Caapi extraction procedure question

[5-htp]

Hi,
I'm in the process of a caapi extraction and am encountering a problem.

I did lots of boils with little fumaric acid over the last 24 hours. The first two gave an oilie, thick, red fluid, which I wasn't able to clear with filtering. (Cotton/CF)

Cooks 3-5 filtered to a nice, clean orange fluid, which (EDIT: after basing) is actually settling with lots of Harmalas.

I wasn't sure how to proceed with cooks 1 and 2 so I based them and nothing is separating.
Now I think I should have defatted because it looks like I have to pull with NP Solvent.

Do the Harmala alkaloids behave different from Mimosa ?

Does Naphtha work for this ?

And when I salt out, can I use vinegar and shake or is it better to use fumaric acid with acetone ?

Would be nice to have them as fumarates too. Another Fumarate realted question. When I use FASA with naphtha and I add an excess of FASA would the excess stay in solution with the naphtha ?

 

[smokerx]

I don't get it. Are you trying to pull Harmalas with Naphtha?

Have you red Gibran's Caapi extraction tek ? Or what tek are you using? If none then maybe its time to start learning first. You need to understand what you are going to do before you ACTUALLY DO IT. Looks like you did it the other way round.

Go to Wiki and read. Then if you don't understand anything come back for help.

PS: I have noticed that you are advising others on Harmalas extractions while having problems with it your self. Maybe you should refrain from that till you are 100% familiar with the extraction techniques.

 

[5-htp]

I don't get it. Are you trying to pull Harmalas with Naphtha?

Have you red Gibran's Caapi extraction tek ? Or what tek are you using? If none then maybe its time to start learning first. You need to understand what you are going to do before you ACTUALLY DO IT. Looks like you did it the other way round.

Go to Wiki and read. Then if you don't understand anything come back for help.

PS: I have noticed that you are advising others on Harmalas extractions while having problems with it your self. Maybe you should refrain from that till you are 100% familiar with the extraction techniques.

Followed the tek and it worked so far as you may see on the yellow fluid.

I think that I understand what I am doing and have the opinion that one is able to give general advise from reading and experimenting even not knowing everything there is to know about everything.

By the way, thanks for answering none of my questions..

 

[5-htp]

well I found something about solubility:

SWIM has tried all sorts of solvents for freebase harmalas; methanol, ethanol, IPA, acetone, xylene are just not good enough. DCM and chloroform are the only way to go.

Since I have no DCM or chloro lying around here that's it.

Guess waiting is the only option to get something out of the sludgey soup.

It seems like these oils make it so much harder to filter and maybe somehow they hinder the alkaloids from falling out.

Just didn't read anything about oily sludges in the techniques and the tek mentioned above doesn't even consider filtering.

Thanks for your time.. :|

 

[SnozzleBerry]

Cooks 3-5 filtered to a nice, clean orange fluid, which is actually settling with lots of Harmalas.

If the solution is acidified, anything settling is not harmala alkaloids.

It really sounds like you need to re-read the tek again. There's zero need for non-polar solvents.

Here's a brief simplification...

Key
What your alkaloids are
S = Salt
FB = Freebase

1. Acidified water extraction(s): S
2. Combine/reduce extractions: S
3. Base extractions: FB
4. Filter solution, collect precipitate: FB
5. Fin.

Harmala salts are water soluble, freebase is not.
If you're having trouble with the precipitates appearing add some more basified water.
If you're having trouble with the precipitates collecting at the bottom, pop it in the fridge.
You don't have to decant the water off the alkaloids, you can collect them in a coffee filter.

EDIT: AHAAAAAAAAA...I think it may be how you've worded your post. You don't need a clear solution to base and precipitate harmalas out of. You can add more base your initial acid cooks without worry. There's no need to defat, especially not caapi. Did you see any color change when you based your first brews?

