Dynamic Nuclear Polarization NMR Enables the Analysis of Sn-Beta Zeolite Prepared with Natural Abundance Sn-119 Precursors

作者：Gunther William R; Michaelis Vladimir K; Caporini Marc A; Griffin Robert G; Roman Leshkov Yuriy^*

来源：Journal of the American Chemical Society, 2014, 136(17): 6219-6222.

DOI：10.1021/ja502113d

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 Sn-119 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 similar to 2 wt % of natural abundance Sn without the need for Sn-119 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 (e) of 75, allowing the characterization of natural-abundance Sn-119-Beta with excellent signal-to-noise ratios in <24 h. Without DNP, no Sn-119 resonances were detected after 10 days of continuous analysis.

• 出版日期2014-4-30