Reducing is most likely not the issue. Reducing is necessary only to get a convenient workable volume. This TEK should work on brew that isn’t reduced at all.

It’s possible, though unlikely, that you didn’t add enough NaOH. Maybe you could take a small sample of the decanted liquid and add more base. If it gets milky, then you’ve found the problem.

Another possibility is that the sediments that have settled are your alkaloids. If you didn’t stir at all, they might be much finer than the usual clumpy aggregations. I’d continue with the extraction, but save at least the first two rinses.

You can always acidify the basic decanted liquids and then boil them down again if you think they might contain some alkaloids. If you discard nothing, and if there are alkaloids present, you should be able to retrieve them.

A final possibility is that your vine is bunk or that you didn’t boil it long enough to get appreciable amounts of alkaloids out. A solution going from brown to black when base is added is consistent with no alkaloids present.

Yeah. When I added the NaOH, I stirred slowly for five minutes after. When I did the boils, I did each one for 30+ minutes. Maybe I gots me some bunk vine. Going off to try adding more NaOH to a small sample of the original liquid, but I doubt anything will happen, because it smells slap you in the face base.

Well, when I added more NaOH the brew got a little cloudy for a few seconds. So I added 10 grams to the original volume of the already black liquid. It got a little cloudy froth on top, but that's all. I'm letting it site for a few hours, then I'll decant. I'm not hopeful though. No obvious precip, but it is dark as night in that jar. So who knows.
The first wash was decanted and the sediments appear to be just that. Black plant material. Second wash settling now.

I guess I'll order some black vine today.


UPDATE - Things seem to be happening. I took the jar that I added more NaOH to out into the sunlight and I can see that there is about an inch thick band of settling precipitates forming at the bottom. Finally! I put the jars in the fridge and will check them 18 hours from now to see how things are moving along. Yes!

Well... I don't know. freebased after removing the insoluble gunk during the second acidifying step. It got dark amber and reddish precips slowly fell out. They sparkle in sunlight but look more like tiny globules of oil than crystals. On the third wash and I'm at about ph 10. I'll decant and wash again in the next hour or so. I wonder if this stuff is going to be active. Has anyone had success with RED VINE before? Is it possible that there's something in the red vine that stops crystals from forming? The only thing I did differently form the original tek was boiling with the lid off. I somehow missed that even though I read the tek several times. What could I have done wrong?

From what I understand, this tek won't give you crystalline caapi alks. In my experience with this tek, you'll end up with an off-white precipitate.

Not sure why yours are an amber color... Maybe it's just a trait of the red vine? I don't have any experience with the red vine, so I can't say for sure.

If you want the caapi crystals, you'll have to try what Narmz said and add the NaOH solution dropwise or look for the other threads by Enoon and Gibran where they explain how to do it with alcohol.

I'm not sure that you did anything wrong just yet. Maybe upload some pics so we can see exactly what's going on.

I have a question about doing this on syrian rue. So you do the a/b, and then most people suggest doing a manske after the a/b to make sure the product doesn't have non harmala alkaloids in it. But will the manske work on a product that is very basic?

The product wont be basic because you need to redissolve it in warm acidified water, and then saturate with salt.

If you do a Manske, it would be done before the final basification, so the solution would still be acidic. The final basification is done only to get the alkaloids into freebase form. If you wanted freebase alkaloids, you would do the final basification AFTER the Manske.

oh, ok. Now I think I might actually be confident enough to attempt this finally.

I'm trying this with the leftover of my last strong brew, approximately equal to the amount I imbibed for the journey that lasted over twelve hours.

I put the remains into some boiling water, and added additional vinegar just in case. It wasn't dissolving with simple stirring, so I put it on a stirplate. Then I noticed this: something extremely gummy and sticky. Should I continue, even though it's refusing to dissolve?

Sure! You've got nothing to lose. Maybe the sticky stuff is just congealed plant resin or something?

Try microwaving it for 30-40 seconds or so. This problem has been encountered before, if that fails try adding 20 or so mL more vinegar. If that fails consider it an impurity and perhaps try filtering it away.

Nice stir-plate !

@Mydriasis, thanks! Adding a bit more boiling water and leaving it on the stir plate got pretty much everything dissolved. The stir plate actually has a huge dent in it, which doesn't show in the picture, which is how I got a hold of it, but it still gets everything done.

My main interest in getting this extraction done was finding out approximately how much weight of harmalas SWIM consumed in this experience. The major portion of the extraction yielded 242mgs of harmalas, with what I suspect to be around 50mgs more retained. This is towards the upper end of the recommended pharma dosage, but not a huge amount by any means.

I do tend to be much more sensitive to harmalas than other reports on the Nexus. When I have the time for a potential 10-hour journey, I will try this dose and compare intensity and length to see if we have more evidence for tannins slowing the processing of bound harmalas.

Edit: And thank you gibran2 for putting this together!

Does anyone know if harmala fumarate would work? After you base, and do the acid wash to remove solid particles, what would happen if you did the acid wash not with vinegar, but with fumaric acid? Could you then let the FASW with harmalas evaporate to yeild solid harmaloid fumarate salts!?!?!!?!?

I've done it with syrian rue and it worked like a champ. After adding the fumaric acid, let it sit in the fridge for a few days. You'll end up growing some pretty cool fumaric crystals. The longer you let it sit, the more it will crystallize.

Excellent! I didn't expect it to precip right out of the water. What amounts of fumaric acid is to be used? What were your yeilds like? Did you also do a manske, or did you just use fumaric acid after basifying?

I can't really say what my yields were, I botched a couple of times by spilling some stuff here and experimenting there...

I don't remember exactly the procedure I used, I do remember doing the manske at least a couple of times to try to clean the alks up as much as possible. They were still really dirty when I put the freebased alks into a small amount of water and then added a boiling hot FASW solution. I remember shaking the hell out of the jar to get everything mixed up real good and then I let it cool down on the counter. Once it was cooled, I let it set in the fridge for a few days.

Attached are the resultant crystals I got. (There were a lot more)
It seems that most of the impurities clung to the fumaric acid.

After a couple of days I filtered the water and basified it and got some really pure harmalas. (In the next photo)

I got quite a bit of each kind but I don't know the exact yields. I've been wanting to try it again but I haven't ordered any more rue seeds yet.

I have read every post in this topic twice now, and have seen nothing said about using Phosphoric acid in place of vinegar or fumerate.

Would this present any problem in the extraction?

I have read every post in this topic twice now, and have seen nothing said about using Phosphoric acid in place of vinegar or fumerate.

Would this present any problem in the extraction?

Dagger comments here, in response to someone having trouble doing a caapi extraction with phosphoric acid, that harmala phosphates have a poor water solubility. If this is true, then it would cause trouble during the removal of non-soluble particulate step in this extraction.