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.
Kobayashi, Takeshi, et al. "Improved strategies for DNP-enhanced 2D <sup>1</sup> H-X heteronuclear correlation spectroscopy of surfaces." Solid State Nuclear Magnetic Resonance, vol. 87, no. C, Aug. 2017. 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., & Pruski, Marek (2017). Improved strategies for DNP-enhanced 2D <sup>1</sup> H-X heteronuclear correlation spectroscopy of surfaces. Solid State Nuclear Magnetic Resonance, 87(C). https://doi.org/10.1016/j.ssnmr.2017.08.002
Kobayashi, Takeshi, Perras, Frederic A., Chaudhary, Umesh, et al., "Improved strategies for DNP-enhanced 2D <sup>1</sup> H-X heteronuclear correlation spectroscopy of surfaces," Solid State Nuclear Magnetic Resonance 87, no. C (2017), https://doi.org/10.1016/j.ssnmr.2017.08.002
@article{osti_1399263,
author = {Kobayashi, Takeshi and Perras, Frederic A. and Chaudhary, Umesh and Slowing, Igor I. and Huang, Wenyu and Sadow, Aaron D. and Pruski, Marek},
title = {Improved strategies for DNP-enhanced 2D <sup>1</sup> H-X heteronuclear correlation spectroscopy of surfaces},
annote = {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},
url = {https://www.osti.gov/biblio/1399263},
journal = {Solid State Nuclear Magnetic Resonance},
issn = {ISSN 0926-2040},
number = {C},
volume = {87},
place = {United States},
publisher = {Elsevier},
year = {2017},
month = {08}}