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Pulling from d-limonene the pleasant way

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Nagual

Nagual

Rising Star
While 5% distilled white vinegar is a fairly popular acidic solution for getting DMT out of D-limonene, I think we can all agree that cleaning up the vinegar/DMT solution is slightly irritating, and left-over vinegar makes your DMT taste nasty. Remembering a lab partner of mine that used to clean glassware with diet coke, I thought - why not use a carbonic acid solution? It turns out that carbonated soda water is ~pH 4.5, which is low enough to get the DMT to salt out. Soda water also evaporates fairly cleanly at lower temperatures, unlike acetate. I put my soda/DMT solution in a beaker and let it sit in a warm water bath, and the result was a light yellowish goo that dried to a nice amber resin, with no acetate smell :)
 
the melting point of carbonic acid is 410 degrees, which like acetic acid can be vaporized with a traditional lighter
 
mew said:
the melting point of carbonic acid is 410 degrees, which like acetic acid can be vaporized with a traditional lighter
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got a reference for that?

carbonic acid only exists in solution, how can one determine its melting point?

also, melting point is not the same as boiling (or vaporisation!) point, so what short of point you're trying to make here is not clear.

And have you personally tried to vaporise dmt carbonate as you'd vaporise and freebase dmt acetate or you're just inferring?
 
good points, and i have no credible source

however the dmt carbonate may not need a solution to exist within as is the case with carbonic acid, if thats the case it is still possible the bp of the salt is low enough to vaporize with a traditional lighter

im not sure how carbonate is as a salt other than some semi failed extractions with carbonated water salting from mescaline saturated limo. the product was nearly impotent from my amateur extraction, i did not know of a way to separate carbonates from excess carbonic acid either.
 
mew said:
however the dmt carbonate may not need a solution to exist within as is the case with carbonic acid
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isnt this the case when using hcl solution, if left to evaporate the hcl vaporizes leaving little to no excess hcl acid but leaving the mesc hcl
 
mew said:
mew said:
however the dmt carbonate may not need a solution to exist within as is the case with carbonic acid
Click to expand...

isnt this the case when using hcl solution, if left to evaporate the hcl vaporizes leaving little to no excess hcl acid but leaving the mesc hcl
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Yup - there is nothing wrong with dmt carbonate existing outside a solution; and your analogy with HCl is correct. Similarly, we are all familiar with sodium carbonate and sodium bicarbonate! It's just the carbonic acid that does not exist out of solution.
 
Infundibulum said:
mew said:
mew said:
however the dmt carbonate may not need a solution to exist within as is the case with carbonic acid
Click to expand...

isnt this the case when using hcl solution, if left to evaporate the hcl vaporizes leaving little to no excess hcl acid but leaving the mesc hcl
Click to expand...
Yup - there is nothing wrong with dmt carbonate existing outside a solution; and your analogy with HCl is correct. Similarly, we are all familiar with sodium carbonate and sodium bicarbonate! It's just the carbonic acid that does not exist out of solution.
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This is a valid observation. My empirical observation is of a fairly clear product with an oily consistency after heating. My hypothesis for this is as follows (please bear with me, my chemistry is a bit rusty):

Carbonic acid readily decomposes into water and carbon dioxide, and the equilibrium for this reaction is very close to complete reaction. Carbonate gains stability from the planar resonance structure it forms, but in order to form this species, you need a good cation. Sodium is an excellent cation, owing in part to its great reducing potential; additionally, sodium fits nicely in the donut shaped clouds of electron density above and below the planar surface of the carbonate ion, formed by resonance of the p orbitals.

I believe that the nitrogen of the amine is the proton acceptor; a strong acid is generally required to protonate indoles. That means that your DMT molecule is complexed to the carbonic acid anion by a long flexible chain, with bulky, electrically 'netural' methyl groups preventing the protonated nitrogen from really nestling in close to the regions of high electron density. Given the configuration of the complex, the DMT molecule is also prone to dissociate as a result of brownian motion in solution, in a temperature dependent fashion. What I believe this means for the end result is that the formation of stable carbonite salts is much less favorable than normal, and thus the Boltzmann distribution for equilibrium of species will be shifted majorly towards carbon dioxide and water. As a result, when the water evaporates, only minuscule (equilibrium) amounts of carbonate salts remain, insufficient to cause visual disturbances in the vitreous DMT.

I believe the difference between this case and the case of mescaline chloride is the qualities of chlorine as an anion. Chlorine is highly electro-negative and small, letting it nestle in very close to protons; it would be no problem for a chlorine anion to slide between two methyls. While oxygen is more electro-negative than chlorine, with carbonic acid you are dealing with dipoles and partial charges. Additionally, carbonic acid is bulky, limiting its ability to form complexes.

Hopefully my memory of phem, molecular geometries and crystallization is ok (it has been a LONG time since I studied that stuff). I trust any errors will be kindly pointed out :)
 
Nagual said:
I believe that the nitrogen of the amine is the proton acceptor; a strong acid is generally required to protonate indoles. That means that your DMT molecule is complexed to the carbonic acid anion by a long flexible chain, with bulky, electrically 'netural' methyl groups preventing the protonated nitrogen from really nestling in close to the regions of high electron density. Given the configuration of the complex, the DMT molecule is also prone to dissociate as a result of brownian motion in solution, in a temperature dependent fashion. What I believe this means for the end result is that the formation of stable carbonite salts is much less favorable than normal, and thus the Boltzmann distribution for equilibrium of species will be shifted majorly towards carbon dioxide and water. As a result, when the water evaporates, only minuscule (equilibrium) amounts of carbonate salts remain, insufficient to cause visual disturbances in the vitreous DMT.
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So you say that if you evaporate down a solution of dmt carbonate you'll end up with the freebase?

