P. 1
NMR

NMR

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Published by: Maulana Senjaya Susilo on Feb 11, 2011
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05/16/2013

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The effects from chemical shift anisotropy and dipolar couplings lead to excessively

broad lines. To a large extend this line-broadening can be removed by spinning the

sample about the magic angle 54.74° (magic-angle spinning, MAS). For this angle the

second-order legendre polynomial (3cos2

β-1)/2, which describes the angular depen-
dence in both the dipolar coupling as well as in the chemical shift Hamiltonians, van-

ishes. In MAS, the sample is placed in a cylindrical rotor which is rapidly spun (up to

30-50 kHz) about an axis that is tilted by 54° away from the direction of the static field.

The tremendous line-narrowing effects due to MAS are displayed in the powder 13

C

spectra of 13

C,15

N labeled glycine below (from ref. Williamson et al.):

At the lower frequencies spinning sidebands fall into the spectral regions of interest.

Upon rising the spinning frequencies those bands occur outside the spectral region. The

broad lines observed in the powder spectrum collapse into rather sharp lines which

occur at the position of the isotropic chemical shift.

Unfortunately spinning the samples at high frequencies does heat up the sample (tens

of degrees!) and the heating effect must be removed by cooling the rotor appropriately.

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