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

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- 88 -<br />

Lorentzian NMR lineshape of Aid 3 solution depends in the first<br />

instance upon the homogeneity of the external magnetic field.<br />

On the other hand the 27A1 resonance line is approximately Gauss-<br />

ian with a width of about 9 kHz. Even if the line centre is<br />

located to an accuracy of 2% of the width the greatest accuracy<br />

to which the Knight shift can be determined in a magnetic field<br />

of around 1 tesla is ±0.02 x<br />

10 3.<br />

Aluminium has a cubic structure at room temperature with only<br />

one naturally occurring isotope. The broadening of the resonance<br />

line from a pure annealed powdered specimen of this metal arises<br />

from the magnetic dipolar interaction between nuclei. The rapid<br />

rotation technique can be used therefore to narrow the resonance<br />

lineshäpe. This enables the line centre and hence the Knight<br />

shift to be determined to a correspondingly greater accuracy.<br />

7.2.2 MEASUREMENTS<br />

Experimental measurements were undertaken following the<br />

procedure described in Section 5.5. Using compressed air, rotors<br />

containing the aluminium powder samples were spun about the magic<br />

angle at spinning frequencies of about'4 kHz. At these speeds the<br />

width of the resonance lineshape is reduced by a factor of approxi-<br />

mately 15. (Typical FIDs and Fourier transformed lineshapes<br />

obtained from static and rotating pure powder specimens are included<br />

in Figures 7.1 and 7.2 respectively. ) The reference material<br />

used was a saturated aqueous solution of 99.999% pure A1C13 as<br />

supplied by Johnson Matthey Chemicals. The solution was enclosed<br />

inside a nylon container, the internal dimensions of which were

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