Dynamic nuclear polarization NMR enables the analysis of Sn-Beta zeolite prepared with natural abundance ¹¹⁹Sn precursors. Gunther, W. R, Michaelis, V. K, Caporini, M. A, Griffin, R. G, & Román-Leshkov, Y. Journal of the American Chemical Society, 136(17):6219–6222, April, 2014. Publisher: American Chemical Society ISBN: 1520-5126 (Electronic)${\}$r0002-7863 (Linking)![Dynamic nuclear polarization NMR enables the analysis of Sn-Beta zeolite prepared with natural abundance ¹¹⁹Sn precursors. [link]](https://bibbase.org/img/filetypes/link.svg "link")
Paper doi abstract bibtex The catalytic activity of tin-containing zeolites, such as Sn-Beta, is critically dependent on the successful incorporation of the tin metal center into the zeolite framework. However, synchrotron-based techniques or solid-state nuclear magnetic resonance (ssNMR) of samples enriched with (119)Sn isotopes are the only reliable methods to verify framework incorporation. This work demonstrates, for the first time, the use of dynamic nuclear polarization (DNP) NMR for characterizing zeolites containing ~2 wt % of natural abundance Sn without the need for (119)Sn isotopic enrichment. The biradicals TOTAPOL, bTbK, bCTbK, and SPIROPOL functioned effectively as polarizing sources, and the solvent enabled proper transfer of spin polarization from the radical's unpaired electrons to the target nuclei. Using bCTbK led to an enhancement ($ε$) of 75, allowing the characterization of natural-abundance (119)Sn-Beta with excellent signal-to-noise ratios in \textless24 h. Without DNP, no (119)Sn resonances were detected after 10 days of continuous analysis.
@article{Gunther2014a,
title = {Dynamic nuclear polarization {NMR} enables the analysis of {Sn}-{Beta} zeolite prepared with natural abundance ¹¹⁹{Sn} precursors.},
volume = {136},
issn = {1520-5126},
url = {http://dx.doi.org/10.1021/ja502113d},
doi = {10.1021/ja502113d},
abstract = {The catalytic activity of tin-containing zeolites, such as Sn-Beta, is critically dependent on the successful incorporation of the tin metal center into the zeolite framework. However, synchrotron-based techniques or solid-state nuclear magnetic resonance (ssNMR) of samples enriched with (119)Sn isotopes are the only reliable methods to verify framework incorporation. This work demonstrates, for the first time, the use of dynamic nuclear polarization (DNP) NMR for characterizing zeolites containing {\textasciitilde}2 wt \% of natural abundance Sn without the need for (119)Sn isotopic enrichment. The biradicals TOTAPOL, bTbK, bCTbK, and SPIROPOL functioned effectively as polarizing sources, and the solvent enabled proper transfer of spin polarization from the radical's unpaired electrons to the target nuclei. Using bCTbK led to an enhancement (\$ε\$) of 75, allowing the characterization of natural-abundance (119)Sn-Beta with excellent signal-to-noise ratios in {\textless}24 h. Without DNP, no (119)Sn resonances were detected after 10 days of continuous analysis.},
number = {17},
journal = {Journal of the American Chemical Society},
author = {Gunther, William R and Michaelis, Vladimir K and Caporini, Marc A and Griffin, Robert G and Román-Leshkov, Yuriy},
month = apr,
year = {2014},
pmid = {24697321},
note = {Publisher: American Chemical Society
ISBN: 1520-5126 (Electronic)\${\textbackslash}\$r0002-7863 (Linking)},
keywords = {Magnetic Resonance Spectroscopy, Magnetic Resonance Spectroscopy: methods, Models, Molecular, Tin, Tin: analysis, Zeolites, Zeolites: chemistry},
pages = {6219--6222},
}
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This work demonstrates, for the first time, the use of dynamic nuclear polarization (DNP) NMR for characterizing zeolites containing ~2 wt % of natural abundance Sn without the need for (119)Sn isotopic enrichment. The biradicals TOTAPOL, bTbK, bCTbK, and SPIROPOL functioned effectively as polarizing sources, and the solvent enabled proper transfer of spin polarization from the radical's unpaired electrons to the target nuclei. Using bCTbK led to an enhancement ($ε$) of 75, allowing the characterization of natural-abundance (119)Sn-Beta with excellent signal-to-noise ratios in \\textless24 h. Without DNP, no (119)Sn resonances were detected after 10 days of continuous analysis.","number":"17","journal":"Journal of the American Chemical Society","author":[{"propositions":[],"lastnames":["Gunther"],"firstnames":["William","R"],"suffixes":[]},{"propositions":[],"lastnames":["Michaelis"],"firstnames":["Vladimir","K"],"suffixes":[]},{"propositions":[],"lastnames":["Caporini"],"firstnames":["Marc","A"],"suffixes":[]},{"propositions":[],"lastnames":["Griffin"],"firstnames":["Robert","G"],"suffixes":[]},{"propositions":[],"lastnames":["Román-Leshkov"],"firstnames":["Yuriy"],"suffixes":[]}],"month":"April","year":"2014","pmid":"24697321","note":"Publisher: American Chemical Society ISBN: 1520-5126 (Electronic)${\\}$r0002-7863 (Linking)","keywords":"Magnetic Resonance Spectroscopy, Magnetic Resonance Spectroscopy: methods, Models, Molecular, Tin, Tin: analysis, Zeolites, Zeolites: chemistry","pages":"6219–6222","bibtex":"@article{Gunther2014a,\n\ttitle = {Dynamic nuclear polarization {NMR} enables the analysis of {Sn}-{Beta} zeolite prepared with natural abundance ¹¹⁹{Sn} precursors.},\n\tvolume = {136},\n\tissn = {1520-5126},\n\turl = {http://dx.doi.org/10.1021/ja502113d},\n\tdoi = {10.1021/ja502113d},\n\tabstract = {The catalytic activity of tin-containing zeolites, such as Sn-Beta, is critically dependent on the successful incorporation of the tin metal center into the zeolite framework. 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