tl/dr: I have gotten over 11g of dried powders from 200g caapi vine. It would be nice if they were all harmalas but I suspect there is something else, me being a noob at this. What is there I don't know and was hoping maybe someone could:
1. enlighten me as to possibilities/probabilities of what this powder is and
2. ultimately suggest a way to clean them if possible?
How did I get here?
Its a long process over the last 4 months!
Basically I have been following Gibran2's tek. I have only ever done harmalas from Rue before and got pretty good yields, some beautiful manske crystals and quite whitish powder.
So now I wanted to utilise some caapi I have had around for years!
Starting material: 200g hammered and hand shredded dried "yellow" caapi.
Boiled 3x with dash vinegar added each time for 45min and liquids reduced to about 800ml
Result a deep red liquid. Filtered through cotton then coffee filters.
Solids run through my blender to mash up further.
Boiled this again 2x for 45min with dash vinegar added each time.
Filtered again through cotton then coffee filter (much more difficult now and much more discarded residues)
Reduced second set of boils (4+5) to around 400ml. Also deep but clear red.
Acted separately from here on in on session 1 (1-3) and session 2 (4-5), thinking session 2 would be quicker to result and I would let session 1 settle longer in the meantime.
Basified both with around 100ml of 10g NaOH/100ml DH2O. Probably too much but I wasn't patient enough
Never went black with white precipitate like Gibran's pics - I have seen this with rue but never once saw this with the caapi. Always was a darkish clouded caramel liquid. Took over 3 days to see any signs of clearing at the top when the precipitate began making itself known.
Whenever I felt there was enough precipitate I would decant, save the liquid (still very cloudy) and then start the add DH2O and settle-decant-add DH2O etc until the supernate was relatively clear golden yellow. I was not in a hurry and did the first session like this over two weeks, always keeping the 'discard' liquid. The bottles of that started obviously proliferating!
After a few decants and add water I did the acidify step and decantered/filterd out the black stuff that dropped out. I then added some NaOH solution as before (maybe too much because of lack of waiting to notice the precipitation - I was expecting something immediate like rue but what happened here was it went cloudy then puffy precipitae stuff was only visible a little later) proceeded to do over 20 of these, letting it settle in between but was never able to get pH lower than 12.
I thought I would add a bit of vinegar to the mix to hasten the drop in pH. Big mistake! The precipitate disappeared and I got black fallout again. It was basically a redo of the acidifcation step!
So - after filtering the black stuff of the cloudy red liquid I add NaOH again, little more carefully as now I knew what to expect. Again, settle, decant and add DH2O. Many times, pH never lower than 10. Each of these steps takes essentially a day. Eventually I give up and dry it.
First result: 3.2g of powder! Wow. Much more yield than expected (I am expecting around 2% from what I have read)
Okay, so imagine what the first 3 boils will deliver!
Meantime, my bottle collection is growing and stuff is still falling out of the "discarded" liquids. I keep siphoning it out and consolidating it. After 3 weeks I go through the process again with this collection (session 2: part 2). Did the acidification twice again. Each time I got fallout so I assume the cleaning step is not good. Never do I get it as white as Gibrans pics.
Anyway, ends up another 1.6g dried, slightly darker this time.
So now I go back to session 1, expecting serious amounts of powder here!
Now, I don't know what went wrong but I ended up with almost nothing!! What I did get was a dark, almost black shiny powder. less than 2g. Most disappointing. Feels like I dried the stuff that the acid step dropped out, but I know it wasnt! For certain. I was ultra careful with this as I expected it to be the primo yield.
Sadly I moved on.
Bottles and bottles of cloudy dark yellow liquids from all sessions...I just left them until they were pretty clear and again consolidated the precipitate and left the liquids to keep settling.
After over 3 months of this (exclusively "discarded" liquids) I go through the clean and dry phases again and reap 6.18g of powder. This time some very white and most this sort of grey tan color.
So now I have well over 11g of powder, excluding the weird shiny black stuff.
And there is still stuff coming out from the discard liquids!!
What the heck do I have here? NaOH? Harmalas? Other alkaloids? Any idea? Can I clean what I have?
Pics follow now.