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Methylene spectral editing in solid-state 13C NMR by three-spin coherence selection

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Title: Methylene spectral editing in solid-state 13C NMR by three-spin coherence selection
Authors: Mao, J.-D., Schmidt-Rohr, K. srohr@iastate.edu
Source: Journal of Magnetic Resonance. Sep2005, Vol. 176 Issue 1, p1-6. 6p.
Subjects: Nuclear magnetic resonance, Ferromagnetism, Methyl groups, Humic acid
Abstract: Abstract: A robust new solid-state nuclear magnetic resonance (NMR) method for selecting CH2 signals in magic-angle spinning (MAS) 13C NMR spectra is presented. Heteronuclear dipolar evolution for a duration of 0.043ms, under MREV-8 homonuclear proton decoupling, converts 13C magnetization of CH2 groups into two- and three-spin coherences. The CH2 selection in the SIJ (C H H) spin system is based on the three-spin coherence S x I z J z , which is distinguished from 13C magnetization (S x ) by a 1H 0°/90° pulse consisting of two 45° pulses. The two-spin coherences of the type S y I z are removed by a 13C 90° x-pulse. The three-spin coherence is reconverted into magnetization during the remainder of the rotation period, still under MREV-8 decoupling. The required elimination of 13C chemical-shift precession is achieved by a prefocusing 180° pulse bracketed by two rotation periods. The selection of the desired three-spin coherence has an efficiency of 13% theoretically and of 8% experimentally relative to the standard CP/MAS spectrum. However, long-range couplings also produce some three-spin coherences of methine (CH) carbons. Therefore, the length of the 13C pulse flipping the two-spin coherences is increased by 12% to slightly invert the CH signals arising from two-spin coherences and thus cancel the signal from long-range three-spin coherences. The signal intensity in this cleaner spectrum is 6% relative to the regular CP/TOSS spectrum. The only residual signal is from methyl groups, which are suppressed at least sixfold relative to the CH2 peaks. The experiment is demonstrated on cholesteryl acetate and applied to two humic acids. [Copyright &y& Elsevier]
Copyright of Journal of Magnetic Resonance is the property of Academic Press Inc. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Label: Title
  Group: Ti
  Data: Methylene spectral editing in solid-state <superscript>13</superscript>C NMR by three-spin coherence selection
– Name: Author
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  Group: Au
  Data: <searchLink fieldCode="AR" term="%22Mao%2C+J%2E-D%2E%22">Mao, J.-D.</searchLink><br /><searchLink fieldCode="AR" term="%22Schmidt-Rohr%2C+K%2E%22">Schmidt-Rohr, K.</searchLink><i> srohr@iastate.edu</i>
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  Data: <searchLink fieldCode="JN" term="%22Journal+of+Magnetic+Resonance%22">Journal of Magnetic Resonance</searchLink>. Sep2005, Vol. 176 Issue 1, p1-6. 6p.
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  Data: <searchLink fieldCode="DE" term="%22Nuclear+magnetic+resonance%22">Nuclear magnetic resonance</searchLink><br /><searchLink fieldCode="DE" term="%22Ferromagnetism%22">Ferromagnetism</searchLink><br /><searchLink fieldCode="DE" term="%22Methyl+groups%22">Methyl groups</searchLink><br /><searchLink fieldCode="DE" term="%22Humic+acid%22">Humic acid</searchLink>
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: Abstract: A robust new solid-state nuclear magnetic resonance (NMR) method for selecting CH2 signals in magic-angle spinning (MAS) 13C NMR spectra is presented. Heteronuclear dipolar evolution for a duration of 0.043ms, under MREV-8 homonuclear proton decoupling, converts 13C magnetization of CH2 groups into two- and three-spin coherences. The CH2 selection in the SIJ (C H H) spin system is based on the three-spin coherence S x I z J z , which is distinguished from 13C magnetization (S x ) by a 1H 0°/90° pulse consisting of two 45° pulses. The two-spin coherences of the type S y I z are removed by a 13C 90° x-pulse. The three-spin coherence is reconverted into magnetization during the remainder of the rotation period, still under MREV-8 decoupling. The required elimination of 13C chemical-shift precession is achieved by a prefocusing 180° pulse bracketed by two rotation periods. The selection of the desired three-spin coherence has an efficiency of 13% theoretically and of 8% experimentally relative to the standard CP/MAS spectrum. However, long-range couplings also produce some three-spin coherences of methine (CH) carbons. Therefore, the length of the 13C pulse flipping the two-spin coherences is increased by 12% to slightly invert the CH signals arising from two-spin coherences and thus cancel the signal from long-range three-spin coherences. The signal intensity in this cleaner spectrum is 6% relative to the regular CP/TOSS spectrum. The only residual signal is from methyl groups, which are suppressed at least sixfold relative to the CH2 peaks. The experiment is demonstrated on cholesteryl acetate and applied to two humic acids. [Copyright &y& Elsevier]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Journal of Magnetic Resonance is the property of Academic Press Inc. and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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RecordInfo BibRecord:
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        Value: 10.1016/j.jmr.2005.04.016
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      – Code: eng
        Text: English
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        PageCount: 6
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        Type: general
      – SubjectFull: Ferromagnetism
        Type: general
      – SubjectFull: Methyl groups
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      – SubjectFull: Humic acid
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      – TitleFull: Methylene spectral editing in solid-state 13C NMR by three-spin coherence selection
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              Text: Sep2005
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