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Title: 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:
 [1];  [1];  [2];  [3];  [3];  [3];  [3]
  1. Ames Lab., Ames, IA (United States)
  2. Iowa State Univ., Ames, IA (United States)
  3. 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
Report Number(s):
IS-J-9361
Journal ID: ISSN 0926-2040; PII: S0926204017300644
Grant/Contract Number:  
AC02-07CH11358
Resource Type:
Journal Article: 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. doi: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. doi: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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