We demonstrate that dynamic nuclear polarization (DNP)-enhanced 1H-X heteronuclear correlation (HETCOR) measurements of hydrogen-rich surface species are better accomplished by using proton-free solvents. This approach notably prevents HETCOR spectra from being obfuscated by the solvent-derived signals otherwise present in DNP measurements. Additionally, in the hydrogen-rich materials studied here, which included functionalized mesoporous silica nanoparticles and metal organic frameworks, the use of proton-free solvents afforded higher sensitivity gains than the commonly used solvents containing protons. We also explored the possibility of using a solvent-free sample formulation and the feasibility of indirect detection in DNP-enhanced HETCOR experiments.
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Improved strategies for DNP-enhanced 2D 1H-X heteronuclear correlation spectroscopy of surfaces #DNPNMR
From The DNP-NMR Blog:
Improved strategies for DNP-enhanced 2D 1H-X heteronuclear correlation spectroscopy of surfaces #DNPNMR
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Kobayashi, T., et al., Improved strategies for DNP-enhanced 2D 1H-X heteronuclear correlation spectroscopy of surfaces. Solid State Nucl Magn Reson, 2017. 87(Supplement C): p. 38-44.
https://www.ncbi.nlm.nih.gov/pubmed/28834782
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11-28-2017 03:58 AM
Chemical-shift-resolved (1)(9)F NMR spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-enhanced diagonal suppressed correlation spectroscopy
From The DNP-NMR Blog:
Chemical-shift-resolved (1)(9)F NMR spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-enhanced diagonal suppressed correlation spectroscopy
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George, C. and N. Chandrakumar, Chemical-shift-resolved (1)(9)F NMR spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-enhanced diagonal suppressed correlation spectroscopy. Angew Chem Int Ed Engl, 2014. 53(32): p. 8441-4.
https://www.ncbi.nlm.nih.gov/pubmed/24962142
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03-13-2017 03:04 PM
[NMR paper] A Different Approach to Multiplicity-Edited Heteronuclear Single Quantum Correlation Spectroscopy
A Different Approach to Multiplicity-Edited Heteronuclear Single Quantum Correlation Spectroscopy
Publication date: Available online 8 August 2015
Source:Journal of Magnetic Resonance</br>
Author(s): Peyman Sakhaii, Wolfgang Bermel</br>
A new experiment for recording multiplicity-edited HSQC spectra is presented. In standard multiplicity-edited HSQC experiments, the amplitude of CH2 signals is negative compared to those of CH and CH3 groups. We propose to reverse the sign of 13C frequencies of CH2 groups in t1 as criteria for editing. Basically, a modified r,x...
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08-08-2015 12:17 PM
Chemical-Shift-Resolved19F NMR Spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-Enhanced Diagonal Suppressed Correlation Spectroscopy
From The DNP-NMR Blog:
Chemical-Shift-Resolved19F NMR Spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-Enhanced Diagonal Suppressed Correlation Spectroscopy
George, C. and N. Chandrakumar, Chemical-Shift-Resolved19F NMR Spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-Enhanced Diagonal Suppressed Correlation Spectroscopy. Angewandte Chemie, 2014. 126(32): p. 8581-8584.
http://dx.doi.org/10.1002/ange.201402320
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01-21-2015 08:39 PM
Chemical-Shift-Resolved19F NMR Spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-Enhanced Diagonal Suppressed Correlation Spectroscopy
From The DNP-NMR Blog:
Chemical-Shift-Resolved19F NMR Spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-Enhanced Diagonal Suppressed Correlation Spectroscopy
George, C. and N. Chandrakumar, Chemical-Shift-Resolved19F NMR Spectroscopy between 13.5 and 135 MHz: Overhauser-DNP-Enhanced Diagonal Suppressed Correlation Spectroscopy. Angewandte Chemie, 2014. 126(32): p. 8581-8584.
http://dx.doi.org/10.1002/ange.201402320
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01-16-2015 09:09 PM
Origin and removal of mixed-phase artifacts in gradient sensitivity enhanced heteronuclear single quantum correlation spectra
Origin and removal of mixed-phase artifacts in gradient sensitivity enhanced heteronuclear single quantum correlation spectra
Abstract Here we describe phasing anomalies observed in gradient sensitivity enhanced 15N-1H HSQC spectra, and analyze their origin. It is shown that, as a result of 15N off-resonance effects, dispersive contributions to the 1H signal become detectable, and lead to 15N-offset dependent phase errors. Strategies that effectively suppress these artifacts are presented.
Content Type Journal Article
Category Article
Pages 199-207
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09-30-2011 08:01 PM
1H Assisted 13C/15N Heteronuclear Correlation Spectroscopy in Oriented Sample Solid-State NMR of Single Crystal and Magnetically Aligned Samples
1H Assisted 13C/15N Heteronuclear Correlation Spectroscopy in Oriented Sample Solid-State NMR of Single Crystal and Magnetically Aligned Samples
Publication year: 2011
Source: Journal of Magnetic Resonance, In Press, Accepted Manuscript, Available online 9 April 2011</br>
Eugene C., Lin , Stanley J., Opella</br>
1H-irradiation under mismatched Hartmann-Hahn conditions provides an alternative mechanism for carrying out 15N/13C transfers in triple-resonance heteronuclear correlation spectroscopy (HETCOR) on stationary samples of single crystals and aligned samples of biopolymers, which...
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04-10-2011 12:52 PM
1H Assisted 13C/15N Heteronuclear Correlation Spectroscopy in Oriented Sample Solid-State NMR of Single Crystal and Magnetically Aligned Samples
1H Assisted 13C/15N Heteronuclear Correlation Spectroscopy in Oriented Sample Solid-State NMR of Single Crystal and Magnetically Aligned Samples
Publication year: 2011
Source: Journal of Magnetic Resonance, In Press, Accepted Manuscript, Available online 9 April 2011</br>
Eugene C., Lin , Stanley J., Opella</br>
1H-irradiation under mismatched Hartmann-Hahn conditions provides an alternative mechanism for carrying out 15N/13C transfers in triple-resonance heteronuclear correlation spectroscopy (HETCOR) on stationary samples of single crystals and aligned samples of biopolymers, which...