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JOURNAL ARTICLE
RESEARCH SUPPORT, NON-U.S. GOV'T
RESEARCH SUPPORT, U.S. GOV'T, NON-P.H.S.
Adiabatic sweep cross-polarization magic-angle-spinning NMR of half-integer quadrupolar spins.
Journal of Magnetic Resonance 2017 April
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 (1 H), 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 I(1/2)→S(1/2) polarization transfers, were evidenced by these analyses even in the presence of the quadrupolar interaction. 1 H-23 Na and 1 H-11 B 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 1 H and 23 Na/11 B 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.
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