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Rotational spin echoes and high resolution NMR in powders

✍ Scribed by Matti Maricq; J.S. Waugh


Publisher
Elsevier Science
Year
1977
Tongue
English
Weight
276 KB
Volume
47
Category
Article
ISSN
0009-2614

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✦ Synopsis


When a powder having linewidth A arising from inhomogeneous second-rank tensor interactions is rotated about the magic axis at trot < A, the free induction decay is a spin echo train, the Fourier transform of whose envelope is the isotropic spectrum.

In obtaining isotropic chemical shift spectra of 13C in powders by combining

[ 1 ] strong proton decoupling [2] with magic-angle sample spinning [3] it might be thought that one would require spinning frequencies vr % A, A being the width of the powder pattern arising from anisotropic chemical shifts. While this is indeed the criterion for complete collapse to the isotropic resonance, Lippmaa et al. [4] and subsequently Stejskal et al. [S] have strikingly demonstrated that much slower spinning suffices to break up the powder pattern into an array of spinning sidebands of width 6 & A; the criterion for this behavior is vr > 6.

We have studied what amounts to the same phenomenon from a different point of view which is generally illuminating and leads to a greatly simplified method for obtaining the isotropic spectrum. We believe that this method is applicable to a considerably wider class of powder spectra, including in particular 2H resonances, from which isotropic proton chemical shifts can be extracted as precisely as and more simply than by competitive methods [6,7], though perhaps at soln= penalty in sensitivity.


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