini, M. A., Vitzthum, V., Miéville, P., Alauzun, J., Roussey, A., Thieuleux, C., Mehdi, A., et al. (2010) · Journal of the American Chemical Society · doi:10.1021/ja104771z · Cited by 585
Dynamic nuclear polarization for sensitivity enhancement in modern solid-state NMR
Lilly Thankamony, A. S., Wittmann, J. J., Kaushik, M., & Corzilius, B. (2017) · Progress in Nuclear Magnetic Resonance Spectroscopy · doi:10.1016/j.pnmrs.2017.06.002 · Cited by 544
Highly Efficient, Water‐Soluble Polarizing Agents for Dynamic Nuclear Polarization at High Frequency
Sauvée, C., Rosay, M., Casano, G., Aussenac, F., Weber, R. T., Ouari, O., & Tordo, P. (2013) · Angewandte Chemie International Edition · doi:10.1002/anie.201304657 · Cited by 503
Self-citationThurber, K. R., & Tycko, R. (2012) · The Journal of Chemical Physics · doi:10.1063/1.4747449 · Cited by 263
Sensitivity-enhanced solid-state NMR detection of expansin’s target in plant cell walls
Wang, T., Park, Y. B., Caporini, M. A., Rosay, M., Zhong, L., Cosgrove, D. J., & Hong, M. (2013) · Proceedings of the National Academy of Sciences · doi:10.1073/pnas.1316290110 · Cited by 234
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Metadata
- Authors
- Rosay, M., Tometich, L., Pawsey, S., Bader, R., Schauwecker, R., Blank, M., Borchard, P. M., Cauffman, S. R., Felch, K. L., Weber, R. T., Temkin, R. J., Griffin, R. G., & Maas, W. E.
- Venue
- Physical Chemistry Chemical Physics
- Publisher
- Royal Society of Chemistry (RSC)
- Published
- 2010
- Volume
- 12
- Issue
- 22
- Pages
- 5850
- ISSN
- 1463-9076 (ISSN-L)
- 1463-9084
- OpenAlex
- W2108846485
- Cited by
- 370
- References
- 0
- FWCI
- 12.99
- Type
- journal article
- Language
- en
- Open access
- green
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- Rosay, M., Tometich, L., Pawsey, S., Bader, R., Schauwecker, R., Blank, M., Borchard, P. M., Cauffman, S. R., Felch, K. L., Weber, R. T., Temkin, R. J., Griffin, R. G., & Maas, W. E. (2010). Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results. Physical Chemistry Chemical Physics. https://doi.org/10.1039/c003685b
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