DMT extraction with limonene and sodium carbonate

[JewishThunder]

Hello everyone, a friend of mine is trying to develop a relatively low odor DMT extraction, as traditional solvents like acetone and naphtha give him quite a serious headache. I figured limonene would be the best option as a solvent for him as it has much less odor than other solvents and any odor it has is relatively pleasant. He would also rather avoid vinegar (for many reasons, one being the same smell issue as the solvents.) Here is his tek at the moment, any thoughts or issues would be welcome.

Materials:
28g Powdered Mimosa Hostilis Root Bark
56ml limonene
~500ml tap water
1 tsp citric acid
50g sodium carbonate
1 1000ml glass jar
1 wide, flat evaporation dish
Pipette and turkey baster for separation of layers
Extra jars or containers for mixing

Procedure:
1. Put powdered MHRB into large jar
2. Mix hot tap water and citric acid in separate container
3. Pour citric acid solution (~PH 4) into large jar with MHRB. Mix well for several minutes
4. Add sodium carbonate to basify solution and mix well
5. Add in limonene, cover jar, and shake vigorously for several minutes. let sit until limonene separates from aqueous layer, and repeat several times
6. Let settle until there are 2 very distinct layers: the clear solvent, and the muddy aqueous layer. Siphon off the solvent layer with pipette and turkey baster, being sure to get all the solvent while not getting any of the aqueous layer. Transfer the solvent into the evap dish
7. Let limonene evaporate completely, leaving behind what I'd assume would look like a slightly brown, waxy substance containing DMT and other related alkaloids, as well as some residue from the limonene that should be safe to smoke.

I'm aware that this might not be the most efficient extraction, but it should be efficient enough to make it worth my friend's time and money. Any feedback would be greatly appreciated.

 

[Brennendes Wasser]

In principle TEK looks good, but just a few thoughts:

1. You say you will place your Bark inside of acidic water for a few minutes - to extract the active compounds.
Why did you come up with a few minutes? I think that would be a little low :/ Better increase the time and also add heat.

My observations are that you extract all actives when doing like this:

At pH 4 or lower, heat up to 80 °C + for 1 h.

Then get rid of all the water and add new pH 4 water and repeat.

And these 2 water fractions are then proceeded to the next step. When only doing 1 cook you may loose some actives, you may still get around 80 % nevertheless. But if not cooking at all / heating, this may decrease yield :/ Also the same goes with the time. If a few minutes only means ~ 10 minutes, then this may be too short. Better do at least 30 minutes. If you dont have a stirring device, then you may increase time, but only stirr every few minutes, to not get your arms fall off at the end ;D

Regarding Limonene: I'm not quite sure how fast it evaporates, this process is not entirely linear to the boiling point, but it may take aaaaages. It boils naturally at 175 °C I believe and therefore this should not be the way to do it. But you may freeze precipitate it like with Naphtha, I guess other "eco TEKs" also use it and they may describe how to proceed from that step. If they tell to evaporate, that would wonder me, so maybe check out what they tell :thumb_up:

Limonene is flamable, so you should definetly make sure that no Limonene is left in your goo ... and this will be hard, as it will only evaporate down to like 0,01 % and the rest will stick in the oil forever. By doing freeze precipitation it may be possible to get much less. Any overly big residue of Limonene may start your herbs catching fire when creating Changa from it for example.

Also keep in mind that even though Limonene is "food-safe" it is not for aqueous systems, so throwing any residual Limonene to down the drain would decrease Karma Overall I think Naphtha would be easier, but if you read other Limonene TEKs and how they separate the DMT then you may still give it some good tries!

 

[Hyper Turtle]

You can't evaporate d-limonene from dmt. And sadly, it also doesn't work for freeze precipitation. You'll need to backsalt. It's a little bit of extra work.

You need to perform several pulls, not just one. Divide your d-limonene into 3 or 4 portions for separate pulls.

But first, you have to decide if you want it to be more A/B or more STB. I think I'd go for the more A/B approach (because emulsions virtually impossible), but both should work in theory.

More A/B:
********
You cook 2 or 3 times (each 1h+) with acidic water.
You collect the filtered teas from your boils. If you reduce it, filter again, as more gunk tends to crash out in the process. Best is to let it cool and settle over night and filter again to get clear tea.
You base your filtered tea, add the limonene, agitate it, let it separate, and pull. It is better to kind of roll/swirl than to shake. If your tea is really clear, it doesn't matter much, but otherwise shaking will lead to an emulsion layer that may or may not separate with time.
You don't need to (but can) wait between pulls.

