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Distilation of DMT Options
 
Caravel
#1 Posted : 3/30/2012 2:21:12 PM

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Been wondering if it would be possible to distil dmt from its solid form as a purification method and the major problem i was faced with is my condenser is for liquid (alcohol) which posed the problem of getting the crystals out of the tube when finished until yesterday

this is what i came up with and my results

oil bath dish (with no oil)
500ml boiling flask (too large for the oil dish so it sits up on the rim)
hot plate
ice
water
dmt crystals (slightly off white)



1. i took the oil dish and added 500mg of dmt
2. filled the flask with ice and water
3. heated my hot plate at #8 about 400-425F
4. placed the oil dish on the hot plate - after a few seconds i noticed the dmt begin to melt)
5. i quickly placed the boiling flask on the oil dish
6. a few seconds later i watched the (now liquid)dmt begin to vaporize in the oil dish
7. the airspace between the dish and flask quickly began to fill with vapor so i reduced the hotplate to #7 about 375-400F
8. i monitored the vapor for about 10-15 minutes
9. when the vapors were gone the end result was a thick sheet of oily dmt on the bottom of the boiling flask



after the dmt was deposited on the bottom of the boiling flask i emptied the water from it and inverted it on a stand (bottom up) and seeded the oil with a few very small dmt crystals and covered it with a large beaker to protect from dust

the next morning i had thick salt white crystals covering the bottom of the flask
AND (this is the interesting part)
a ring around the outside of the crystals that was discolored (at the location of the glass-glass interface)

this leads me to believe that the dmt-oxy condenses at a diferent temp than dmt

when i scraped the crystals i took great care to keep the two separate but was not able to scrape 100% from the base of the boiling flask

the clean crystals were about 350mg
the discolored was about 60mg
nothing was left in the oil dish
im assuming that my makeshift still was the reason i experienced such a dramatic loss of product (very little left on the base of the flask



~MY CONCLUSION~
-this would be a good process for extracting dmt-oxy and trace amounts of solvents from dmt crystals
- the purity was on par with a column but a column has a better yield although its a lot more work to setup a column and nobody needs that high of purity unless preparing to make DMT-HCL (for injection)
-more thought needs to be put into the still design as to eliminate the vapors from escaping via the glass-glass interface (maybe put some grease at the interface?)
-if one was looking for a very fast "clean-up" this process would eliminate the need for a chemical cleaning completely and would also remove any lye that may have been picked up in the original extraction (so long as you dont mind a 15-20% loss of product



~MY THEORY~
- if one was to dry a stb soup and grind it back into dust i think it would be possible to do a chemical free extraction(no solvent) by heating and condensing the dmt vapors as lye and root bark would not evaporate but as long as the entire mixture reached your ideal operating temp you could essentially pull 100% of the available dmt from the bark in under an hour eliminating the need to mix, separate, wash and precipitating dmt with solvent

- when i did this i did not add enough ice to the boiling flask when the ice melted i may have lost product due to the glass slowly warming up, i think my yield may have been greatly increased if i'd have used more ice (or possible salted ice) to get the glass as cold as possible throughout the process so the dmt would condense on the glass at a faster rate



if i would have used an erlenmeyer flask for the evaporation chamber i could have used my still head with a thermometer and greased fittings to eliminate any vapor barriers and control temp better but then i would be scraping crystals from a condenser with a pipe cleaner so this is why a proper setup was not used - i have not tried a primary extraction using this method and this was my first attempt at purifying this way but i think i will wait till i can devise a better setup before trying again as a 20% loss is staggering but this experiment did show me that it is possible to go from dmt then to vapor then back to dmt extremely fast and without destroying it in the process and i also picked up a couple extra ideas along the way so i feel as though this was a success even though i did lose a couple doses along the way
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benzyme
#2 Posted : 3/30/2012 2:59:12 PM

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I've got a better idea..

use a friedrich condenser instead.
I've done this when decarboxylating tryptophan in mineral oil, tryptamine crystallizes on
the condenser.
"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
 
InMotion
#3 Posted : 3/30/2012 6:13:55 PM
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Usually distillation of high boiling sensitive organic compounds is done either by kugelrohr which is a bit impractical here Pleased or by short path distillation under vacuum. In the case of DMT it is likely beneficial to provide an inert atmosphere.

What you seem to be talking about is sublimation at atmosphere pressure. Expecting a solid is probably a little too optimistic. Maybe if the flask was filled with something very very cold such as dry-ice/acetone and the temperature was carefully controlled. Tryptamines appear to exhibit a cohesive attraction with glass and are kind of notorious with clandestine experimenters to be tricky to crystalize. Not in all cases, but in the case of DMT-n-oxide, it will likely follow this tendency. Which is a likely by-product of high heat and open air atmosphere.

Sublimation at a lower temperature and a lower pressure is more likely where you want to be. I'm not sure what the decomposition point of DMT is, might be worth looking into(if its reported in the literature?).
 
luckytriple6
#4 Posted : 5/21/2012 3:32:49 PM
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Wouldn't steam distillation of the freebase work to purify and remove color?
 
tryptographer
#5 Posted : 5/21/2012 9:31:31 PM

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I once tried to (steam)distill DMT from a rootbark powder and Ca(OH)2 sludge... the distillate was a bit milky and smelled vaguely of DMT, but yield was virtually zero. But this was a very amateurish setup, I even cracked the flask by local overheating. But DMT certainly doesn't boil below 100 C as often stated.
 
 
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