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has anyone done a melting point test? Options
 
benzyme
#1 Posted : 8/1/2009 7:18:16 PM

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on their spice?

I know many do recrystallizations and freeze precip, but I postulate a/b and stb extractions also pull NMT, an intermediate that may also be present in the end product, even in white crystals
subliming yields absolutely pure dmt
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WSaged
#2 Posted : 8/1/2009 7:48:30 PM

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Could you explain what "subliming" is, for the rest of us?Wink


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benzyme
#3 Posted : 8/1/2009 7:56:57 PM

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heating a compound to its specific boiling point, and having it collect on a coldfinger (a tube with cold water, ice, etc.)
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
69ron
#4 Posted : 8/2/2009 12:41:50 AM

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Do you know the details on how to sublime DMT? What level of vacuum is needed?
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benzyme
#5 Posted : 8/2/2009 1:09:53 AM

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see, that is something that needs further investigation.
and the b.p. range listed for dmt is too wide, imo (60-80C).

ya boy tried subliming 50mg pink spice at 49C and 21.5"Hg (probably too much vac), and ended up with a clear residue that smelled strongly of fish/plastic.
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tryptographer
#6 Posted : 8/2/2009 1:42:54 AM

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Nice work Benzyme, I remember this from another thread Smile

Interesting notion of NMT (monomethyltryptamine). Could it work like a catalyst, not really active by itself but potentiating or altering a pure DMT experience?

I'm still intrigued by the boiling point...
It's even more important than the melting point because vaporization is often the chosen route of administration. I only it would vaporize more easily!
I saw with my own eyes it doesn't even boil at 100 C - I think it boils at a higher temperature than most people think.

Shulgin himself says the 'official' value is incorrect. Quote from Tihkal:
"The Merck Index gives the very early, very low values of 46 °C and 44.6-46.8 °C and claimes that the bp is 60-80 °C with atmospheric pressure being implied. It is clearly in error on both matters."

so.. has anyone here measured the boiling point?
 
benzyme
#7 Posted : 8/2/2009 2:02:33 AM

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thanks
i don't know if NMT is active, shulgin mentioned it wasn't in TIHKAL. but if it's vaporized and absorbed in the lung tissue, it could in theory get methylated by INMT to dmt.
it's also an intermediate in human metabolism, first-pass metabolism of tryptamine via INMT

69ron and I did discuss sublimation in a thread titled 'sublimators'; it would be cool to do a sublimation at atmospheric pressure, as he suggested.
*edit* a glance back to that thread told me that it doesn't work.

NMT has a considerably higher melting point, so it stands to reason the boiling point will also be higher.
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69ron
#8 Posted : 8/2/2009 2:55:36 AM

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Sublimation is a great isolation tool WHEN IT WORKS. It's hard to get it right though. Often just the right amount of vacuum is needed or it doesn't work.

It’s interesting that Shulgin states that the DMT boiling point in the Merck Index is wrong, but doesn’t then give us the correct boiling point. Man!
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benzyme
#9 Posted : 8/2/2009 3:53:31 AM

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yep
and dmt's b.p range lies well below the corrected b.p range in a nomograph.


gotta calculate it

as for ya boy, he's gotta tinker with regulator valves, and maintain constant temp.
would be nice to have enough spice to work with.
"Nothing is true, everything is permitted." ~ hassan i sabbah
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bufoman
#10 Posted : 8/2/2009 5:15:51 PM

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If one had enough spice they could theoretically separate the NMT from the DMT by acetylating the NMT and performing so extractions. Shulgin uses this method in his synthesis of a variety of alkylated tryptamines using acetic anhydride. There is then a subsequent extraction process that will remove the NMT acetylated derivative and leave the resulting freebase DMT in a organic solvent. In addition the NMT could be technically regenerated.

Trouts Notes claims that freebase NMT (MMT) is soluble in water. Even in a Ethylacetate:Water partition experiment. And water can be used to crystalize it upon slow evaporation (Filho and Gilbert 1975). If this is the case it is unlikely to be extracted in significant amounts. Although I find this strange as neither tryptamine nor DMT is water soluble. Nor would one expect NMT to be water soluble however chemistry does many unpredictable things.

Shulgin claimed to vacuum distilled NMT at 135-145 at .1m/Hg yielding a white oil which formed white crystals which darkened on air exposure. So it definitely looks like DMT and has similar properties. It maybe that DMT would distill off earlier and thus they could be separated by sublimation. A chromatography column should also be able to separate them. Recrystalzied DMT typically gives a single peak on TLC. Although I have seen it before the second recrystalization have a minor spot with a lower Rf value. Based on MS and HPLC these are minor-trace components however.

Twice hexane Re-crystalized DMT is likely to be pretty pure. NMT may be a component of jungle spice. Although it maybe picked up in the hexanes it would not be as hydrophobic as DMT. Especially since it is water soluble as the freebase this seems unlikely.

There are also color tests to determine the presence of primary, secondary, and tertiary amines that one could do.
 
benzyme
#11 Posted : 8/2/2009 5:36:00 PM

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what initially confused swim is the lack of crystal resolution from purified dmt. it was crystal clear, but the consistency was that of vaseline. it would seem to him, given the low melting point, that pure dmt free base does not stay crystalline at RT.
"Nothing is true, everything is permitted." ~ hassan i sabbah
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bufoman
#12 Posted : 8/2/2009 5:40:02 PM

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SWIM agrees most DMT she has seen that if pure will melt if placed at anything slightly greater than room temp.
 
69ron
#13 Posted : 8/2/2009 8:02:18 PM

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SWIM has often seen DMT with the consistency of Vaseline after it vaporizes and collects again.

When SWIM uses his test tube vaporizer setup, he allows the DMT to form a giant cloud of vapor before inhaling from the vapor whip. Inevitably, some of the DMT sticks to the walls of the test tube, especially if SWIM waits too long to inhale the vapor. SWIM is using pure DMT crystals for this. But what’s seen on the inside of the vapor tube is NOT crystalline. It looks just like Vaseline. It’s sticky and oily. You can recollect it and re-freeze precipitate it to get crystals again.

My point being just because it looks oily doesn’t mean it’s impure or something other than DMT. Under certain conditions it’s very difficult for DMT to crystallize.
You may remember me as 69Ron. I was suspended years ago for selling bunk products under false pretenses. I try to sneak back from time to time under different names, but unfortunately, the moderators of the DMT-Nexus are infinitely smarter than I am.

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Pancho
#14 Posted : 8/23/2009 2:23:16 PM

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Another thing but maybe related...

I had my recently freezed naphtha bottle with the snowy spice on the bottom, It was a little yelow so I warmed it with a boiled water bath and inmediatly the precipitated spice melted into a traslucent yelow liquid. So, I had the bottle with the naphtha and the liquid on the bottom, there were two layers.
I dont understand why did Not It disolve again Wut?

Then I shaked It and the liquid disolved in the naphtha solution turnning it a little yelow.
I never understood if that liquid was spice, fats and oils, or spice in fats and oils.

Story continues: After the shake I had the hot yelow naphtha solution and a drop of brown goo on the bottom. I siphoned it with a syringe, It was difficult because this crap was very stickyShocked
Then I freezed again and my snow was cleaner than before, but still with a slight yelow tone (as slight as to evaporate the powder, I didnt want to screw up the spice with more procedures).
Some explanation? What (the hell) did I take off (the brown crap)?
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