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

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- 96 -<br />

near the time origin. <strong>By</strong> using the solid echo (and Jeener and<br />

Brockaert) pulse sequence it was shown that the decay curves for<br />

sample (a) were Gaussian right back to the time origin. However<br />

this was not found to be the case for the other samples. Both<br />

the FIDs and the solid echo responses became more exponential<br />

than Gaussian close to zero time. The anomalously high values of<br />

second moment measured by other workers in samples similar to (c)<br />

are regarded generally as indicating the presence of a nuclear<br />

quadrupole interaction. If this is so, the validity of the data<br />

points predicted by the solid echo sequence is brought into quest-<br />

ion. The response following the 90-T-9090 sequence has been calc-<br />

ulated for those cases where the internal spin interactions arise<br />

either-from the dipolar coupling between spins<br />

(71) or from the<br />

first order quadrupole broadening in an imperfect cubic crystal<br />

but not a combination of the two. Nevertheless for times less<br />

than T2 the observed solid echoes were found to follow the shape<br />

of the FIDs. ' Consequently the FID dead time points were estimated<br />

so that the preliminary part of the decay envelope resembled the<br />

outline of the solid echo maximum.<br />

Experimental values of the second and fourth moments are recorded<br />

in Table 7.1. The large variation in the second moment values of<br />

the different specimens is indicative of the relative Lorentzian<br />

character of the experimental lineshapes. The errors quoted refer<br />

to the spread of measured values about the mean. The large error<br />

values given for samples (b) and (c) arise out of the variation in<br />

the tails of the transformed lineshapes caused by the uncertainty<br />

in fitting the dead time points. These estimates do not however<br />

include any consideration of the contribution to the second moment

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