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Separating DMT Without Any Solvent Options
 
gibran2
#1 Posted : 4/27/2010 9:26:50 PM

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I recently had an extraction go bad for some unknown reason – it yielded spice that looked just like brown sugar (both color and texture). So I decided to do a re-extraction. Not a re-crystallization, but a re-extraction.

I took the spice, dissolved it in vinegar, diluted with water, then basified with NaOH. The solution becomes very opaque and white as the DMT freebase precipitates out – looks almost like a big glass of milk.

Anyhow, the freebase, being lighter than water, slowly rises and floats in a layer on the surface. I added naptha, heated slightly, and began doing my pulls. After several pulls (successful in cleaning up the spice), I noticed some hard yellowish “chunks” floating in the water layer. It turns out that these chunks were DMT that had liquefied when I heated the naptha, then solidified when the solution cooled.

It made me think – could DMT be separated from solution this way – without using any solvent at all? Heat the solution just hot enough to melt the DMT, allow it to float to the top, cool the solution and remove the solidified DMT?

My thinking is that a mimosa “soup” doesn’t allow the DMT to freely float to the top as it does with a fairly clean solution. Any thoughts?
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mew
#2 Posted : 5/10/2010 7:16:24 AM

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it would be good to know what temperature dmt acetate melts/freezes at

does anyone have any info on this?
 
Infundibulum
#3 Posted : 5/10/2010 7:36:49 AM

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gibran2 wrote:
It made me think – could DMT be separated from solution this way – without using any solvent at all? Heat the solution just hot enough to melt the DMT, allow it to float to the top, cool the solution and remove the solidified DMT?

My thinking is that a mimosa “soup” doesn’t allow the DMT to freely float to the top as it does with a fairly clean solution. Any thoughts?


You're right on that; dmt freebase precipitates out of basic solution (SWIM did and reported it ages ago, look there), but it needs a fairly "clean" solution (e.g. dmt, water and base) to work. It will not work on a dirty basic MHRB solution where al sorts of stuff will not only prevent dmt from separating but will also form clathrate complexes thus further preventing anything frm happening.

BTW, dmt is denser than water, this means that it normally sinks, doesn't float. In your case it floated; this because the ionic composition of your aqueous solution (sodium hydroxide+sodium acetate) apparently made the water more dense than dmt. Sort of an object that sinks in water but floats when the generous amount of salt is dissolved in water.


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q21q21
#4 Posted : 5/10/2010 7:45:42 AM

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SWIM has done that process nearly a dozen times and never gotten yellow chunks. He has seen the floating DMT in the water before but separating them from water was always super low yielding and extremely messy. He never got enough product to measure from it.

Are you sure those yellowish chunks are DMT. SWIM has seen something similar before and they were harsh and nasty (lye?) impurities with a small bit of DMT in them.

Good original thinking but it's doesn't seem too practical if possible
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Infundibulum
#5 Posted : 5/10/2010 8:44:58 AM

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Dagger wrote:
"Infundibulum" wrote:
You're right on that; dmt freebase precipitates out of basic solution (SWIM did and reported it ages ago, look there), but it needs a fairly "clean" solution (e.g. dmt, water and base) to work.

Can you recover most of the dmt this way or will there be much dmt freebase still dissolved in the water?

There will only be traces dissolved in the water. Theoretically it sounds good, but in practise it is not very amazing and one will need at least some acetone or alcohol to fully clean the product from traces of base and salts.... SWIM did this by trying to find an easy way to freebase dmt fumarate but he never really liked this route very much.




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endlessness
#6 Posted : 5/10/2010 9:17:06 AM

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Infundibulum wrote:


You're right on that; dmt freebase precipitates out of basic solution (SWIM did and reported it ages ago, look there), but it needs a fairly "clean" solution (e.g. dmt, water and base) to work.


I remember reading you mentioning this but it didnt work for me for some reason. After base was added to clean solution containing redissolved dmt in acidified water, it did seem to have some precipitation at the moment, but after days and days on the fridge, there were a few tiny specs on the bottom and nothing more, and I knew I had plenty of dmt in that solution. I couldnt find out what went wrong, and just gave up this way of retrieving altogether. Wonder what happened...
 
Infundibulum
#7 Posted : 5/10/2010 10:49:34 AM

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endlessness wrote:
Infundibulum wrote:


You're right on that; dmt freebase precipitates out of basic solution (SWIM did and reported it ages ago, look there), but it needs a fairly "clean" solution (e.g. dmt, water and base) to work.


I remember reading you mentioning this but it didnt work for me for some reason. After base was added to clean solution containing redissolved dmt in acidified water, it did seem to have some precipitation at the moment, but after days and days on the fridge, there were a few tiny specs on the bottom and nothing more, and I knew I had plenty of dmt in that solution. I couldnt find out what went wrong, and just gave up this way of retrieving altogether. Wonder what happened...

