Publication Date

8-11-2020

Department

Ames Laboratory; Chemistry

Campus Units

Ames Laboratory, Chemistry

OSTI ID+

1668253

Report Number

IS-J 10314

DOI

10.1016/j.ssnmr.2020.101685

Journal Title

Solid State Nuclear Magnetic Resonance

Volume Number

109

First Page

101685

Abstract

Dynamic nuclear polarization (DNP) and indirect detection are two commonly applied approaches for enhancing the sensitivity of solid-state NMR spectroscopy. However, their use in tandem has not yet been investigated. With the advent of low-temperature fast magic angle spinning (MM) probes with 1.3-mm diameter rotors capable of MAS a 40 kHz it becomes feasible to combine these two techniques. In this study, we performed DNP-enhanced 2D indirectly detected heteronuclear correlation (idHETCOR) experiments on C-13, N-15, Cd-113 and 89 Y nuclei in functionalized mesoporous silica, CdS nanoparticles, and Y2O3 nanoparticles. The sensitivity of the 2D idHETCOR experiments was compared with those of DNP-enhanced directly-detected 1D cross polarization (CP) and 2D HETCOR experiments performed with a standard 3.2-mm rotor. Due to low CP polarization transfer efficiencies and large proton linewidth, the sensitivity gains achieved by indirect detection alone were lower than in conventional (non-DNP) experiments. Nevertheless, despite the smaller sample volume the 2D idHETCOR experiments showed better absolute sensitivities than 2D HETCOR experiments for nuclei with the lowest gyromagnetic ratios. For Y-89, 2D idHETCOR provided 8.2 times better sensitivity than the 1 (DY)-Y-89-detected CP experiment performed with a 3.2-mm rotor.

DOE Contract Number(s)

AC02-07CH11358

Language

en

Publisher

Iowa State University Digital Repository, Ames IA (United States)

IS-J 10314 SI.pdf (104 kB)
Supplementary Information

Available for download on Wednesday, August 11, 2021

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