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Title: Enhanced 1H-X D-HMQC performance through improved 1H homonuclear decoupling

Abstract

The sensitivity of solid-state NMR experiments that utilize 1H zero-quantum heteronuclear dipolar recoupling, such as D-HMQC, is compromised by poor homonuclear decoupling. This leads to a rapid decay of recoupled magnetization and an inefficient recoupling of long-range dipolar interactions, especially for nuclides with low gyromagnetic ratios. We investigated the use, in symmetry-based 1H heteronuclear recoupling sequences, of a basic R element that was principally designed for efficient homonuclear decoupling. By shortening the time required to suppress the effects of homonuclear dipolar interactions to the duration of a single inversion pulse, spin diffusion was effectively quenched and long-lived recoupled coherence lifetimes could be obtained. Furthermore we show, both theoretically and experimentally, that these modified sequences can yield considerable sensitivity improvements over the current state-of-the-art methods and applied them to the indirect detection of 89Y in a metal-organic framework.

Authors:
 [1]; ORCiD logo [2];  [1]; ORCiD logo [2];  [2]
  1. Ames Lab., Ames, IA (United States)
  2. Ames Lab. and Iowa State Univ., Ames, IA (United States)
Publication Date:
Research Org.:
Ames Lab., Ames, IA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1494939
Alternate Identifier(s):
OSTI ID: 1547877
Report Number(s):
IS-J-9865
Journal ID: ISSN 0926-2040
Grant/Contract Number:  
AC02-07CH11358
Resource Type:
Accepted Manuscript
Journal Name:
Solid State Nuclear Magnetic Resonance
Additional Journal Information:
Journal Volume: 98; Journal Issue: C; Journal ID: ISSN 0926-2040
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY; Heteronuclear correlation; Homonuclear decoupling; Solid-state NMR; Symmetry-based recoupling

Citation Formats

Perras, Frédéric A., Goh, Tian Wei, Wang, Lin -Lin, Huang, Wenyu, and Pruski, Marek. Enhanced 1H-X D-HMQC performance through improved 1H homonuclear decoupling. United States: N. p., 2019. Web. doi:10.1016/j.ssnmr.2019.01.001.
Perras, Frédéric A., Goh, Tian Wei, Wang, Lin -Lin, Huang, Wenyu, & Pruski, Marek. Enhanced 1H-X D-HMQC performance through improved 1H homonuclear decoupling. United States. https://doi.org/10.1016/j.ssnmr.2019.01.001
Perras, Frédéric A., Goh, Tian Wei, Wang, Lin -Lin, Huang, Wenyu, and Pruski, Marek. Thu . "Enhanced 1H-X D-HMQC performance through improved 1H homonuclear decoupling". United States. https://doi.org/10.1016/j.ssnmr.2019.01.001. https://www.osti.gov/servlets/purl/1494939.
@article{osti_1494939,
title = {Enhanced 1H-X D-HMQC performance through improved 1H homonuclear decoupling},
author = {Perras, Frédéric A. and Goh, Tian Wei and Wang, Lin -Lin and Huang, Wenyu and Pruski, Marek},
abstractNote = {The sensitivity of solid-state NMR experiments that utilize 1H zero-quantum heteronuclear dipolar recoupling, such as D-HMQC, is compromised by poor homonuclear decoupling. This leads to a rapid decay of recoupled magnetization and an inefficient recoupling of long-range dipolar interactions, especially for nuclides with low gyromagnetic ratios. We investigated the use, in symmetry-based 1H heteronuclear recoupling sequences, of a basic R element that was principally designed for efficient homonuclear decoupling. By shortening the time required to suppress the effects of homonuclear dipolar interactions to the duration of a single inversion pulse, spin diffusion was effectively quenched and long-lived recoupled coherence lifetimes could be obtained. Furthermore we show, both theoretically and experimentally, that these modified sequences can yield considerable sensitivity improvements over the current state-of-the-art methods and applied them to the indirect detection of 89Y in a metal-organic framework.},
doi = {10.1016/j.ssnmr.2019.01.001},
journal = {Solid State Nuclear Magnetic Resonance},
number = C,
volume = 98,
place = {United States},
year = {Thu Jan 10 00:00:00 EST 2019},
month = {Thu Jan 10 00:00:00 EST 2019}
}

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