Titration would be ideal, actually.

SWIM is in the works of ordering some THH to run some solubility tests on. Going to dissolve it into a slightly acidic solution then titrate Sodium Carbonate dropwise until precipitation occurs. SWIM might be able to get a chemical color indicator to put in solution to help signal when the proper pH is reached.

Hmmmm, Cosmic Lion while you are at it , could you please try a "mini manske" on THH HCl (dissolve it,add salt to saturation,freeze) to finally see if THH does not precipitate during manske? It would be rather refreshing to see questions that are nowadays within our reach finally getting an answer, instead of sufficing oneself to a general broad conjecture for the years to come. Heh, that will be a "first" , a rather "quoteable" experiment!

Totally.

SWIM will work up several experiments, run them through all of you all here first for input, then procede with some specific THH tests.

Also, once separated it would be nice to do a full 3-Harmala separation from Caapi to be able to test actual percentages of each one.

this is awesome! I must once again say how I love this site and you people, and how its so nice to see real new knowledge being generated, novel areas explored, and so much colaborative work around the globe made possible by the internet! What amazing community!

cant wait to see the results of this

Does anyone see any reason why I would not be able to substitute pickling Lime CaOH for sodium carbonate. And assuming yes, how would I go about determining how much to add; first to water; and then to the caapi solution. IS there a specific PH one is aiming for. Or is one just waiting until no more precipitates form? Would saturate Lime water be the goal before adding to the acid caapi solution? I have noticed when drinking Lime water to alkalize the body, that it doesn't stay dissolved very well.

Calcium salts tend not to be very soluble in water... I could see that causing problems (like calcium acetate precipitating and ending up in your final product)

entropymancer: I don't know if thats a very good rule to stick to, for example calcium carbonate is very soluble in water. Is that the rule, anyone?

It is a good rule to stick to and no, calcium carbonate is not very soluble in water. In some practical demonstrations in chemistry production of carbonic acid (or dissolition of CO2 in water (= carbonic acid for all practical purposes) is monitored by CaOH which forms the insoluble calcium carbonate.

Calcium chloride and calcium citrate are from the few calcium salts that are fairly soluble in water.

In addition, contrary to what usually happens, solubility of some calcium salts increases as the temperature drops!

Cosmic, may I ask how you came up with the 200ML sodium carbonate saturated water volume per quart of concentrated 250G-cappi water extract.
Might this be based upon reaching a desired PH, as opposed to manske-tech whereby the saturated salt drives the Harmalas out of solution. Thanks for your time.
I would like to try this recipe yet am still trying to refine it in my head.

Great Thread.
Been wondering/thinking about extracting from my Caapi although may still keep if for brewing purposes instead.
Good reading material while I decide!

Wondering how much, if any, sodium carbonate ends up in the product. Also wondering if Baking Soda could replace Washing Soda; I don't mind eating Baking Soda...

@infundibulum ah, sorry you're completely right. Chalk is quite insoluble in water and then your rule is correct. open arse, insert head.

May I ask how you came to a 1:5 ration saturated sodium carbonate solution, 200ml per quart.
Do you have a PH meter; are you aiming for a particular PH.
I realize that you have boiled of all the acetic acid in reduction, so you obviously do not have that to contend with.
I am wondering if 10 or so is considered sufficient to precipitate all harmalas.

Update: Caapi can be pretty dark on first basification, hard to detect color change.
Therefore, having a PH goal to work with would be helpful.
IT seems excess Sodium Carbonate should be eliminated if possible because it obviously is stuck a little in the moisture in the first pull of harmalas, it can be detected by smell on the drying wet filtrate paper. Approximately 2.5 ounces of almost saturated Sodium Carbonate solution was added to 5 ounces reduced Black Caapi solution that was 125 grams to start and excessively reduced beyond the goal of 12-16 oz after being cooked several times.

Another question: How much Sodium Carbonate saturated solution does it take to raise the PH from neutral to 10?

I do have a pH meter but didn't use it for this extraction.

Titration was used and concentrated solution was added until color change was no longer noted. I would let settle for a while then add a little bit more to see if anything crashed out.

It reached equilibrium a little bit before 200ml was used but the rest was added to ensure the reaction went to completion.

A good technique may be to do the initial freebasing then instead of doing it again maybe mix it in with 99% IPA and filter the solution through a 3 micron vacuum-bag filter to remove any solid material. The IPA could be evaporated to hopefully yield fairly clean Harmine & Tetrahydroharmine crystals.

Aren't you concerned about Harmala Red with that IPA proposal?

I am not. I was under the impression this originated from one of two things:

Harmaline itself or some other compound(s) in Syrian Rue.

Seeing as how this technique uses Caapi and the fact it has very little to no Harmaline I don't see Harmala Red becoming a serious issue.

I know Harmaline has issues in alcohol but as far as I know Harmine and Tetrahydroharmine SHOULD be safe in IPA.

Alright.... i got this thing going. I won't be able to build the pump filter and finish the process until after the weekend because of travel. I ran loads of water/vinegar through and reduced it down. I filtered it and have a super clear amber ale colored quart from 100-ish grams of caapi.

Thanks allot for the tek lion. I will post my own pics when its done.

Good job dude! Keep up the good work! It seems to be the boil-down phase that turns away most people. That IS a lot of water to cook down!

I'm glad you found the tek useful, I hope it all turns out well for you. May your yields be high and your product dank!

From what I understand, Caapi doesn't really have any toxins, so why not keep the crude weight?

It seems like there is a lot of loss after the cleanup. Is the cleanup really worth it?

It's always better to have something much purer so you ingest or smoke less useless junk.