NMR-CDCL3 Posted February 10, 2016 Share Posted February 10, 2016 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 Link to comment Share on other sites More sharing options...
NMR-CDCL3 Posted February 11, 2016 Author Share Posted February 11, 2016 Could someone help me please Link to comment Share on other sites More sharing options...
hypervalent_iodine Posted February 11, 2016 Share Posted February 11, 2016 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. Link to comment Share on other sites More sharing options...
BabcockHall Posted February 12, 2016 Share Posted February 12, 2016 (edited) 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 Link to comment Share on other sites More sharing options...
hypervalent_iodine Posted February 12, 2016 Share Posted February 12, 2016 I was under the impression that this was done neat, not in CDCl3. Agree with doing a carbon NMR though. Link to comment Share on other sites More sharing options...
BabcockHall Posted February 13, 2016 Share Posted February 13, 2016 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. Link to comment Share on other sites More sharing options...
hypervalent_iodine Posted February 13, 2016 Share Posted February 13, 2016 Quite likely. Hard to know for sure until the OP gives more info. 1 Link to comment Share on other sites More sharing options...
NMR-CDCL3 Posted February 24, 2016 Author Share Posted February 24, 2016 Thank you everyone. The Peak at 0 is of grease and not TMS. As of now unable to use the product Link to comment Share on other sites More sharing options...
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