Extracting DMT with ethanol, vinegar and sodium carbonate

[modern]

I actually checked and do have more ethanol 96 so I'll reattempt this using a pure extract and work backwards. I'll weight to see 'efficacy' and test washing the salt using the ethanol 96 which you suggested. I'll likely get around to it this weekend.

 

[modern]

so i didn't get a suspended precipitate of freebase this time but I'm sure it is from being too dilute. I'll be reducing it down by atleast half or reattempt with more DMT.

I treated 300mg dmt oxalate with sodium carbonate solution and filtered thru cotton ball removing sodium carbonate and sodium oxalate. I used 50ml of ethanol 96. Then added 50ml saturated salt brine and it formed a oil later on top which I assume is the DMT freebase. I stirred and it was a bit cloudy. I added to the freezer and the next day mostly have salt precipitate. Decanted and treated that with ethanol 96 to hopefully pull any dmt freebase. Then added all the insoluble salt back to the original solution. Became very cloudy but no clear precipitate/suspention.

In theory the solubility should be 0.5mg/ml so 50mg "lost" but 150mg should precipitate. the 300mg dmt oxalate should be around 200mg freebase. IDK if I posted the reference I found for this.

 

[Sakkadelic]

Recent discussions have been suggesting - as a working hypothesis - that we're seeing deliquescence in humid environments due to the formation of a hygroscopic carbonate. This may be due to recent increases in atmospheric CO₂ concentration. But, as I say, this only a hypothesis at present and would require some kind of experimental confirmation.

There are likely several factors involved in deliquescent goo, not least being DMT's relatively low melting point(s), along with its tendencies towards polymorphism and oligomerisation.

Salt probably just makes the deliquescence worse - but you should be able to pull the DMT back out with fresh 95 - 100% ethanol.

when I tried pulling dmt freebase from sodium carbonate cake using >95% ethanol, and then used the ethanol to make changa, I got a changa that would dry with a fan but then quickly rehydrate when left in a closed jar. I assume that was due to sodium carbonate contamination, even though I tried drying the ethanol with magnesium sulfate, I think I was unable to remove all the water. would using calcium hydroxide instead and hot ethanol be better as calcium hydroxide is less soluble in water?

 

[modern]

Just remembered I forgot to adjust the ph closer to 7.2 rather than 9 it is currently.

https://cdn.caymanchem.com/cdn/seawolf/msds/13959m.pdf

Magnesium sulfate can't dry ethanol... you can use calcium oxide to dry it. I'll probably reattempt doing this at some point trying to use dry ethanol. I attempted this exact idea but salting with fumaric acid rather than evaporating the ethanol. I'll probably have better luck distilling a majority of the alcohol then evaporating the last few ml.

 

[modern]

I actually decided to get some PBS salts so I can more properly try to replicate that source… would fix the salt issue as well and may precipitate better

I’ll update whenever I get around to it

 

[Icon]

If you need to dry ethanol 100% you can do it with molecular sieves. Takes a few cycles; keep measuring with a hydrometer, sifting out the sieves, baking them dry, re-adding. Then distill over fresh sieves for good measure.

 

[modern]

If you need to dry ethanol 100% you can do it with molecular sieves. Takes a few cycles; keep measuring with a hydrometer, sifting out the sieves, baking them dry, re-adding. Then distill over fresh sieves for good measure.

I'm not doing any reactions so true anhydrous ethanol isn't my need. I attempted using a crude 99% ethanol made from the top portion of CaO dried alcohol without distilling. The issue is I still had 'calcium' ions (would still have from freebasing the dmt) so had calcium/sodium fumarate when I added the acid... wouldn't be an issue for me however testing with ehlrich reagent showed it was still in the ethanol 99. I also tried salting out adding salt but didn't work.

I found that salt doesn't work as a buffer which I attempted with salt brine but PBS seems to make a difference.

I did get some DMT to precipitate with the salt in the freezer but I'm fairly sure there is more in solution. (maybe wrong?) The same 'salt' forms where in humidity it form a transparent goo. I added this glass to a silica jar to see how it behaves over a bed of sodium hydroxide would also work but I have dried silica.

