Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy

Wang, Zhuoran; Hanrahan, Michael P.; Kobayashi, Takeshi; Perras, Frédéric A.; Chen, Yunhua; Engelke, Frank; Reiter, Christian; Purea, Armin; Rossini, Aaron J.; Pruski, Marek

doi:10.1016/j.ssnmr.2020.101685

Title: Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy

Journal Article · Tue Aug 11 00:00:00 EDT 2020 · Solid State Nuclear Magnetic Resonance

DOI:https://doi.org/10.1016/j.ssnmr.2020.101685· OSTI ID:1668253

^[1]; Hanrahan, Michael P. ^[1]; Kobayashi, Takeshi ^[1]; Perras, Frédéric A. ^[1]; Chen, Yunhua ^[1]; Engelke, Frank ^[2]; Reiter, Christian ^[2]; Purea, Armin ^[2]; Rossini, Aaron J. ^[1]; Pruski, Marek ^[1]

Ames Lab., and Iowa State Univ., Ames, IA (United States)
Bruker Biospin, Rheinstetten (Germany)

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 (MAS) probes with 1.3-mm diameter rotors capable of MAS at 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 ¹³C, ¹⁵N, ¹¹³Cd and ⁸⁹Y 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. Finally, for ⁸⁹Y, 2D idHETCOR provided 8.2 times better sensitivity than the 1 D⁸⁹Y-detected CP experiment performed with a 3.2-mm rotor.

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Research Organization:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1668253

Alternate ID(s):: OSTI ID: 1660304

Report Number(s):: IS-J-10,314

Journal Information:: Solid State Nuclear Magnetic Resonance, Vol. 109; ISSN 0926-2040

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
solid-state NMR
dynamic nuclear polarization
fast magic angle spinning
indirect detection

Title: Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy

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