I distilled off dichloromethane (DCM) from a mixture of epichlorohydrin (ECH)/DCM. How can I confirm all DCM is gone?
I would appreciate if someone suggest me any better separation method rather than distillation.
Hi Ehsan
DCM boils at approximately 40 degrees, so you should be confident its all gone if you are using rotary evaporator at 40 degrees under vacuum. I think the epoxide ring of your sample should survive this condition. If your sample is not thermally stable, you may consider using a vacuum desiccator or purging with Nitrogen gas. DCM is volatile and it should be easy to get rid of it completely.
I hope this helps.
Kavnen,
Thank you for your answer. I did the same but now I want to prove that no DCM is left. How should I do that?
Hi Ehsan
I can't think of any test at the moment save NMR, or mass spec techniques. I recommend NMR in any deuterated solvent of choice. If you use CDCl3, you should see a singlet DCM peak around 5.3ppm (I think) if there's still residual DCM. The peak should be absent if no DCM is left.
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