Actions for Hydrogen and deuterium NMR of solids by magic-angle spinning [electronic resource].

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Hydrogen and deuterium NMR of solids by magic-angle spinning [electronic resource].

Published
Berkeley, Calif. : Lawrence Berkeley National Laboratory, 1982.
Oak Ridge, Tenn. : Distributed by the Office of Scientific and Technical Information, U.S. Dept. of Energy.
Physical Description
Pages: 225 : digital, PDF file
Additional Creators
Lawrence Berkeley National Laboratory and United States. Department of Energy. Office of Scientific and Technical Information
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Summary
The nuclear magnetic resonance of solids has long been characterized by very large specral broadening which arises from internuclear dipole-dipole coupling or the nuclear electric quadrupole interaction. These couplings can obscure the smaller chemical shift interaction and make that information unavailable. Two important and difficult cases are that of hydrogen and deuterium. The development of cross polarization, heteronuclear radiofrequency decoupling, and coherent averaging of nuclear spin interactions has provided measurement of chemical shift tensors in solids. Recently, double quantum NMR and double quantum decoupling have led to measurement of deuterium and proton chemical shift tensors, respectively. A general problem of these experiments is the overlapping of the tensor powder pattern spectra of magnetically distinct sites which cannot be resolved. In this work, high resolution NMR of hydrogen and deuterium in solids is demonstrated. For both nuclei, the resonances are narrowed to obtain liquid-like isotropic spectra by high frequency rotation of the sample about an axis inclined at the magic angle, ..beta../sub m/ = Arccos (3/sup -1/2/), with respect to the direction of the external magnetic field. For deuterium, the powder spectra were narrowed by over three orders of magnitude by magic angle rotation with precise control of ..beta... A second approach was the observation of deuterium double quantum transitions under magic angle rotation. For hydrogen, magic angle rotation alone could be applied to obtain the isotropic spectrum when H/sub D/ was small. This often occurs naturally when the nuclei are semi-dilute or involved in internal motion. In the general case of large H/sub D/, isotropic spectra were obtained by dilution of /sup 1/H with /sup 2/H combined with magic angle rotation. The resolution obtained represents the practical limit for proton NMR of solids.
Report Numbers
E 1.99:lbl-14200
lbl-14200
Subject(s)
Other Subject(s)
Note
Published through SciTech Connect.
10/01/1982.
"lbl-14200"
"DE83003634"
Eckman, R.R.
Funding Information
AC03-76SF00098
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