More STB:
********
... would be to not separate the liquid from the bark (therefore, just 1 boil/soak but for longer). You can choose to use minimal acidic water, go for dough consistency when mixing in the base, and pull by stirring d-limonene into the dough then decanting away, or to use more water, add base until it's black, and pull from that soup. If you choose that, DO NOT SHAKE. Do the roll.
It is beneficial to wait a bit between pulls.

Backsalting from d-limonene:
***********************
Backsaltng means to use an acid to convert the dmt into a salt again, which either crashes out (FASI/FASA) or moves into an aqueous phase (vinegar, FASW, citric acid water, ...) that can then be evaporated to retrieve the salt form, or based again and pulled from with a small amount of petrochemicals.
The salt forms can be converted to freebase if needed.

 

[JewishThunder]

Thanks for the replies! I was not aware that evaporation would not be possible for limonene. The other option I had in mind was to pull the alkaloids from the limonene with vinegar and evap. My plan with the acidic solution was to leave it sitting for around 30 minutes to an hour while shaking/stirring fairly frequently then basify and pull.

 

[Brennendes Wasser]

30 Minutes may be a little bit short if you do not heat it at all. Maybe heat it very high (80 °C maybe) for 30 minutes or enlarge the time to maybe 3 h if you keep it at room temperature. Temperature really makes a difference when dissolving stuff from solid mass :/ Therefore increasing time wont hurt, especially as you dont have to do much meanwhile. Maybe just d oa little stirring from time to time. Maybe you can try a 30 min run first and then do a 3 h and see if it got you further.

Now getting the Alkaloids out of Limonene with Vinegar is a good step to get rid of the Limonene.
But then the next problem is: The alkaloids are then in their salt form again, that will not vaporize like Changa would. They are in their salzed Form "Alk + H+" and not "Alk". Therefore you would have to get rid of that "H+" again. The problem is: If you throw a base inside of the soup, then after evaporating you will be left with Alkaloids, but also with the Base+Vinegar. Even though they are not chemically bound to your alkaloids, they will be mixed together like apples and oranges in a basket and you would still throw both at your changa blend.
So you would have to get rid of those unwanted compounds again.
The only "easy" method I could think of would be to basify the vinegar and then check if after some hours or even 1 night the Alkaloids will settle to the bottom. Then you could decant everything and the Alkaloids will stay on the ground, ready to be converted to Changa with Alcohol.
I may try if that works, that was something I was wondering since a long time: Normally DMT is so unpolar it should not be held in water at pH 11+ for a long time, since even the more-water-soluble chemical predecessor Tryptamine will also separate from the water when treated the same way.
The last convern would be that you will have more steps than with a regular TEK and therefore it will naturally occur that the yield may be lower or even quite low. You should ensure that the first step when cooking the plant material would definetly be as efficient as possible (stirring, heat, long time) and also when pulling with Limonene from that soup and also when pulling with vinegar from Limonene. Always mix very intense and I would also apply high heat when pulling from 1 solvent into another (just below vaporization point of the lesser boiling solvent).

 

[JewishThunder]

Alright, how would this work: after alks are in limonene, salt out with vinegar, evap, and use this method to convert to freebase. Does that method only work for fumarate or for all salts? I'm aware it's an extra step but I'd like to use limonene because of the reasons stated before, as well as the fact that it collects the most alkaloids.

 

[doubledog]

You can easily separate DMT from vinegar water after salting out limonene by adding some base. Freebase precipitates as white solids, keep it few hours in the fridge.
Filter it afterwards, it will not settle at the bottom.
Wash filter with solids with water, dissolve solids in ethanol or isopropanol, evaporate, and wash residue with water. Let dry.
It will be light brown waxy material, do not expect white crystals.

 

[JewishThunder]

Thanks for all the help everyone. I was not aware how difficult limonene is to extract with. I'll probably end up using limo anyway just to avoid the dangerous and stinky other solvents but if it doesn't work out ill give up on my quest for dmt without stinking up the whole house
Expect a post relatively soon on how that goes, might even include pictures. Safe travels my friends!

 

[doubledog]

You will probably find that limo odour is not that pleasant as it seems to be.
Anyhow, it is possible to minimize smell by keeping the solvent enclosed and by using very small amount of it.

 

[Brennendes Wasser]

Wash filter with solids with water, dissolve solids in ethanol or isopropanol, evaporate, and wash residue with water.

Isnt this a kind of double step where you dissolve the alkaloids in ethanol/iso again just to evaporate it then again?

