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Topic: Spectroscopy question  (Read 3517 times)

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Offline kapital

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Spectroscopy question
« on: December 26, 2015, 09:11:50 AM »
If in an classical NMR analysis there is a solution of analyze and also some other (non-soluble) solid compound, would the spectrum show only soluble compound or both and why?
 Thanx for answers.

Offline Irlanur

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Re: Spectroscopy question
« Reply #1 on: December 27, 2015, 04:15:05 AM »
two aspects:

1) solid compounds show extremely broad spectra (this can be overcome by magic angle spinning). so if you have solid and liquid samples together, all you would see from the solid might be some "baseline noise". obviously this depends on the relative amounts in the sample.

2) solid particles in a solution can lead to huge field inhomogeneities, ("bulk susceptibility")  leading to broad lines (also of the liquid part). -> you should filter it if possible.

Offline kapital

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Re: Spectroscopy question
« Reply #2 on: December 27, 2015, 05:54:01 AM »
two aspects:

solid compounds show extremely broad spectra
What is the reason for that?

Am asking this more from theoretical than practical view.

Offline Irlanur

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Re: Spectroscopy question
« Reply #3 on: December 27, 2015, 06:34:41 AM »
Quote
What is the reason for that?

chemical shift anisotropy and dipolar couplings. The chemical shift depends on the orientation of the molecule wrt the external magnetic field. In solution, the tumbling is so fast that you only see the average, which gives you a sharp line. In a powdered sample (means: not a single crystal) you see a superposition of all orientations -> broad lines.

The dipolar coupling broadens all lines, but in solution the average is actually zero and is not directly observable in the spectrum.

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