Gibran's Caapi + Muriatic acid = Fail ?

[FastFourierT]

Hi all, I recently overheard a conversation between 2 bystanders while waiting for a bus. Couldn't help but remember the details :d


"Something seems to be wrong

Started a Gibran's caapi tek with 120g of powdered caapi, but decided my modify the first step(boiling 3x) to pull more alkaloids into the solution. The following were done:

120g of very fine powder was put in a blender with 1.5L of water, muriatic acid was added until the taste was slightly sour, and it turned the blender on high for a few minutes.
Then brew was simmered for a few minutes and frozen.
Defrosted, brought to a simmer again, cooled down to room temp and went thru blender again.

Murky red liquid was decanted, and additional 2L distilled were run thru THP(approx same HCL content) with all the gunk

Result is deep red, non-clear liquid.

Same procedure was repeated on the filtered solids again, cept this time it was frozen only once and boiled in 5L of fresh acidic water(again, approx the sameHCL). THP yielded beatiful clear deep orange/reddish 5L this time.

approx additional 4-5L of warm acidified water were run thru THP, until the liquid started coming out barely yellow.


Resulting liquid(13-15L) was simmered down to 500ml pyrex cup overnight. Color was deep purple - just like mimosa brew, except it was murky.


Now the next step is where I seem to be stuck. I expected to use larger quantity of NaOH since I used much more acid than suggested tek. So I made twice of the suggested amount of NaOH water(10g/100ml) and started pouring in.

Minimal discoloration has accured, went from deep red to black with reddish hint. Keep mixing in more till nothing happened and mixed thoroughly. After an hour in the fridge nothing has happened, its still the same, no visible separation seems to occur. Looking against bright light there are some very fine particles suspended in the solution however theyre not precipitating even a little. It seems theyre uniformly spread across the entire body of water and just float like they have same mass as water.


I added more and more lye heavy water to that... perhaps up to 25g now. Nothing.

Redissolved in approx 1.5L of water and kept adding more lye solution... again still the same.

At this point the amount of lye is almost unreasonable(35g+) and still nothing is happening.

Tasting the solution I dont notice any sourness/bitterness tho... perhaps its still not basic enough even with this much lye ? It clearly does have that same soapy lye smell. I dont have pH papers unfortunately.

Is there anything I can do at this point to save the precious Caapi ?"


I wonder if indeed the use of muriatic acid is harmfull to that process, so that others don't repeat the same mistake ?

 

[gibran2]

First of all, I would advise you find a better method of testing pH than tasting your solutions! :shock: Putting concentrated hydrochloric acid or sodium hydroxide solution in your mouth is not a good idea. How about buying some pH test papers?

The acid used should make no difference. I’ve used acetic acid and fumaric acid, and got good results with both. I haven’t used hydrochloric acid, but I can’t see any reason why it shouldn’t work.

I think the problem was probably your extraction method. You used 15L of water to extract 120g of powdered caapi? I just completed an extraction of (coincidence) 120g hand-shredded caapi and needed only 2.5L. When the caapi is powdered, even less water should be needed.

Another possibility is that you used way too much acid and still haven’t neutralized it all. If the solution isn’t strongly basic (about pH 12), then you haven’t made it basic enough.

However, you say that you’ve already added 35g NaOH (to freebase what will probably be between 1-2g of alkaloids), so who knows what is going on.

With powdered caapi, all you need to do to get the alkaloids out is do about 3 simmers of 1L of water with 25mL vinegar. Allow each to settle, siphon off the liquid and collect it. Boil down the 2.5L (or so) to about 0.5 L and proceed as in the TEK. It sounds like you did something wrong in the initial step – the “preparation of the brew”.

 

[ragabr]

Infundibulum claims that HCl salts of harmalas are poorly water soluble.

 

[FastFourierT]

First of all, I would advise you find a better method of testing pH than tasting your solutions! :shock: Putting concentrated hydrochloric acid or sodium hydroxide solution in your mouth is not a good idea. How about buying some pH test papers?

The acid used should make no difference. I’ve used acetic acid and fumaric acid, and got good results with both. I haven’t used hydrochloric acid, but I can’t see any reason why it shouldn’t work.

I think the problem was probably your extraction method. You used 15L of water to extract 120g of powdered caapi? I just completed an extraction of (coincidence) 120g hand-shredded caapi and needed only 2.5L. When the caapi is powdered, even less water should be needed.

Another possibility is that you used way too much acid and still haven’t neutralized it all. If the solution isn’t strongly basic (about pH 12), then you haven’t made it basic enough.

However, you say that you’ve already added 35g NaOH (to freebase what will probably be between 1-2g of alkaloids), so who knows what is going on.

With powdered caapi, all you need to do to get the alkaloids out is do about 3 simmers of 1L of water with 25mL vinegar. Allow each to settle, siphon off the liquid and collect it. Boil down the 2.5L (or so) to about 0.5 L and proceed as in the TEK. It sounds like you did something wrong in the initial step – the “preparation of the brew”.

Hey thanks for a quick responce.

I do realise that tasting its not an ideal method to test pH of the solution, however using reasonable amount of common sense one can be pretty safe about it. I mean say theres few drops of HCL in 5L of water, I think its a pretty reasonable assumption that one can dip a finger in it without a burn. If finger doesnt burn even a bit, tasting the tip of the finger with a tongue shouldnt be dangerous either. It's not precise enough to separate harmine from harmaline but accurate enough to tell if the solution is basic or acidic.

Also, when doing the extraction, I just wanted to deviate a bit and test your method with whatever I could offer. Given my previous experiences of brewing(coupla of years), it was interesting to apply those techniques in the extraction process with the goal of draining the vine of absolutely everything. Hence the freezing/blending etc. I did not plan to have an excess of 10L in the end, however it was a cut-off point when THP stopped yielding any colour.

What if the yeild was significantly better ? worth a try, my reasoning was that in the worst case scenario Im just going to have a dirtier solution in with more undesirables pulled(I lose nothing), best case scenario - increase in the yield.(even if theres a small chance of that happening).


Ragabr, thanks for pointing that out.

Seems like theres only 1 thing I could do - reduce it down back to 500ml(going to be nasty with so much NaOH in it) and start pouring in vinegar in hopes of at least some product recovery.

Anyone has better ideas ? Could the reducing step be skipped if I can manage working with 2L of solution ?

 

[FastFourierT]

I added generous amounts of vinegar to a small part of the solution(reducing is impossible at this point due to strong NaOH smell) and fine particles(sludge almost) started to precip. Lets see if this batch is salvagable and what kind of yields its gonna produce.