Measuring Long-Range 13C–13C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range 13C–13C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR]

Kobayashi, Takeshi; Slowing, Igor I.; Pruski, Marek

doi:10.1021/acs.jpcc.7b08841

Title: Measuring Long-Range ¹³C–¹³C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range ¹³C–¹³C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR]

Abstract

Here, we report that spatial (<1 nm) proximity between different molecules in solid bulk materials and, for the first time, different moieties on the surface of a catalyst, can be established without isotope enrichment by means of homonuclear CHHC solid-state nuclear magnetic resonance experiment. This ¹³C–¹³C correlation measurement, which hitherto was not possible for natural-abundance solids, was enabled by the use of dynamic nuclear polarization. Importantly, it allows the study of long-range correlations in a variety of materials with high resolution.

Authors:

Kobayashi, Takeshi ^[1];

^[2];

^[2]

Ames Lab., Ames, IA (United States)
Ames Lab. and Iowa State Univ., Ames, IA (United States)

Publication Date:: Fri Oct 13 00:00:00 EDT 2017

Research Org.:: Ames Lab., Ames, IA (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1408771

Report Number(s):: IS-J-9435
Journal ID: ISSN 1932-7447; TRN: US1703178

Grant/Contract Number:: AC02-07CH11358

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Physical Chemistry. C

Additional Journal Information:: Journal Volume: 121; Journal Issue: 44; Journal ID: ISSN 1932-7447

Publisher:: American Chemical Society

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Dynamic Nuclear Polarization; Solid-state NMR; homonuclear correlation; natural abundance; catalyst surface

Citation Formats


                    Kobayashi, Takeshi, Slowing, Igor I., and Pruski, Marek. Measuring Long-Range 13C–13C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range 13C–13C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR].  United States: N. p., 2017. 
Web.  doi:10.1021/acs.jpcc.7b08841.

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                    Kobayashi, Takeshi, Slowing, Igor I., & Pruski, Marek. Measuring Long-Range 13C–13C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range 13C–13C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR].  United States.  https://doi.org/10.1021/acs.jpcc.7b08841

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                    Kobayashi, Takeshi, Slowing, Igor I., and Pruski, Marek. Fri .  
"Measuring Long-Range 13C–13C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range 13C–13C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR]".  United States.  https://doi.org/10.1021/acs.jpcc.7b08841.  https://www.osti.gov/servlets/purl/1408771.

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@article{osti_1408771,

  title        = {Measuring Long-Range 13C–13C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range 13C–13C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR]},

  author       = {Kobayashi, Takeshi and Slowing, Igor I. and Pruski, Marek},

  abstractNote = {Here, we report that spatial (<1 nm) proximity between different molecules in solid bulk materials and, for the first time, different moieties on the surface of a catalyst, can be established without isotope enrichment by means of homonuclear CHHC solid-state nuclear magnetic resonance experiment. This 13C–13C correlation measurement, which hitherto was not possible for natural-abundance solids, was enabled by the use of dynamic nuclear polarization. Importantly, it allows the study of long-range correlations in a variety of materials with high resolution.},

  doi          = {10.1021/acs.jpcc.7b08841},

  journal      = {Journal of Physical Chemistry. C},

  number       = 44,

  volume       = 121,

  place        = {United States},

  year         = {Fri Oct 13 00:00:00 EDT 2017},

  month        = {Fri Oct 13 00:00:00 EDT 2017}

}

Copy to clipboard

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https://doi.org/10.1021/acs.jpcc.7b08841

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Untangling the Condensation Network of Organosiloxanes on Nanoparticles using 2D ²⁹ Si– ²⁹ Si Solid-State NMR Enhanced by Dynamic Nuclear Polarization
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Quantitative Structural Constraints for Organic Powders at Natural Isotopic Abundance Using Dynamic Nuclear Polarization Solid-State NMR Spectroscopy
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Mollica, Giulia; Dekhil, Myriam; Ziarelli, Fabio
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A New Tool for NMR Crystallography: Complete ¹³ C/ ¹⁵ N Assignment of Organic Molecules at Natural Isotopic Abundance Using DNP-Enhanced Solid-State NMR
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Direct Spectroscopic Evidence for Isolated Silanols in SiO _x /Al ₂ O ₃ and Their Formation Mechanism
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Spatial distribution of organic functional groups supported on mesoporous silica nanoparticles: a study by conventional and DNP-enhanced ²⁹ Si solid-state NMR
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Works referencing / citing this record:

