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

被引:7
作者
Sorensen, Morten K. [1 ,2 ]
Bakharev, Oleg [1 ,2 ]
Jensen, Ole [3 ]
Jakobsen, Hans J. [2 ,4 ]
Skibsted, Jorgen [2 ,4 ]
Nielsen, Niels Chr. [1 ,2 ]
机构
[1] Aarhus Univ, Ctr Insoluble Prot Struct InSPIN, Interdisciplinary Nanosci Ctr iNANO, DK-8000 Aarhus C, Denmark
[2] Aarhus Univ, Dept Chem, DK-8000 Aarhus C, Denmark
[3] Nanonord AS, DK-9220 Aalborg O, Denmark
[4] Aarhus Univ, Instrument Ctr Solid State NMR Spect, Interdisciplinary Nanosci Ctr iNANO, DK-8000 Aarhus C, Denmark
基金
新加坡国家研究基金会;
关键词
Low-field NMR; Magic-angle spinning; Na-23 second-order quadrupolar coupling; P-31-F-19 dipole-dipole coupling; Sodium nitrate; Potassium monofluorophosphate; MAGNETIC-FIELD; SHIELDING TENSORS; SPECTROSCOPY; MOUSE; FOOD; QUADRUPOLE; SIMPSON; NUCLEI; SENSOR; ARRAY;
D O I
10.1016/j.jmr.2013.10.015
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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 Na-23 MAS NMR with enhanced second-order quadrupolar coupling effects and P-31 MAS NMR where reduced influence from chemical shift anisotropy at low field may facilitate determination of heteronuclear dipole-dipole couplings. (C) 2013 Elsevier Inc. All rights reserved.
引用
收藏
页码:20 / 25
页数:6
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