 

[5-htp]

Cooks 3-5 filtered to a nice, clean orange fluid, which is actually settling with lots of Harmalas.

If the solution is acidified, anything settling is not harmala alkaloids.

It really sounds like you need to re-read the tek again. There's zero need for non-polar solvents.

Here's a brief simplification...

Key
What your alkaloids are
S = Salt
FB = Freebase

1. Acidified water extraction(s): S
2. Combine/reduce extractions: S
3. Base extractions: FB
4. Filter solution, collect precipitate: FB
5. Fin.

Harmala salts are water soluble, freebase is not.
If you're having trouble with the precipitates appearing add some more basified water.
If you're having trouble with the precipitates collecting at the bottom, pop it in the fridge.
You don't have to decant the water off the alkaloids, you can collect them i na coffee filter.

Thanks for the answer. I'm sorry that I didn't express myself clearly and see where I made the error. The settling in the picture is after basing of course. I'm aware of the procedure and know the difference between freebase and salt .

The only problem so far is the combined solution of cooks 1 and 2 which is not separating alkaloids from the solution (but is cloudy). I added around 20 G of base in solution so far which should be more than enough (No PH-Strips available at the moment).

Both pictures are from the same batch at the same stage with the same preparation and just different "fractions".

I tried the fridge for several hours and there seem to be small fractions where the liquid is just clear black, like holes in the solution but overall it hasn't moved down.

Maybe filtering the sludge now would speed things up, but the Harmalas don't coalesce like in the yellow fluid and maybe this will be very inefficient as they may slip through/get stuck in the filter. Or maybe I have to add more water, maybe with some base to dilute further so the alkaloids can coalesce. Will try this now. THX !

 

[SnozzleBerry]

The only problem so far is the combined solution of cooks 1 and 2 which is not separating alkaloids from the solution. I added around 20 G of base in solution so far which should be more than enough (No PH-Strips available at the moment).

Both pictures are from the same batch at the same stage with the same preparation and just different "fractions".

Maybe filtering the sludge now would speed things up, but the Harmalas don't coalesce like in the yellow fluid and maybe this will be very inefficient as they may slip through/get stuck in the filter.

I'm with you now.

Two questions on those first brews:
1) Did you see a color change after basing (good visual indicator, no need for pH strips)?
2) Did the solution appear to get thicker/sludgier, like things precipitated into an oily-ish solution?

If yes, I would attempt to collect the alks with a coffee filter and re-a/b.

If no/they slip through the filter (indicating, imo, they aren't fully based), I would add some more lye solution just for kicks and see what happens.

Sorry for the initial confusion Long day at the office.

 

[5-htp]

Two questions on those first brews:
1) Did you see a color change after basing (good visual indicator, no need for pH strips)?
2) Did the solution appear to get thicker/sludgier, like things precipitated into an oily-ish solution?

If yes, I would attempt to collect the alks with a coffee filter and re-a/b.

If no/they slip through the filter (indicating, imo, they aren't fully based), I would add some more lye solution just for kicks and see what happens.

Sorry for the initial confusion Long day at the office.

AWESOME :d

1) Jep, went darker/black with tiny lighter particles floating in it which I can't differentiate from plant matter.
2) Can't really say, because it was sludgy to begin with.

You know what, I will simply try base some more and try filtering and see what I get

 

[5-htp]

When I looked at my soup again, I saw something happening. So guess I wait and procede with the tek as written. (Re A/B/washing) and report back so that this may be useful for someone encountering a similar problem.

I wonder if washing cooks 1 and 2 before the basing with NP Solvent would have helped the process. Maybe I try this next time.

The picture is taken 6 hours after basing.

 

[smokerx]

By the way, thanks for answering none of my questions..

No need to thank me if you do not appreciate my critical words and advise.

I still believe and as I read here I am not on my own, that you do not understand your tek properly that is why I wrote the comment above.

I suggest you read the attitude section if you have not done it yet.