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NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...

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- 41 -<br />

of as forming a continuum of sidebands which become unobservably<br />

weak; hence resulting in the characteristic Lorentzian line-<br />

shape. For macroscopic sample rotation at the magic angle the<br />

central component of the absorption spectrum is flanked by a series<br />

of sidebands at integer multiples of vr. As the rotation rate is<br />

increased these sidebands move further out and become less intense.<br />

When yr is greater than the linewidth the intensity of the satellites<br />

falls as Vr -2n for the nth satellite, thus preserving the total<br />

second moment. Both the central component and the satellites have<br />

a finite width which decreases with increasing spinning frequency(43,44)<br />

Accurate adjustment of the magic angle is an important criter-<br />

ion in achieving a minimum linewidth. A reduction of the dipolar<br />

linewidth to 1% of its original value requires that the magic angle<br />

is set to an accuracy of better than half a degree. Such an<br />

adjustment can best be performed empirically by direct observat-<br />

ion of the FID from the rotated sample. With the assumption that<br />

there is no antisymmetric component of the spin-spin interaction<br />

the fully resolved central spectrum for any solid rotated about<br />

the magic axis is determined by the Hamiltonian<br />

, ýl° a -3i yß(1 -a)I. HO +I 3.. I.. Iý<br />

J 1J<br />

the same as that relating to fluids in high resolution NMR.<br />

In practice complete resolution of the central line from the<br />

first spinning sidebands flanking it either side is dependent upon<br />

the frequency of rotation. The faster the sample is spun the<br />

greater likelihood there is of attaining some rotationally invar-<br />

iant limit. There have been several suggestions as to the manner<br />

in which the residual dipolar broadening of the central spectrum<br />

varies with rotation<br />

rate,<br />

(33<br />

34,38,45,46)<br />

,<br />

However experimental<br />

(3.17)

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