I'm interested because if losing THH is not a problem, I'm not convinced basify-ing is the best approach for Caapi extraction.
Maybe it is, but it would be curious do to a side by side with the two approaches and see what comes of it.

This might not be of interest to all you folk conveniently ordering you harmalas these days, but I hope it is

SWIM has been wondering for a while, so he took 5 drops (17.5 mg) and placed in a shot glass, filled it 2/3 up with boiling water and thoroughly saturated it with salt. (had to poor into another shot glass because not all would dissolve)

This literally happened (in his imagination) about 5 minutes ago

The shot glass is still warm but is cloudy and looks like FASA added to limonene right now (lots of flakes). SWIM thinks probably yes, but he'll have to collect and bioessay it to be sure.

So SWIM filtered the manske'd stuff and there was a white precipitate. He re-dissolved the precipitate in vinegar and it had the same color as the THH.



Since 17.5mg is not very strong dose, or at least SWIM would assume the effects would be almost enough to write off as placebo he added 5 more drops to the mix to make 35mg and took it sublingually.

He feels effects very similar to those he has felt from 40mg THH sublingually.

He is convinced it does work.

SWIM would be completely comfortable doing a manske on his caapi without fear of losing THH!

Thats the kind of experimentation i like...There seems generally to be much information going around like a dogma that CAN be tested if it is true or not (purely physical data) but noone seems to bother really. I wonder why...People cant be asked?

Two thumbs up for veryfying it!

Thanks I am grateful and realize that those who really want to push the envelope actually need to accept that the process of testing involves failure, and therefore loss, which equates often with finances. It is easy, for example, to see why an average person would rather see the other-fellow do the test, and thereby lose 'his' product but not mine. I feel that well constructed experiements are worth the lossage that accompany them. However, being a bit of a newb it is a little harder to get up the courage to attempt experiements for the sake of entheogenic science. I see this efforts and prime toward our evolution period. And my heartfelt thanks to see this carried one step further. As my understanding exapnds, and as I find myself more capable I would love to be willing to take on the 'loss' that it takes to further the important experiements. i had envisioned an introductory post that touched upon this as other significant points regarding the contribution potential of a nexus member. Good Day to all...

SWIM is gettting a PH meter (soon he hopes) and he has probably 300mg left of THH.

Considering now it is proven to be manske'able he could just get a bunch of caapi. Thus he could put up most of it for experimentation.

SWIM is nowhere near a chemist, could someone spell out a method to approximate or even pin-point the PKA.

SWIM was thinking taking 100mg.
raising the PH in .5 increments
waiting ? hours for precipitation/crystalization.
Pour off, color crystals (weigh)
repeat until no precipitation is found.

Then do a more precise test using .1PH increments or something.

SWIM heard something similar to that to be done with caapi-extract but lots of harmine would require a lot more work.

if anyone can spell out the experiment, SWIM will perform it.

Sounds like a process of narrowing down...

For example if the PKA-- which I belive it is-- is the PH point at which Half of a given compound becomes available-- mutating from either the base or salt to the opposite-- then the experiment involves guessing and revovering the precipitates. For example, if you guessed late and you have 2/3 of freebase thh-- converting from the salt-- then you would back down the pka. I'm not exactly sure of what use the technical PKA is compared to the-- and I'm not sure why they dont have a fancy acryonm for this-- the point at which all the salt is rendered into freebase. And it seems, for those trying to isolate, with a given plant with various, versions of harmalas, then there is that possibly even more elusive point that one wants to stop at. For sake of dividing. Sorry for the ramble; I'm not exactly sure what I am trying to say; but I guess I am having a little bit of fun trying to figure it out... Hope you are too...

looks like we need to find some way to to seperate THH and Harmine without using PH ranges, then just manske it out (whichever one is left in)

If I remember correctly 69ron posted that THH would not dissolve in over a cup of citric acid + water. This may be the answer, precipitate THH with citric acid then manske the harmine out (if it works with harmine citrate)

I wonder if you just stumbled on FV's tech?


P.S. q21, may I ask the pourocity of that filter bag/material, kind of looks like a bubble bag.
That looks like very fine precipitates, the kind that seem to be flowing right through my coffee filters and 101 filter paper.

hahaha (completely respectfully laughing at the situation)

It's a 100 count for $1 coffee filter, manske particals are much much bigger than those tiny freebase particles.

