PMID: 9178419Mar 1, 1997Paper

Multiple-quantum magic-angle spinning and dynamic-angle spinning NMR spectroscopy of quadrupolar nuclei

Solid State Nuclear Magnetic Resonance
S H WangAlexander Pines

Abstract

Several aspects of the Multiple-Quantum Magic-Angle Spinning (MQMAS) technique (L. Frydman and J.S. Harwood, J. Am. Chem. Soc., 117 (1995) 5367) are compared with Dynamic-Angle Spinning (DAS). Examples of MQMAS spectra are shown for I = 3/2 nuclei with CQ up to 3.6 MHz, and for 27Al (I = 5/2) with CQ up to 10 MHz. The MQMAS linewidth is largely independent of the magnitude of the homonuclear dipolar interaction, while the spinning sideband manifold is similar to that observed in DAS experiments. MQMAS is technically simple and routinely useful for studying nuclei with short spin-lattice relaxation times, but care must be taken in its use for quantitative studies as the excitation of the triple-quantum coherence is not uniform. In this regard, MQMAS is most useful for samples with small quadrupolar coupling constants. In the specific case of 17O, DAS would give spectra with excellent resolution in comparison to MQMAS. The different advantages of DAS and MQMAS make them useful complementary techniques in many cases. Two additional methods are also presented for extracting the chemical shift anisotropy (CSA) directly for quadrupolar nuclei using the multiple-quantum scheme.

References

Apr 1, 1993·Solid State Nuclear Magnetic Resonance·J P Amoureux
Jan 1, 1996·Solid State Nuclear Magnetic Resonance·C Fernandez, J P Amoureux
Feb 1, 1996·Solid State Nuclear Magnetic Resonance·D MassiotP J Grandinetti

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Citations

Mar 14, 2003·Solid State Nuclear Magnetic Resonance·Ulla Gro NielsenJørgen Skibsted
May 29, 1998·Solid State Nuclear Magnetic Resonance·J P Amoureux, C Fernandez
Jul 30, 2010·Progress in Nuclear Magnetic Resonance Spectroscopy·Redouane HajjarPascal P Man
Apr 13, 2002·Solid State Nuclear Magnetic Resonance·Yannick Millot, Pascal P Man
Nov 4, 1998·Journal of Magnetic Resonance·S Ding, C A McDowell
May 26, 1999·Journal of Magnetic Resonance·A Medek, L Frydman
Jul 26, 2008·Journal of the American Chemical Society·Jason T AshPhilip J Grandinetti
Jul 21, 2006·The Journal of Physical Chemistry. B·Magali BenoitMark E Tuckerman

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