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Issue 6, 2016
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High resolution triple resonance micro magic angle spinning NMR spectroscopy of nanoliter sample volumes

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Abstract

To be able to study mass-limited samples and small single crystals, a triple resonance micro-magic angle spinning (μMAS) probehead for the application of high-resolution solid-state NMR of nanoliter samples was developed. Due to its excellent rf performance this allows us to explore the limits of proton NMR resolution in strongly coupled solids. Using homonuclear decoupling we obtain unprecedented 1H linewidths for a single crystal of glycine (Δν(CH2) = 0.14 ppm) at high field (20 T) in a directly detected spectrum. The triple channel design allowed the recording of high-resolution μMAS 13C–15N correlations of [U-13C–15N] arginine HCl and shows that the superior 1H resolution opens the way for high-sensitivity inverse detection of heteronuclei even at moderate spinning speeds and rf-fields. Efficient decoupling leads to long coherence times which can be exploited in many correlation experiments.

Graphical abstract: High resolution triple resonance micro magic angle spinning NMR spectroscopy of nanoliter sample volumes

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Supplementary files

Article information


Submitted
20 Dec 2015
Accepted
14 Jan 2016
First published
15 Jan 2016

Phys. Chem. Chem. Phys., 2016,18, 4902-4910
Article type
Paper
Author version available

High resolution triple resonance micro magic angle spinning NMR spectroscopy of nanoliter sample volumes

J. O. Brauckmann, J. W. G. (. Janssen and A. P. M. Kentgens, Phys. Chem. Chem. Phys., 2016, 18, 4902
DOI: 10.1039/C5CP07857A

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