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Pictorial Guide to Caapi Vine Alkaloid Extraction Options
 
Nibs
#461 Posted : 5/15/2020 6:47:43 AM

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I did this tek with a few tweaks and got some very strange results. I did a combination of Endless's Harmala Extraction Tek and this one. I used 112 gram of Caapi vine. The tweaks I made were as follows:
- powdered the vine
- filtered the boiled reduction with a cotton stuffed funnel to remove excess plant material
- used sodium carbonate (Na₂CO₃) as a base because its less toxic
- dissolved alkaloids with hot 1:3 vinegar/water
- rather than decanting, I used a coffee filter to speed up the separation of alkaloids from base solution, and then insolubles from the acid solution.
-i let base solutions settle in fridge overnight at each step, so at no point did it appear that there wasn't a sufficient amount of freebase forming.

So throughout the process the alkaloids were crashing nicely. The biggest issue I had with this though was the carbon dioxide foam reaction that would form when basifying the acid. I would have to scoop out the foam until the solution was finally neutral and stopped reacting, and then i would add Na₂CO₃ until it was fully saturated and the color of the solution stopped changing (as it is done the Endless's Tek). The first time I did this step, I didn't save the foam and dumped it. The second time though I decided to keep it and shook it in a jar with water, added more Na₂CO₃ then let it settle in the fridge. To my surprise it did take a lot of alkaloids with it.

I finished the tek with the foam alkaloids separate from the main batch and the results were very different. The foam produced a lighter brown freebase like they did in this teks pictures, and confirmed its potency by vaporizing it. Unfortunately this only produced about 150mg of freebase. The main batch produced 2 grams of a darker brown and heavier freebase, even after washing until the water it was suspended in was clear. When I vaporized it there were very little effects, and it left behind a hard creosote like material and not a light ash like it shoukd have.

I don't know what the final product is that was produced from the main batch, but it was inferior compared to what was recovered from the foam reaction. I do not recommend using sodium carbonate for this tek, and I will be using lye next time hopefully with more consistent results.
Nibs attached the following image(s):
20200514_231110.jpg (1,934kb) downloaded 140 time(s).
 

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Ruffles
#462 Posted : 9/19/2021 5:47:27 PM
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I would like to thank (a lot) Gibran for the time to develop this simple and effective tek.

I would also like to make a contribution in the tek.

After the acidification step (mid tek) and decanting the yellow-brown supernatant, basification should be done drop wise with slow mixing of the supernatant. When pH is low (up to 3-6), addition of base dropwise will cloud it but it will dissipate, this should be repeated with calm and patience as the pH of the whole solution must equilibrate before adding more. When you reach pH 7-8 the first magic happens as the clouds do not dissipate, the whole solution will cloud up and very quickly brown-darkbrown precipitates will form, pH checking will show pH between 6-8, don`t go higher than this right now, it`s very easy to overshoot without electronic pH meters. Stop shaking and let it fall to the bottom.

Near this threshold pKa for harmine, a lot of it will drop out, some harmaline certainly drops out as well but way less. After solution clarifies the supernatant will continue to be light yellowish, meaning harmine-harmaline still dissolved. Also, at this pH brown harmine may precipitate cleanly giving you yellow-brown needles, brown precipitates after washing turn yellowish. A good sign, beautiful sight, specially because the crystals size will help it fall to the bottom quickly.

The yellow solution can now be basified further to drop harmaline and the rest of harmine out. Just keep slow mixing and dropwise add base, don`t overshoot! This makes the precipitates drop out too fast and become a powder which do not fall to the bottom. If this happens, reacidify dropwise then rebasify. Harmaline will drop out as white precipitates, if your pH is not very high (pH 9-10), white needles will fall out (they have a smaller length than the previous). Stop shaking, wait for the full precipitation to occur. Decant supernatant (that will remain somewhat yellowish but not fluorescent, you can try recovering whatever is in it by adding more base and putting it in the fridge, not much will come out).

Follow up with final cleanup until pH is 7-8 and you`re good to go. I suggest washing the precipitates with water pH 7-8 (just prepare a bunch using small amount of base), not plain tap water or distilled, as it it too acidic and you may dissolve crystals.

My contribution here is simple: do gradual pH increases on the basification steps and you get cleaner and bigger crystals that will speed up decanting and you can separate harmine and harmaline in a very visual way, stupid easy to execute. It takes more patience but turns out it speeds up further steps. Do not overbasify!

If you add too much base at once, pH climbs too fast and alkaloids drop out instantly, resulting in a cloud that takes way too long to decant. Near the pKa, the alkaloids drop out slowly, sequentially adding themselves to precipitates making them larger.

Image shows unclean `harmine` to the left and `harmaline (+ harmine surely)` to the right. Further cleanup of harmine leads to yellow needles, takes little washes to get to it, since you didn`t add too much base at once. You can also wash once and readd acid (pH 4) to redissolve it, decant-filter brown gunk, then rebase it slowly to get the yellow crystals.
Ruffles attached the following image(s):
handh.jpg (3,904kb) downloaded 88 time(s).
 
Ruffles
#463 Posted : 9/20/2021 12:33:46 AM
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Nibs wrote:
I don't know what the final product is that was produced from the main batch, but it was inferior compared to what was recovered from the foam reaction. I do not recommend using sodium carbonate for this tek, and I will be using lye next time hopefully with more consistent results.


If the main batch you mean the dark brown, that is probably because the dark brown is just gunk that is grabbed into the crystalline-like matrices of your precipitates, the lightbrown-yellow-white stuff is purer and so pound for pound, more of the true magic sand of Morpheus. This means the initial base washes or filtering weren`t enough.

You`ll have to dose more of the brown stuff. Maybe the foam keeps out the gunk while the precipitates form within the emulsion, like a sieve, leaving them clean, not a bad thing in my opinion.

You can always grab the brown stuff and acidify, filter with a tighter mesh or decant or centrifuge out the brown gunk (since it already passed through filter, the brown stuff is way less dense, it might not decant), and rebase it. The `new` precipitates likely will grab less contaminants and turn out cleaner. You can also grab the brown stuff and wash it with something slightly acidic distilled water (pH 5-6), strong shakes, maybe readjust pH up to 8, then decant.

Be prepared to lose some mass due to the gunk and losing a bit of the magic. Overall, it is worthy to have cleaner stuff, specially for smoking. You are lucky you got part of it cleaner, sometimes all you get is dark brown. Maybe accumulate more of the brown stuff before to cleanup a bigger batch at once.
 
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