Improved strategies for DNP-enhanced 2D 1 H-X heteronuclear correlation spectroscopy of surfaces
Abstract
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. Here, we also explored the possibility of using a solvent-free sample formulation and the feasibility of indirect detection in DNP-enhanced HETCOR experiments.
- Authors:
-
- Ames Lab., Ames, IA (United States)
- Iowa State Univ., Ames, IA (United States)
- Ames Lab. and Iowa State Univ., Ames, IA (United States)
- Publication Date:
- Research Org.:
- Ames Laboratory (AMES), Ames, IA (United States)
- Sponsoring Org.:
- USDOE
- OSTI Identifier:
- 1399263
- Alternate Identifier(s):
- OSTI ID: 1495835
- Report Number(s):
- IS-J-9361
Journal ID: ISSN 0926-2040; PII: S0926204017300644
- Grant/Contract Number:
- AC02-07CH11358
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Solid State Nuclear Magnetic Resonance
- Additional Journal Information:
- Journal Volume: 87; Journal Issue: C; Journal ID: ISSN 0926-2040
- Publisher:
- Elsevier
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 36 MATERIALS SCIENCE; Dynamic nuclear polarization; Solid-state NMR; Heteronuclear correlation; Catalysis; Surface science
Citation Formats
Kobayashi, Takeshi, Perras, Frederic A., Chaudhary, Umesh, Slowing, Igor I., Huang, Wenyu, Sadow, Aaron D., and Pruski, Marek. Improved strategies for DNP-enhanced 2D 1 H-X heteronuclear correlation spectroscopy of surfaces. United States: N. p., 2017.
Web. doi:10.1016/j.ssnmr.2017.08.002.
Kobayashi, Takeshi, Perras, Frederic A., Chaudhary, Umesh, Slowing, Igor I., Huang, Wenyu, Sadow, Aaron D., & Pruski, Marek. Improved strategies for DNP-enhanced 2D 1 H-X heteronuclear correlation spectroscopy of surfaces. United States. https://doi.org/10.1016/j.ssnmr.2017.08.002
Kobayashi, Takeshi, Perras, Frederic A., Chaudhary, Umesh, Slowing, Igor I., Huang, Wenyu, Sadow, Aaron D., and Pruski, Marek. Sat .
"Improved strategies for DNP-enhanced 2D 1 H-X heteronuclear correlation spectroscopy of surfaces". United States. https://doi.org/10.1016/j.ssnmr.2017.08.002. https://www.osti.gov/servlets/purl/1399263.
@article{osti_1399263,
title = {Improved strategies for DNP-enhanced 2D 1 H-X heteronuclear correlation spectroscopy of surfaces},
author = {Kobayashi, Takeshi and Perras, Frederic A. and Chaudhary, Umesh and Slowing, Igor I. and Huang, Wenyu and Sadow, Aaron D. and Pruski, Marek},
abstractNote = {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. Here, we also explored the possibility of using a solvent-free sample formulation and the feasibility of indirect detection in DNP-enhanced HETCOR experiments.},
doi = {10.1016/j.ssnmr.2017.08.002},
journal = {Solid State Nuclear Magnetic Resonance},
number = C,
volume = 87,
place = {United States},
year = {Sat Aug 12 00:00:00 EDT 2017},
month = {Sat Aug 12 00:00:00 EDT 2017}
}
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