I mean you would get your alkaloids from Limonene by extracting with vinegar and then let them crash out in pH 10+. But then these are the Alkaloids, no need to dissolve them back in a solvent, which you evaporate right afterwards? ;0 Would only make sense if you then use a solvent that is more selective to DMT, to do this as a kind of purification step. But the usage of Naphtha/Hexane was not considered so I guess that step could be avoided.

Also another possibility:

Why hesitate to handle the smelly solvents at home, couldnt you maybe just hang out around somewhere and do you extraction work there? You would basically need 2 containers and maybe 1 big soup trowel to separate layers.

I would do it like this:

> basify your soup at home to pH > 11

> fill this soup in a PET plastic bottle big enough for extraction

> add your desired amount of Naphtha and close the container. Now either shake like hell (faster extraction, but causes emulsions and you have to wait afterwards for them to vanish) or gently swirl it bottom to top and over. By not applying heat you have to do many extractions, therefore I would suggest to apply heat. You could place the bottle for 10 min in hot water until the inside will also be quite hot.
Doing this would make you extract with Naphtha at high temperatures without emitting fumes. You should not bring it to a boil, the plastic bottle will not explode, but still dont let too much pressure build up.

> Now fill the soup + Naphtha in a big pot with a suitable lid and close everything to avoid fumes and more important that the Naphtha will stay in place. If you shook strongly then wait for emulsions to disappear. Then go somewhere out in a hidden spot and open the pot and use a big soup trowel to separate the Naphtha from your soup and place the Naphtha in a different PET bottle. This Naphtha needs to be placed at -20 °C to drop reasonably pure DMT crystals, otherwise evaporate it to get more impure yellow stuff, in worst case not even crystaline, but okay to use.
You should still do 1 or 2 more extractions like this if you want a reasonable yield. Just fill the acidic soup (after separating it from the Naphtha) back in the former PET bottle which is now empty again and put in new Naphtha, then heat it up again (so do this step at home again) and then proceed like the last time.

This way you may work odorless and still use the easier methods. May sound complicated, but in summary this will actually safe you work I guess. And you could just place the PET Bottles and the pot in a bag which you take with you.

 

[Hyper Turtle]

Yeah, the limo smell is pretty intense

To be honest, naphtha didn't produce much smell at all, against my expectations. You should probably give it a try at some point, freeze precipitation is really neat.

But if you already have limonene, by all means just do it! Limo is still great. The extra work isn't as bad as it sounds.

From the end of my previous answer, again the link to fumarate -> freebase conversion. It has three methods, all of which should also work for acetate, i think. I haven't tried the first two, water based methods with acetate. Before i started using fumaric acid, i used vinegar, and i did my conversions with the sodcarb paste method. It always worked, but sometimes it produced viscous freebase that wouldn't fully harden for weeks. I suspect it was because i didn't let the paste dry thoroughly enough.

You can also smoke dmt acetate on herbs. It is NOT ADVISED, but possible. Don't do it, especially if you're not normally a smoker. But IF you do it, make sure to remove residual acetic acid from the goo, eg. by heating it for a while. This will turn the smoke from very harsh to almost not harsh. Heat it just enough to barely see smoke/vapor, verify that it is acetic acid by cautiously smelling. When the acetic smell disappears and the dmt smell gets stronger, you're done. Be careful with the heat, you don't wanna burn or evaporate your goo.

I mean you would get your alkaloids from Limonene by extracting with vinegar and then let them crash out in pH 10+. But then these are the Alkaloids, no need to dissolve them back in a solvent, which you evaporate right afterwards? ;0 Would only make sense if you then use a solvent that is more selective to DMT, to do this as a kind of purification step. But the usage of Naphtha/Hexane was not considered so I guess that step could be avoided.

To me, it sounds like a good way to separate the dmt freebase from the filter, as the precipitate will likely not be large hard crystals, but soft stuff sticking to the filter paper. It will also make extra sure to get rid of any traces of the base, plus yield larger crystals if evaping slowly.

 

[doubledog]

Wash filter with solids with water, dissolve solids in ethanol or isopropanol, evaporate, and wash residue with water.

Isnt this a kind of double step where you dissolve the alkaloids in ethanol/iso again just to evaporate it then again?

I mean you would get your alkaloids from Limonene by extracting with vinegar and then let them crash out in pH 10+. But then these are the Alkaloids, no need to dissolve them back in a solvent, which you evaporate right afterwards? ;0 Would only make sense if you then use a solvent that is more selective to DMT, to do this as a kind of purification step. But the usage of Naphtha/Hexane was not considered so I guess that step could be avoided.

You are right. It can be avoided.
alcohol step is just for removing freebase from filter, it has just this practical purpose. so it is enough just to dry the filter with alks directly.
I use it because in my simple setup it is more convenient.