That's easy to test if it holds true.
 
Infundibulum said:
Nagual said:
I believe that the nitrogen of the amine is the proton acceptor; a strong acid is generally required to protonate indoles. That means that your DMT molecule is complexed to the carbonic acid anion by a long flexible chain, with bulky, electrically 'netural' methyl groups preventing the protonated nitrogen from really nestling in close to the regions of high electron density. Given the configuration of the complex, the DMT molecule is also prone to dissociate as a result of brownian motion in solution, in a temperature dependent fashion. What I believe this means for the end result is that the formation of stable carbonite salts is much less favorable than normal, and thus the Boltzmann distribution for equilibrium of species will be shifted majorly towards carbon dioxide and water. As a result, when the water evaporates, only minuscule (equilibrium) amounts of carbonate salts remain, insufficient to cause visual disturbances in the vitreous DMT.
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So you say that if you evaporate down a solution of dmt carbonate you'll end up with the freebase?

That's easy to test if it holds true.
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My experience has been that the purity of the product is good. Just make sure you use soda water without added sodium/potassium. That would of course leave you with carbonate salts, which are stable to higher temperatures than DMT.
 
so what im getting out of all your scientific mumbo jumbo wizardry is....

salting with carbonic acid solution and evaporating with less heat than the freebase bp of dmt would succesfully yield freebase dmt with miniscule amounts of dmt carbonate?

this sounds like a great way to acquire fb dmt without converting your salts to fb and pulling and evapping. thanks for the upcoming experiment! is there going to be sodium in the end product, if so the end product could be pulled with acetone or ipa to (dry) to separate from sodium
 
mew said:
so what im getting out of all your scientific mumbo jumbo wizardry is....

salting with carbonic acid solution and evaporating with less heat than the freebase bp of dmt would succesfully yield freebase dmt with miniscule amounts of dmt carbonate?

this sounds like a great way to acquire fb dmt without converting your salts to fb and pulling and evapping. thanks for the upcoming experiment! is there going to be sodium in the end product, if so the end product could be pulled with acetone or ipa to (dry) to separate from sodium
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mumbo jumbo? :(

That is my observation, yes. There will be some sodium in the end product just because it is very hard to find soda water that is electrolyte free. The quantity should be very small though. Just put your beaker in a water bath with drip feed and heat it gently overnight, should be sufficient to get it all the way down. My final solution is a clear dark orange that dries to a waxy solid.

I would get a couple of different kinds of soda water and test the pH on each of them as well, I've seen the gamut from pH 3.5 to 5.5. Pulling from the limonene will go faster if you can get the low pH solution.
 
sounds like a great innovation!

instead of drip feeding into a hot bathing beaker all evening, i think a food dehydrator not exceeding 155 f will be fine , a nice flat pie pan fits in perfectly and can evap 100 ml per hour safely


p.s. the mumbo jumbo was supposed to be a compliment, i had a hard time following what was said and wouldnt have been able to explain it as you had :)
 
mew said:
sounds like a great innovation!

instead of drip feeding into a hot bathing beaker all evening, i think a food dehydrator not exceeding 155 f will be fine , a nice flat pie pan fits in perfectly and can evap 100 ml per hour safely


p.s. the mumbo jumbo was supposed to be a compliment, i had a hard time following what was said and wouldnt have been able to explain it as you had :)
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The food dehydrator sounds like a great idea. I have been planning on getting one for mycology experiments anyhow! Thanks :)

I have found that the carbonated water you buy in the stores is both overpriced and not as acidic as I would like. This results in less DMT per pull compared to acetic acid. The solution? How To Make Your Own Home Drink Carbonation System. With this bad boy very heavy pulls should be achieveable; just pour the limonene in a screw cap airtight wine or liquor bottle with fresh soda water and swirl gently every couple of minutes for an hour or so (or just let it sit overnight).

I've also figured out a nice way to combat solvent loss and get a lot of DMT into the limonene with each pull. If you dry out your basified mimosa paste to a crumbly powder-ish consistency, saturate it with limonene, let it sit overnight, then add water and stir until all the limonene floats to the surface, you get huge pulls and don't lose any solvent. When you want to do another pull, just gently heat the mimosa paste until it is crumbly again and repeat.

I think I feel a new TEK post coming soon ;)
 
I'm very interested in this if it means that carbonated water could replace FASW when one intends to do water precipation (as in BLAB step 6).

In the UK, you can buy used SodaStream drinks makers for very cheap on eBay; using one with very cold distilled water would carbonate the water very well.
 
Nagual said:
I've also figured out a nice way to combat solvent loss and get a lot of DMT into the limonene with each pull. If you dry out your basified mimosa paste to a crumbly powder-ish consistency, saturate it with limonene, let it sit overnight, then add water and stir until all the limonene floats to the surface, you get huge pulls and don't lose any solvent. When you want to do another pull, just gently heat the mimosa paste until it is crumbly again and repeat.
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I was wondering if there was a good way to get solvent back like this. This could surely be done with cactus powder as well. That is some great information, many thanks! :d
 
I believe 69ron...or perhaps amor fati (but I think it was ron) claimed to have successfully done this with cactus in a post preceding the creation of his cactus tek. I think it's in the FASA thread, but I'm not sure. The difference is that he didn't add water, iirc...he just fully dried the basified cactus and then pulled with limonene and repeated. Perhaps its worth digging around for that post :)
 
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