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Adiabatic Sweep Cross-polarization Magic-angle-spinning Nmr Of Half-integer Quadrupolar Spins

Title: Adiabatic Sweep Cross-polarization Magic-angle-spinning Nmr Of Half-integer Quadrupolar Spins.
Name(s): Wi, Sungsool, author
Kim, Chul, author
Schurko, Robert, author
Frydman, Lucio, author
Type of Resource: text
Genre: Journal Article
Journal Article
Date Issued: 2017-04
Physical Form: computer
online resource
Extent: 1 online resource
Language(s): English
Abstract/Description: The use of frequency-swept radiofrequency (rf) pulses for enhancing signals in the magic-angle spinning (MAS) spectra of half-integer quadrupolar nuclides was explored. The broadband adiabatic inversion cross-polarization magic-angle spinning (BRAIN-CPMAS) method, involving an adiabatic inversion pulse on the S-channel and a simultaneous rectangular spin-lock pulse on the I-channel (H-1), was applied to I (1/2) -> S(3/2) systems. Optimal BRAIN-CPMAS matching conditions were found to involve low rf pulse strengths for both the I- and S-spin channels. At these low and easily attainable rf field strengths, level-crossing events among the energy levels |3/2 >, |1/2 >, | -1/2 >, | - 3/2 > that are known to complicate the CPMAS of quadrupolar nuclei, are mostly avoided. Zero- and double-quantum polarization transfer modes, akin to those we have observed for 1(1/2) -> S(1/2) polarization transfers, were evidenced by these analyses even in the presence of the quadrupolar interaction. H-1-Na-23 and H-1-B-11 BRAIN-CPMAS conditions were experimentally explored on model compounds by optimizing the width of the adiabatic sweep, as well as the rf pulse powers of the H-1 and Na-23/B-11 channels, for different MAS rates. The experimental data obtained on model compounds containing spin-3/2 nuclides, matched well predictions from numerical simulations and from an average Hamiltonian theory model. Extensions to half-integer spin nuclides with higher spins and potential applications of this BRAIN-CPMAS approach are discussed. (C) 2017 Elsevier Inc. All rights reserved.
Identifier: FSU_libsubv1_wos_000399861500017 (IID), 10.1016/j.jmr.2017.02.021 (DOI)
Keywords: resonance, spectroscopy, solid-state nmr, Adiabatic inversion, brain-cpmas, dynamic nuclear-polarization, Frequency-sweep, Half-integer quadrupolar nuclei, operator-formalism, quantum nmr, sequence, wurst
Publication Note: The publisher's version of record is available at
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Host Institution: FSU
Is Part Of: Journal of Magnetic Resonance.
Issue: vol. 277

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Wi, S., Kim, C., Schurko, R., & Frydman, L. (2017). Adiabatic Sweep Cross-polarization Magic-angle-spinning Nmr Of Half-integer Quadrupolar Spins. Journal Of Magnetic Resonance. Retrieved from