SWIM finds this interesting, because there was another guy who tried that with acetic acid and got no results. SWIM did get, but he dissolved dmt fumarate in water, then based with sodium carbonate. Is it possible that if one uses acetic acid this approach may not work? SWIM would love to try when he's got more time in his hands, for the moment he's ultra busy!




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endlessness
#8 Posted : 5/10/2010 10:59:21 AM

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interesting, it was indeed acetic acid for me too... that would be interesting to test, I might try with dmt fumarate in water sometime and see what I come up with. I think it will be interesting comparing the yields of this kind of freebasing technique, with the usual dry sodium carb/fumarate mix and alcohol/acetone pull
 
Infundibulum
#9 Posted : 5/10/2010 12:03:17 PM

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endlessness wrote:
interesting, it was indeed acetic acid for me too... that would be interesting to test, I might try with dmt fumarate in water sometime and see what I come up with. I think it will be interesting comparing the yields of this kind of freebasing technique, with the usual dry sodium carb/fumarate mix and alcohol/acetone pull

Acetic acid is a weird acid in many ways. Just by the structure alone, it is the simplest fatty acid. And salts of fatty acids are basically soaps, which means that sodium acetate is the simplest soap, hence being able to dissolve lipophilic substances (like fats or dmt in this case). Sodium acetate (= the byproduct of neutralisation of dmt acetate with sodium carbonate or lye) is not exactly hydrophobic (lipophilic) but maybe hydrophobic enough to keep dmt in solution. It does have moieties to potentially provide a lipophilic environment, as illustrated in the diagram below. And vinegar has been used as a mild degreaser for centuries.

This may be pushing the argument a bit too much, but we've seen quite some wonders from the acetic acid lately (e.g. being able to break free from the dmt acetate and produce dmt freebase) so I wouldn't be surprised if the above theory is right.


Infundibulum attached the following image(s):
acetic acid complex.bmp (341kb) downloaded 911 time(s).

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Infundibulum
#10 Posted : 5/10/2010 12:07:30 PM

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Dagger wrote:
I am not sure that dmt freebase is completely insoluble in water. I did some experiments today on my gelatin cleaned mimosa. It was a concentrated solution. I added sodium carbonate and loads instantly precipitated. However, it may be that there are other things precipitating than dmt.

When I added more water, the precipitates went back into solution. So it may be that the difference experienced has to do with how much water was used compared to dmt.

Yes, dmt is not completely insoluble in water, but generally insoluble. Given enough water dmt can definitely dissolve. Dagger, was the brew in the trial you describe made with vinegar or just plain water? And you're right, in either case the precipitates could have been anything else...


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Infundibulum
#11 Posted : 5/10/2010 1:20:22 PM

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Dagger wrote:
Infundibulum wrote:
Dagger, was the brew in the trial you describe made with vinegar or just plain water? And you're right, in either case the precipitates could have been anything else...

It was an old brew, but I think I made it with vinegar. Either that or phosphoric acid.

One question. DMT acetate, is it colourless when mixed with water?

Yes, it is colourless - or with a slight yellow tint if there's any n-oxide present.


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hummus
#12 Posted : 5/11/2010 6:17:12 PM

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After leaving a large jar of basified mimosa for a few days in cold (about 16C) temperatures, a large mass of pretty big individual crystals covering the whole surface was seen floating on the top. The crystals were not taken out as the solution had not been filtered so it would be very dirty but it would be interesting to try an extraction with some variant of this. They were big enough to scoop out pretty easily though. IIRC it was 250g mhrb in 1L water with 100g lye and it looked like a good few grams of crystals, hard to tell though. Perhaps filtering the mimosa solution very well and reducing it down then putting it in a fridge and scooping the crystals off the top followed by some sort of cleaning could work, maybe put some small seed crystals in. Would be interesting if anyone's doing an STB to try it and if it doesn't work just carry on with the extraction.
 
gibran2
#13 Posted : 5/13/2010 8:28:31 PM

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q21q21 wrote:
SWIM has done that process nearly a dozen times and never gotten yellow chunks. He has seen the floating DMT in the water before but separating them from water was always super low yielding and extremely messy. He never got enough product to measure from it.

Are you sure those yellowish chunks are DMT. SWIM has seen something similar before and they were harsh and nasty (lye?) impurities with a small bit of DMT in them.

Good original thinking but it's doesn't seem too practical if possible

Sorry for the late response – I haven’t been following this thread.

Yes – the chunks were definitely DMT. I removed them, rinsed them in plain water to remove any NaOH, dried them, and then recrystallized. It yielded nice white crystals.

The re-extraction I did was on a rather large amount of DMT – about 6g, and if I remember correctly, after dissolving in a minimum amount of vinegar, I diluted the solution to about 500mL. After adding the NaOH and waiting, all of the DMT precipitate floated to the top, so I suppose that the DMT was less dense than the solution, even if it’s not less dense than water.

