solid state nmr – part 2 · 2013-04-10 · then connected to the input pulley of the nmr probe as...
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Solid state NMR –Part 2
- Chapter 14, on web site: http://www.chem.ubc.ca/faculty/straus/c518_09.html
A) Averaging – Magic angle sample spinning
B) Polarization transfer - CP
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Interactions in solid state
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Chemical shift:
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Spherical tensor notation:
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where
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Dipolar interaction:
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How averaging of CSA works under MAS:
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average A20
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In the LAB frame:
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Or rewritten in a different way:
FT
signal at isotropic chemical shift, with sidebands due to theterm
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e.g. 13C spectrum ofalanine
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Alternative methods: Magic angle hopping and Magic angle turning
MAS continuous rotation, averaging over a full rotation
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Given
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Final result:
= 0
How is this achieved experimentally?
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Analogous approach: magic angle turning
rotor is synchronized so that signal is detected at the appropriate angles (120° apart) requires slow spinning
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A quick look at MAS and quadrupolar nuclei:
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To average the P4 term completely dynamic angle spinning (DAS) ordouble rotation (DOR)
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B) Cross-polarization
Why use it? To enhance sensitivity (analogous to INEPT in solution state)
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oscillations proportional todipolar coupling constant
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Dipolar oscillations PISEMA