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2.) 1H+13C NMR Spectra of yellowish-white DMT


Sample: 


Spice extracted with Naphtha, NO defat, Colour is orange-yellow-whiteish. This shall symbolize what one would actually call *already very good usable, but still definetly not pure spice*.

Therefore I would like to use this to discuss how usable spice at that stage really is. But of course keep in mind: this discussion can only be refered directly to that one sample here which I got. Picture:



Here is the 1H-NMR of that sample. The molecule is included in that picture to show what Signal belongs to what Atom.

But in all future NMRs this will not be shown anymore, just come back here to check it:



Observation:


All the Signals are very nicely visible! But actually it was totally clear that the signals should be visible perfectly, otherwise I would have had a sample of something different than spice =P. So let’s move to the other signals:

There are only a few which don’t belong to DMT: 5 Signals and the Signals that only have an Integral of 0,81. Compared to the Integral of 15 from DMT this is only a very low amount of unfamiliar Peaks. When calculating, the DMT-only-Signals are 94,62 %, which is surprisingly high as it still has a slightly yellowish / orange colour!



Here is the 13C-NMR of that sample. The molecule is included in that picture to show what Signal belongs to what Atom. But in all future NMRs this will not be shown anymore, just come back here to check it:



Observation:


Well not much to say here. The Spectrum looks perfect. ONLY the DMT Signals visible – hooray! Don’t be confused by that thing at ~ 77 ppm. Dichloromethane (DCM) always produces a Signal at 13C-NMR as it also contains a Carbon. For the other samples the 13C-NMR will also not be of that interest ... it’s mostly included to give a complete view of NMR, but for 5.) Photooxidized DMT it will also be very interesting.


Conclusion:


As told in the Observation in the 1H-NMR, the total Signal Integral of DMT is 94,62 %. Therefore it is already a condition of superior purity. Even if we may see really strong colours except white, being it orange or yellow, the DMT may still be more than 90 % + pure. But this is of course still only refering to my sample. But you could probably compare your sample to the foto of mine and judge by view, if the purity level could be around the same based on the colour comparison.


At last it would be interesting what the impurities are. But as they are only visible in trace amounts it is impossible to check them for any multiplicity etc. This is also a reason why I will post a Sample of the IMPURITY ONLY within the future. Then we may see the signals isolated and nicely.

But what can we says based on this: The only foreign signals we observe are in the range of 0,77 – 2,30. Those are aliphatic signals, meaning that they are produced by C-H bonds in saturated molecules. This would fit to molecules like Naphtha (but this should definetly be evaporated to a point where it’s invisible) or plant fats.

Maybe someone will have a further thought on this, but I think we may get some more information when I have that Impurity-only-Sample ready.


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