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Article
Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy
Ames Laboratory Accepted Manuscripts
  • Zhuoran Wang, Iowa State University and Ames Laboratory
  • Michael P. Hanrahan, Iowa State University and Ames Laboratory
  • Takeshi Kobayashi, Ames Laboratory
  • Frédéric A. Perras, Ames Laboratory
  • Yunhua Chen, Iowa State University and Ames Laboratory
  • Frank Engelke, Bruker Biospin
  • Christian Reiter, Bruker Biospin
  • Armin Purea, Bruker Biospin
  • Aaron J. Rossini, Iowa State University and Ames Laboratory
  • Marek Pruski, Iowa State University and Ames Laboratory
Publication Date
8-11-2020
Department
Ames Laboratory; Chemistry
OSTI ID+
1668253
Report Number
IS-J 10314
DOI
10.1016/j.ssnmr.2020.101685
Journal Title
Solid State Nuclear Magnetic Resonance
Abstract

Dynamic nuclear polarization (DNP) and indirect detection are two commonly applied approaches for enhancing the sensitivity of solid-state NMR spectroscopy. However, their use in tandem has not yet been investigated. With the advent of low-temperature fast magic angle spinning (MM) probes with 1.3-mm diameter rotors capable of MAS a 40 kHz it becomes feasible to combine these two techniques. In this study, we performed DNP-enhanced 2D indirectly detected heteronuclear correlation (idHETCOR) experiments on C-13, N-15, Cd-113 and 89 Y nuclei in functionalized mesoporous silica, CdS nanoparticles, and Y2O3 nanoparticles. The sensitivity of the 2D idHETCOR experiments was compared with those of DNP-enhanced directly-detected 1D cross polarization (CP) and 2D HETCOR experiments performed with a standard 3.2-mm rotor. Due to low CP polarization transfer efficiencies and large proton linewidth, the sensitivity gains achieved by indirect detection alone were lower than in conventional (non-DNP) experiments. Nevertheless, despite the smaller sample volume the 2D idHETCOR experiments showed better absolute sensitivities than 2D HETCOR experiments for nuclei with the lowest gyromagnetic ratios. For Y-89, 2D idHETCOR provided 8.2 times better sensitivity than the 1 (DY)-Y-89-detected CP experiment performed with a 3.2-mm rotor.

DOE Contract Number(s)
AC02-07CH11358
Language
en
Publisher
Iowa State University Digital Repository, Ames IA (United States)
Disciplines
Citation Information
Zhuoran Wang, Michael P. Hanrahan, Takeshi Kobayashi, Frédéric A. Perras, et al.. "Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy" Vol. 109 (2020) p. 101685
Available at: http://works.bepress.com/aaron-rossini/96/