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

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- 93 -<br />

approximately 0.4 ppm. We remark in passing that a separate calc-<br />

ulation(99) has predicted that the bulk susceptibility effect will<br />

in fact be averaged out in a sample undergoing sufficiently rapid<br />

macroscopic rotation at the magic angle. The bulk susceptibility<br />

of the saturated Aid 3 reference solutions is unknown but can prob-<br />

ably be safely neglected in comparison to-the metal. It follows<br />

that the possible contribution of the sample bulk susceptibilities<br />

to the experimental Knight shift is less than the experimental error.<br />

(d) Other Effects. For small grain aluminium powders the Knight<br />

shift has been reported to be dependent upon particle size(100)9<br />

but this effect has only been detected at temperatures below 4K<br />

and for particle sizes under 100 Field dependent oscillations<br />

in the Knight shift due to the de Haas Van Alphen effect have been<br />

measured at very low temperatures(101). The magnitude of these<br />

oscillations is small and the average Knight shift value was found<br />

to be unaffected. Both of these effects should be negligible at<br />

room temperatures.<br />

In conclusion it can be stated that neglecting the possibility<br />

of unsuspected systematic errors, the experimental value of the<br />

isotropic Knight shift was 1640 ppm with a maximum possible error<br />

in measurement of ±1 ppm. If a possible contribution due to the<br />

bulk susceptibility of the aluminium samples is included the error<br />

limits should probably be extended to +1 and -2 ppm. From a detailed<br />

theoretical calculation . Shyu, Das and Gaspari(102) obtained<br />

'a value<br />

for the aluminium Knight shift of 1624 ppm. Although their analysis<br />

included a core polarization correction it did not take into account<br />

any possible differences in the chemical shift interaction<br />

of the

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