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Improved strategies for DNP-enhanced 2D H-1-X heteronuclear correlation spectroscopy of surfaces

TitleImproved strategies for DNP-enhanced 2D H-1-X heteronuclear correlation spectroscopy of surfaces
Publication TypeJournal Article
Year of Publication2017
AuthorsKobayashi, T, Perras, FA, Chaudhary, U, Slowing, II, Huang, WK, Sadow, AD, Pruski, M
JournalSolid State Nuclear Magnetic Resonance
Volume87
Pagination38-44
Date Published10
Type of ArticleArticle
ISBN Number0926-2040
Accession NumberWOS:000415816200006
Keywordsabundance, catalysis, chemistry, correlation, dynamic nuclear polarization, dynamic nuclear-polarization, efficient, Heteronuclear, high-frequency, Mesoporous silica nanoparticles, metal-organic frameworks, n-15 nmr, physics, proteins, sensitivity enhancement, solid-state nmr, Spectroscopy, surface science
Abstract

We demonstrate that dynamic nuclear polarization (DNP)-enhanced H-1-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.

DOI10.1016/j.ssnmr.2017.08.002
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