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journal, December 2019

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Magnetic Resonance in Chemistry
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Title: Measuring Long-Range 13C–13C Correlations on a Surface under Natural Abundance Using Dynamic Nuclear Polarization-Enhanced Solid-State Nuclear Magnetic Resonance [Measuring Long Range 13C–13C Correlations on Surface under Natural Abundance Using DNP-enhanced Solid-state NMR]

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Citation Formats

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Broadband dipolar recoupling in the nuclear magnetic resonance of rotating solids: A compensated C7 pulse sequence journal, February 1998

Investigation of complex networks of spin-spin coupling by two-dimensional NMR journal, September 1981

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13C–1H dipolar-assisted rotational resonance in magic-angle spinning NMR journal, August 2001

Diluting Abundant Spins by Isotope Edited Radio Frequency Field Assisted Diffusion journal, May 2004

Improved magnetization transfer in solid-state NMR with fast magic angle spinning journal, February 2009

2D CP/MAS13C Isotropic Chemical Shift Correlation Established by1H Spin Diffusion journal, October 1998

Spin Diffusion with 13 C Selection and Detection for the Characterization of Morphology in Labeled Polymer Blends with MAS NMR journal, December 1998

2D13C–13C MAS NMR Correlation Spectroscopy with Mixing by True 1H Spin Diffusion Reveals Long-Range Intermolecular Distance Restraints in Ultra High Magnetic Field journal, August 2002

Structural Constraints from Proton-Mediated Rare-Spin Correlation Spectroscopy in Rotating Solids † journal, August 2002

CHHC and 1H–1H magnetization exchange: Analysis by experimental solid-state NMR and 11-spin density-matrix simulations journal, August 2009

Crystal Structure and Hydrogen-Bonding System in Cellulose Iβ from Synchrotron X-ray and Neutron Fiber Diffraction journal, August 2002

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Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization
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journal, September 2014

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journal, March 2015

A New Tool for NMR Crystallography: Complete ¹³ C/ ¹⁵ N Assignment of Organic Molecules at Natural Isotopic Abundance Using DNP-Enhanced Solid-State NMR
journal, October 2015

Atomic-Level Structure Characterization of Biomass Pre- and Post-Lignin Treatment by Dynamic Nuclear Polarization-Enhanced Solid-State NMR
journal, January 2017

Welcoming natural isotopic abundance in solid-state NMR: probing π-stacking and supramolecular structure of organic nanoassemblies using DNP
journal, January 2017

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Spatial distribution of organic functional groups supported on mesoporous silica nanoparticles: a study by conventional and DNP-enhanced ²⁹ Si solid-state NMR
journal, January 2017

Broadband dipolar recoupling in the nuclear magnetic resonance of rotating solids: A compensated C7 pulse sequence
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Investigation of complex networks of spin-spin coupling by two-dimensional NMR
journal, September 1981

Observation of spin exchange by two-dimensional fourier transform 13C cross polarization-magic-angle spinning
journal, May 1982

13C–1H dipolar-assisted rotational resonance in magic-angle spinning NMR
journal, August 2001

Diluting Abundant Spins by Isotope Edited Radio Frequency Field Assisted Diffusion
journal, May 2004

Improved magnetization transfer in solid-state NMR with fast magic angle spinning
journal, February 2009

2D CP/MAS13C Isotropic Chemical Shift Correlation Established by1H Spin Diffusion
journal, October 1998

Spin Diffusion with ¹³ C Selection and Detection for the Characterization of Morphology in Labeled Polymer Blends with MAS NMR
journal, December 1998

2D13C–13C MAS NMR Correlation Spectroscopy with Mixing by True 1H Spin Diffusion Reveals Long-Range Intermolecular Distance Restraints in Ultra High Magnetic Field
journal, August 2002

Structural Constraints from Proton-Mediated Rare-Spin Correlation Spectroscopy in Rotating Solids ^†
journal, August 2002

CHHC and 1H–1H magnetization exchange: Analysis by experimental solid-state NMR and 11-spin density-matrix simulations
journal, August 2009

Crystal Structure and Hydrogen-Bonding System in Cellulose Iβ from Synchrotron X-ray and Neutron Fiber Diffraction
journal, August 2002

Measurement of the local 1H spin-diffusion coefficient in polymers
journal, February 2006

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journal, January 2017

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