Even the white outer edge I think is just dmt since humidity also affects that portion. I'll try adding a flame to this in the future.

 

[modern]

so I’ve been trying to get the Freebase DMT to precipitate from the 50:50 ethanol/PSB but nothing works… I’ve had a precipitate at first but was salt that precipitated. Second I added to fridge and more salts precipitated but zero DMT according to my elrich reagent. The salt brine originally did have a precipitate suspended in solution but didn’t get it this time.

Im gonna take a break on this. It did provide a cloudy solution at first however no promising results from my attempts.

It does seem to precipitate fats/oils which may make this a good clean up step but I don’t think it is work the trouble from my attempts maybe someone else would be interested in trying.

 

[Transform]

so I’ve been trying to get the Freebase DMT to precipitate from the 50:50 ethanol/PSB but nothing works… I’ve had a precipitate at first but was salt that precipitated. Second I added to fridge and more salts precipitated but zero DMT according to my elrich reagent. The salt brine originally did have a precipitate suspended in solution but didn’t get it this time.

Im gonna take a break on this. It did provide a cloudy solution at first however no promising results from my attempts.

It does seem to precipitate fats/oils which may make this a good clean up step but I don’t think it is work the trouble from my attempts maybe someone else would be interested in trying.

That's interesting in a way, since the oiling out from ~30% aqueous ethanol I've observed at c.-22°C now seems to have been a complete fluke. Subsequent experiments have recovered ice crystals rather than two liquid phases - although it should be noted these subsequent experiments used a crude, detanninised MHRB "TnT" tincture rather than relatively pure freebase.

I'd be interested to know if anyone can replicate the oiling out using aqueous ethanol between 20 and 30% ABV, with a freezer that comfortably goes to -22°C or lower.

It tends to be the "wrong" phase that separates out under all other conditions, squeezing tryptamines into an ethanolic phase while seeing either salts or water crystallising out.

I wonder why the oiling out occurred at that concentration, although a rather high DMT concentration relative to everything else probably contributed significantly to it. Getting some more precise figures for this phenomenon would be helpful.

 

[xa]

This is my recently quite noob effort, the extraction from a good mimosa bark, and i follow this thread but i follow my own noob way in doing it, the result you see here it's a Changa with peganum harmala freebase as maoi, then mullein unripe/flowers, hops flowers, malva (??) flower, wild mint. Unfortunately my phone broke badly so i post the results, all others photo of the process depends if they/me can backup from my phone, otherwise I am very happy to replicate the process, i didn't try the result yet.

Edit: forgot to mention that the dmt freebase raw extract smell like honey not plastic, i know that if smoked turn into .... but don't know yet, mixed with herbs the smell now after drying....it's awesome !!!!

 

[Transform]

This is my recently quite noob effort, the extraction from a good mimosa bark, and i follow this thread but i follow my own noob way in doing it, the result you see here it's a Changa with peganum harmala freebase as maoi, then mullein unripe/flowers, hops flowers, malva (??) flower, wild mint. Unfortunately my phone broke badly so i post the results, all others photo of the process depends if they/me can backup from my phone, otherwise I am very happy to replicate the process, i didn't try the result yet.

Edit: forgot to mention that the dmt freebase raw extract smell like honey not plastic, i know that if smoked turn into .... but don't know yet, mixed with herbs the smell now after drying....it's awesome !!!!

So you used the ethanol and sodium carbonate method (just to clarify the obvious)? We look forward to your other pictures once they're recovered. It would make a nice accompaniment to a brief description of your extraction process.

Crude ethanol extracts from mimosa can indeed smell quite pleasant!

Don't forget, we also have a "how does your changa look?" thread.

How does your changa look like ?

Here is mine

forum.dmt-nexus.me

 

[xa]

This is my recently quite noob effort, the extraction from a good mimosa bark, and i follow this thread but i follow my own noob way in doing it, the result you see here it's a Changa with peganum harmala freebase as maoi, then mullein unripe/flowers, hops flowers, malva (??) flower, wild mint. Unfortunately my phone broke badly so i post the results, all others photo of the process depends if they/me can backup from my phone, otherwise I am very happy to replicate the process, i didn't try the result yet.

