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Purifying Alcohol Pulls by salting out?

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modern

Esteemed member
This is just an idea that I'll be working on in my free time but was wondering if anyone things there is any chance it might work

I got the idea from this paper Salt Effect on Ethanol-Based Aqueous Biphasic Systems Applied to
Alkaloids Partition: An Experimental and Theoretical Approach Sci-Hub | Salt Effect on Ethanol-Based Aqueous Biphasic Systems Applied to Alkaloids Partition: An Experimental and Theoretical Approach. Journal of Chemical & Engineering Data | 10.1021/acs.jced.8b01024

So I chose to use 70% isopropanol but in the future I'll be using ethanol since all our rubbing alcohols are ethanol. Isopropanol has a lower polarity and better salting out effect than ethanol.

Potassium carbonate is most effective at phase separation but I went with sodium carbonate due to cost and access for me. Even Sodium chloride is possible but has a higher solubility in the alcohols than wash soda.

So I just did a mini run with a few grams of lopho fresh weight. I let it soak in the 70% iso for 3 days so it pulled as much as possible in 2-3x volume. In total I started with 30mL alcohol.

So I filtered out the plant material which had very little color and continued to process the extract.
I added 1:1 saturated sodium carbonate solution with the alcohol and it started to separate phases. I did this a few times separating with a syringe. In theory the mescaline should be freebase and any that is still soluble in water should be pushed out of the salt rich water phase and into the alcohol phase that likely still has around 9+% water.

After these pulls I added citric acid to see if there was any clouding that occurred. It would gas so likely nutralizing the ph from the water in the alcohol. I started with same ratio as cielo 5g/L but it took around 25g/L to become about neutral ph maybe a bit more. I ended up adding 10x or 50g/L to the solution which is very excess and the ph at around 25-30g/L was already acidic.

After it all dissolved I put it in the freezer for a couple hours but nothing happened due to the water so I evaporated everything on a hot plate. Ended up with a thick hard goo. I added 99+% isopropanol mixed well trying my best to break up the goo and mix. I heated up the alcohol and filter out the hard dry goo.
I now have the alcohol in the freezer.

I'm not expecting anything really since I started off with a tiny amount of material but This might work with an already reduced tea/tar. I'll try this again in the future with a higher starting material so if it works atleast I can visually confirm. Crystalizing directly in the salted out alcohol is very unlikely but this could work to purify the reduced tea/tar and then you crystalize with 99% iso.
 

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Sodium carbonate does a nice job of separating ipa and water. I was playing around with this several years ago and even found that it could produce 3 liquid phases if a naphtha phase was also present! In that instance, a red DMT migrated into the middle alcohol layer. There were also crystals of SC that formed at the very bottom, so I clearly remember being entertained by it being a four phase situation. It does hint that DMT may migrate to an alcohol phase in preference to naphtha as well, since its solubility is far greater than that in the latter.

Not that this applies to mescaline, which doesn't really dissolve in naphtha at all - however, it does now make me wonder what the analogous situation would be with something like toluene, xylene or limonene. Where would the mescaline freebase prefer to be then? Pushing it from a hydrocarbon into a moist alcohol could possibly be advantageous. Adding an antisolvent like naphtha or, better, heptane could help with the push/pull too. Not that this would be necessarily useful but now that the concept has presented itself, well, it would be fun to find out (assuming it doesn't just make a total mess :lol: )

There was recently a Welcome Area thread about the salting out of alcohols from aqueous mixtures. There were some links to useful patent information so a cross-reference is in order here.
 
Check out Ogunbodede's original work. He describes initial alcohol extraction followed by traditional A/B. Alcohols (EtOH / MeOH) are the go to for botanical extraction; there's a reason nobody has been able to recover clean crystal alkaloids by directly salting the alcohol extract - there simply too much other stuff in there. The reason CEILO works is the extraction solvent, ethyl acetate, is more selective than alcohol (which pulls more junk). Perhaps there is a way to selectively precipitate the tars, chlorophyll, etc from the alcohol extract prior to alkaloid recovery via salting, but seems unlikely.
 
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