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Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids
Open accessAbstract
Dynamic nuclear polarization (DNP) solid-state NMR has been applied to powdered microcrystalline solids to obtain sensitivity enhancements on the order of 100. Glucose, sulfathiazole, and paracetamol were impregnated with bis-nitroxide biradical (bis-cyclohexyl-TEMPO-bisketal, bCTbK) solutions of organic solvents. The organic solvents were carefully chosen to be nonsolvents for the compounds, so that DNP-enhanced solid-state NMR spectra of the unaltered solids could be acquired. A theoretical model is presented that illustrates that for externally doped organic solids characterized by long spin-lattice relaxation times (T(1)((1)H) > 200 s), (1)H-(1)H spin diffusion can relay enhanced polarization over micrometer length scales yielding substantial DNP enhancements (ε). ε on the order of 60 are obtained for microcrystalline glucose and sulfathiazole at 9.4 T and with temperatures of ca. 105 K. The large gain in sensitivity enables the rapid acquisition of (13)C-(13)C correlation spectra at natural isotopic abundance. It is anticipated that this will be a general method for enhancing the sensitivity of solid-state NMR experiments of organic solids.
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Cited by
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
Viger-Gravel, J., Schantz, A., Pinon, A. C., Rossini, A. J., Schantz, S., & Emsley, L. (2018) · The Journal of Physical Chemistry B · doi:10.1021/acs.jpcb.7b10795 · Cited by 202
Takahashi, H., Ayala, I., Bardet, M., De Paëpe, G., Simorre, J.-P., & Hediger, S. (2013) · Journal of the American Chemical Society · doi:10.1021/ja312501d · Cited by 149
Metadata
- Authors
- Rossini, A. J., Zagdoun, A., Hegner, F., Schwarzwälder, M., Gajan, D., Copéret, C., Lesage, A., & Emsley, L.
- Venue
- Journal of the American Chemical Society
- Publisher
- American Chemical Society (ACS)
- Published
- 2012-09-25
- Volume
- 134
- Issue
- 40
- Pages
- 16899-16908
- ISSN
- 0002-7863 (ISSN-L)
- 1520-5126
- OpenAlex
- W2075072191
- Cited by
- 293
- References
- 0
- FWCI
- 10.24
- Type
- journal article
- Language
- en
- Open access
- green
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- Rossini, A. J., Zagdoun, A., Hegner, F., Schwarzwälder, M., Gajan, D., Copéret, C., Lesage, A., & Emsley, L. (2012). Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids. Journal of the American Chemical Society. https://doi.org/10.1021/ja308135r
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