I agree that it doesn’t seem practical, but maybe some clever variation could be? Imagine being able to extract without solvent. That would be great!
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threeleggedlion
#14 Posted : 5/31/2010 11:00:55 AM

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gibran2, I appreciate your investigation of this. I too extracted "brown sugar" and did exactly what you did. I made a mistake however.. I didn't add enough acetic acid to the sugar so it didn't dissolve fully (hope this isn't a problem). I poured in the sodium carbonate water and the whole solution turned milky off white-like a light chocolate milk. When I pulled with naphtha, it also took this milky appearance. Was your naphtha clear or milky? I think I lost the spice Sad
 
gibran2
#15 Posted : 5/31/2010 12:49:34 PM

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threeleggedlion wrote:
gibran2, I appreciate your investigation of this. I too extracted "brown sugar" and did exactly what you did. I made a mistake however.. I didn't add enough acetic acid to the sugar so it didn't dissolve fully (hope this isn't a problem). I poured in the sodium carbonate water and the whole solution turned milky off white-like a light chocolate milk. When I pulled with naphtha, it also took this milky appearance. Was your naphtha clear or milky? I think I lost the spice Sad

If the naphtha is saturated, it will be cloudy. Cloudiness is usually a good sign – it means you’ve got lots of product in there.
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Mindlusion
#16 Posted : 11/12/2013 9:55:25 PM

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Infundibulum wrote:
endlessness wrote:
interesting, it was indeed acetic acid for me too... that would be interesting to test, I might try with dmt fumarate in water sometime and see what I come up with. I think it will be interesting comparing the yields of this kind of freebasing technique, with the usual dry sodium carb/fumarate mix and alcohol/acetone pull

Acetic acid is a weird acid in many ways. Just by the structure alone, it is the simplest fatty acid. And salts of fatty acids are basically soaps, which means that sodium acetate is the simplest soap, hence being able to dissolve lipophilic substances (like fats or dmt in this case). Sodium acetate (= the byproduct of neutralisation of dmt acetate with sodium carbonate or lye) is not exactly hydrophobic (lipophilic) but maybe hydrophobic enough to keep dmt in solution. It does have moieties to potentially provide a lipophilic environment, as illustrated in the diagram below. And vinegar has been used as a mild degreaser for centuries.

This may be pushing the argument a bit too much, but we've seen quite some wonders from the acetic acid lately (e.g. being able to break free from the dmt acetate and produce dmt freebase) so I wouldn't be surprised if the above theory is right.





I extracted some DMT, via A/B (mimosa 250g was filtered) basified with NaOH and extracted with xylene.

I have run out of fumaric acid so this time I used vinegar.

I salted the alkaloids out of the xylene with undiluted vinegar. (5% w/w acetic acid)
And then added saturated sodium carbonate solution to the salted vinegar.

This is the skeptical part.

Well, nothing looked out of the ordinary to me, Upon addition of base, a white precipitate, formed and redissolved with some bubbling.

Once the acid was neutralized, the precipitation persisted. I put this in the fridge, hours later I find crystals had formed. 0.550g of tryptamines from that pull.



Perhaps when I get more fumaric acid, I will do a side by side with each acid and the xylene pull. See if the vinegar produces less yield due to molecular interactions
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Connor137
#17 Posted : 5/27/2020 9:38:33 PM

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gibran2 wrote:

I agree that it doesn’t seem practical, but maybe some clever variation could be? Imagine being able to extract without solvent. That would be great!


After a few days browsing this forum, I have found myself drawn to the nature of this particular discussion, as well as others alike. As patience is critical to precipitating DMT in a basic solution, I believe there is much to be appreciated in this extraction method - perhaps even much yet to be clarified. While some, understandably, care for reliable yields, by commonly utilising various pollutants, an approach such as this seems to encourage a beneficial and wholesome interaction with the system, our virtual organised development environment.
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Jagube
#18 Posted : 5/28/2020 12:40:58 AM

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Has it been confirmed that this doesn't work with DMT acetate?

I see some of the experiments were done on vinegar pulls directly, without evaporating them. If the pulls are evaporated, the amount of acetate ions is reduced to the molar equivalent of the DMT, which will reduce the amount of sodium acetate in solution after basing. Will that still be enough sodium acetate to prevent the crashing out of the freebase DMT?

Also, does the fact that sodium acetate is a soap imply that cooking the raw plant material with e.g. phosphoric acid instead of vinegar would reduce emulsions in the pulls from the basic soup?

Edit: one more question: would using calcium hydroxide instead if a sodium base make a difference? I've heard calcium salts don't cause emulsions as much as sodium salts, so presumably they're less soapy?
 
 
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