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J Magn Reson. 2014 Jan;238:20-5. doi: 10.1016/j.jmr.2013.10.015. Epub 2013 Nov 01.

Magic-angle spinning solid-state multinuclear NMR on low-field instrumentation.

Journal of magnetic resonance (San Diego, Calif. : 1997)

Morten K Sørensen, Oleg Bakharev, Ole Jensen, Hans J Jakobsen, Jørgen Skibsted, Niels Chr Nielsen

Affiliations

  1. Center for Insoluble Protein Structures (inSPIN), Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry, Aarhus University, Gustav Wieds Vej 14, DK-8000 Aarhus C, Denmark.
  2. Nanonord A/S, Skjernvej 4A, DK-9220 Aalborg Ø, Denmark.
  3. Instrument Centre for Solid-State NMR Spectroscopy, Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry, Aarhus University, Langelandsgade 140, DK-8000 Aarhus C, Denmark.
  4. Center for Insoluble Protein Structures (inSPIN), Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry, Aarhus University, Gustav Wieds Vej 14, DK-8000 Aarhus C, Denmark. Electronic address: [email protected].

PMID: 24291330 DOI: 10.1016/j.jmr.2013.10.015

Abstract

Mobile and cost-effective NMR spectroscopy exploiting low-field permanent magnets is a field of tremendous development with obvious applications for arrayed large scale analysis, field work, and industrial screening. So far such demonstrations have concentrated on relaxation measurements and lately high-resolution liquid-state NMR applications. With high-resolution solid-state NMR spectroscopy being increasingly important in a broad variety of applications, we here introduce low-field magic-angle spinning (MAS) solid-state multinuclear NMR based on a commercial ACT 0.45 T 62 mm bore Halbach magnet along with a homebuilt FPGA digital NMR console, amplifiers, and a modified standard 45 mm wide MAS probe for 7 mm rotors. To illustrate the performance of the instrument and address cases where the low magnetic field may offer complementarity to high-field NMR experiments, we demonstrate applications for (23)Na MAS NMR with enhanced second-order quadrupolar coupling effects and (31)P MAS NMR where reduced influence from chemical shift anisotropy at low field may facilitate determination of heteronuclear dipole-dipole couplings.

Copyright © 2013 Elsevier Inc. All rights reserved.

Keywords: (23)Na second-order quadrupolar coupling; (31)P–(19)F dipole–dipole coupling; Low-field NMR; Magic-angle spinning; Potassium monofluorophosphate; Sodium nitrate

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