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Thursday, October 28, 2010

13C NMR of "Perdeuterated" Solvents

When one acquires a 13C NMR spectrum of a sample, the deuterated solvent is observed with resonances characterized by the J coupling pattern of the deuterons attached to the carbon atoms. (CD = 1:1:1 triplet, CD2 = 1:2:3:2:1 quintet, CD3 = 1:3:6:7:6:3:1 septet). Often, however; small peaks are observed near the main solvent resonances. These are due to other isotopomers of the solvent. An example of this is shown in the bottom spectrum of the figure below for the high frequency resonance of "THF-d8". The spectrum consists mainly of the expected 1:2:3:2:1 quintet however, there is a small peak present on the high frequency side of the quintet marked by the arrow. It is due to one of the components of the C1 resonance from THF-1,2,2,3,3,4,4-d7. The supplier of the solvent claims that the isotopic purity is 99.5 atom % D. If the deuteration is uniform, approximately 0.5 % of the molecules will contain a single proton. Half of these molecules will be mono-protonated on the high frequency carbons. If a DEPT spectrum is acquired on the same sample, the non-protonated carbons are suppressed leaving only the mono-protonated carbons. This is shown in the top spectrum of the figure, which shows a 1:1:1 triplet from CHD. The isotope shift between CHD and CD2 is 0.354 ppm. Other examples can be found here and here.

1 comment:

John said...

I always wondered what that little peak was. I thought I just had trace impurity that I would ignore...

Thanks Glen, and good to see a new post!