Thanks for clarifying that...
I was getting anoyed but am a little less now.

I don't understand why cosmic-lion didn't seem to be having that (precipitates running through filter) issue collecting his harmalas with his pressure pump and coffee filter paper.

To me this is another good point for Manske over Carbonate Freebase for Caapi extraction: size of precipitate.

It seems the smaller it gets, it is also hard avoid the gunk/particles sticking to/with the precipitates...

I just ordered some 102 & 103 to try and resolve this...

Are you setting up the citric acid experiemenet as we speak...

Was that with a Manske-style extraction? (by which I mean, was there salt in the solution?)

With Manske precipitations, there's a couple of equilibria involved. There's the equilibrium between the protonated (ionic) and unprotonated (free base) forms in solution, which favors the protonated form below the pKa of the molecule. But there's also the equilibrium between the dissolved free base and the undissolved (precipitated) free base. The ionic strength of the solution causes some of the free base to precipitate, which by law of mass-action causes more of the protonated form to convert to the unprotonated form (to maintain that equilibrium), and again some of this new free base precipitates, again converting more protonated molecule to free base by law of mass action, and so on... this continues until the whole system has reached equilibrium (exactly when this is depends on the exact amount of salt dissolved in the solution, as that's the primary factor influencing the free base precipitation equilibrium)

I guess I'm not understanding the question then...



Are you saying that only 50% precipitated total, the other 50% remained in solution up to pH 10? Or that 50% precipped at pH 6.9, but the rest could be precipped by taking it up to 7 (at which point more would precip and the pH would drop slightly) several times?



As to the initial question of how to pinpoint the pKa, precipitation is not a good indication, because the precipitation equilibrium is separate from the protonation equilibrium. To find the pKa, you'd want to monitor the presence of the protonated form in solution (for example by using a spectrometer to look at a wavelength emitted by the protonated form but not the unprotonated form), and titrate to find where the concentration has been reduced by 50%.

The results still seem inconclusive.

Someone needs to take a gram of THH HCL and do a Manske then weigh the results and compare to see if any THH is lost during process.

At least so far from my first experiment, there seems like there might be a little trouble getting all the caapi alkaloids to precipitate in this manner.

Approximately 1 gram of Freebase Caapi Harmalas were dissolved in hot-vinegar-water and then precipitated using the standard 10/100 salt/water ratio respectively.

This was after attempting to use 20/100 salt/water ratio. Figuring that solubility of salt in water is approximately 36/100, Swim figured this would give a little more assurance toward the goal-- hopefully avoiding possible excess loss. However, this amount of salt, being added first created instant precipitation in the boiling glass teapot, thereby indicating an excess of salt, once again, at 20/100 ratio. Solution was then given double the water and cleared up.

As a matter of fact just tested, was a solution after re-x 1 gram rue alkaloids Manske style: 10/100 Salt/Water
Solution was basified yielding absolutely no color change and additional alkaloids.

Caapi alkaloid solution however, after collection of beautiful Yellow Salts, was re-basified and showed classic color change and released what seem to be, at most, an additional 5-10%.
Unfortunately, not having recorded exact weights, an exact figure will not be available for this experiment.

Nevertheless, the conclusion is that there is some trouble when attempting Manske of Caapi.
Not to mention the large needles, characteristic of Rue Harmala Salts (harmaline?) were not present in the Caapi salt precipitation.
And, guessing due to the salted water and very small crystal formation, precipitates were a bit harder to collect that the standard Manske on Syrian Rue.

I'm going to try one more time; and if loss seems excessive enough to indicate-- especially-- non precipitating THH, then this approach will be discarded in favor of some kind of re-acidification and evaporation to yield the desired Caapi Harmala Salts for tincture making.

Update, collected alkaloids weight more than expected, maybe due to settling for a couple of days this time.

To recap the experiment:
Base Caapi alkaloids were re-dissolved in vinegar/water and then Manske'd at 10/100 salt/water ratio.

.94 were collected as lovely yellow salts.

The remaining solution was basified.
Color change indicating plenty remaining alkaloids.

Total base alkaloids collected = .64 X 1.28 =.81

Conclusion: Almost half of the Caapi alkaloids Didn't precipitate applying Manske salt tek.

WIll try one more time...