Edit: forgot to mention that the dmt freebase raw extract smell like honey not plastic, i know that if smoked turn into .... but don't know yet, mixed with herbs the smell now after drying....it's awesome !

So you used the ethanol and sodium carbonate method (just to clarify the obvious)? We look forward to your other pictures once they're recovered. It would make a nice accompaniment to a brief description of your extraction process.

Crude ethanol extracts from mimosa can indeed smell quite pleasant!

Don't forget, we also have a "how does your changa look?" thread.

How does your changa look like ?

Here is mine

forum.dmt-nexus.me

I used an citric acid step first, cold, my bark was not totally shredded ...but wait, Next week i should get the photo, or i have the steps write on paper....wait s little.... Yes i will post on thread you mention....if i try it.

 

[Transform]

Magnesium sulfate can't dry ethanol... you can use calcium oxide to dry it. I'll probably reattempt doing this at some point trying to use dry ethanol. I attempted this exact idea but salting with fumaric acid rather than evaporating the ethanol.

I was reminded of this thread when looking through some photos and finding this:

The condensation is from moisture, distilled out of the toothpicks by the sun's heat. Oven dried wooden toothpicks would absorb a fair amount of water from azeotropic ethanol, and might be cleaner than the trick of using wood shavings or sawdust.

 

[stuartroelke]

Maybe this was already covered, but would it be possible to defat by adding a neutral oil that separates once chilled? Like, make an emulsion and then let it separate out in the fridge? Asking because I only use homegrown chacruna...

Mushroom extract will develop a black oil slick that you can often get rid of with coffee filters (so long as you're just using water, cause fats bind to alcohol and will then pass through filters). If the water has a low or high pH—during an A/B for example—it should prevent contamination while in the fridge for... ever?

Just a thought about defatting with more patience and less solvent—might try this with my summer harvest. If the oil separates out overnight, I could even test this with a salvinorin A extraction.

EDIT:

Nvm, DMT and salvinorin A are lipophilic (apparently salvinorin A and chlorophyl both bind easily to fats). So, adding neutral oil would reduce yield and cause other problems. There's also no benefit to having actives and contaminants bind to fats—basically the same as having a reduced tar.

 

[Transform]

Maybe this was already covered, but would it be possible to defat by adding a neutral oil that separates once chilled? Like, make an emulsion and then let it separate out in the fridge? Asking because I only use homegrown chacruna...

Mushroom extract will develop a black oil slick that you can often get rid of with coffee filters (so long as you're just using water, cause fats bind to alcohol and will then pass through filters). If the water has a low or high pH—during an A/B for example—it should prevent contamination while in the fridge for... ever?

Just a thought about defatting with more patience and less solvent—might try this with my summer harvest. If the oil separates out overnight, I could even test this with a salvinorin A extraction.

EDIT:

Nvm, DMT and salvinorin A are lipophilic (apparently salvinorin A and chlorophyl both bind easily to fats). So, adding neutral oil would reduce yield and cause other problems. There's also no benefit to having actives and contaminants bind to fats—basically the same as having a reduced tar.

Acidification of the ethanol would protonate the DMT and turn it hydrophilic, so you could possibly attempt combining this with some sort of defatting process. Maybe that's where a water-immiscible defatting solvent could come into play.

I don't know if you ever been served ice-cold ouzo, but I reminded of this because it's a good example of a solvent substance - in this case, anethole - separating out as crystals on chilling a hydroethanolic solution. Plant fats might disrupt crystallisation, but there's a good change that phase separation will still occur.

The hard part still comes in separating the two phases, unless you can get the precipitate to aggregate into a large piece.

Salvinorin A is a different ball game, no acid/base changes to exploit there, awart from hydrolysis, which you'll want to avoid at all costs. You might be able to recrystallise from aqueous ethanol using temperature.

Still plenty of experiments to be tried!