Methyl Iodide D3

[NMR-CDCL3]

I have recently purchased Methyl Iodide D3 and ran an NMR. The spectra does not look too good. Can someone please tell me what is wrong with the material as my supplier refuses to take back the material. If there are impurities how can i purify it.

Thank you all in advance

Methyl Iodide-D3.pdf

[NMR-CDCL3]

Could someone help me please

[hypervalent_iodine]

Who was your supplier and what does the CD₃I look like?

 

Were your NMR tubes completely dry? I am not familiar with what solvent peaks look like in CD₃I, but I wonder if the 1.43ppm peak is water. This could be either because your tubes aren't dry or because the bottle has a small amount of water in it. Does it come with any drying agents and how has it been stored? Was it stored cold and pending the answer to that, did you use it cold or at room temp? Could you try adding a small amount of water of D₂O to a sample and running an NMR of that?

 

The 2.14 peak is residual CH₃I. Did you add TMS or something to the sample? Not sure what the 0 ppm peak is otherwise.

[BabcockHall]

My guess is that the 1.43 ppm peak is water in the deuterated chloroform (which is unlikely to be completely dry), but I don't see a residual HCCl₃ peak near 7.26 ppm. Did you use CDCl₃ as your NMR solvent? If you had some ICHD₂ it would show up as a 1:2:3:2:1 pentet. A C-13 spectrum might not be a bad idea, especially if your present sample is at sufficient concentration.

Edited February 12, 2016 by BabcockHall

[hypervalent_iodine]

I was under the impression that this was done neat, not in CDCl₃. Agree with doing a carbon NMR though.

[BabcockHall]

I wonder whether the peak at 2.09 ppm might be acetone. Some people clean their NMR tubes with acetone, and so seeing a little residual peak from it is not impossible.

[hypervalent_iodine]

Quite likely. Hard to know for sure until the OP gives more info.

[NMR-CDCL3]

Thank you everyone. The Peak at 0 is of grease and not TMS. As of now unable to use the product