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Mark Ornoff

What could cause a peak to split into 2 resonances as temperature increases in NMR spectroscopy

Amita Dey  Follow

Since I do not know which compound it is, my guess is that you have two different $\ce{H^1}$ that have almost the same chemical shift at room temperature. The chemical shifts change with temperature as for instance in sucrose:

enter image description here

Here are represented mainly the $\ce{H^1}$ of the $\ce{-OH}$ but the $\ce{C-H}$ (the peak of 1) shifts also.

In your case, one is almost fixed, while the other one moves to higher $\delta$ and, therefore, they split into two.

More info on the sucrose spectrum here.

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