Harmala Freebase doesn't dissolve... Help?

[Huxley]

Hi all,
I'm doing my first rue extraction right now and after days of filtering the liquid looked very fine. First freebasing with Soda went good and after decanting most of the basic liquid I tried to re-dissolve the alkaloids-base-mix (around 0,5L) in a hot vinegar-water-solution.
But unexpectedly it didn't work: after adding lots of the acid (3L+) there was still a lot of yellow precipitate that didn't dissolve. The liquid looks dark reddish now as it should, but the alkaloids didn't dissolve.
What went wrong?
Maybe the Soda wasn't converted well and the Bicarbonate is still buffering the solution (which is not really possible as I put so much acid into it).

So here are my questions:
- does anybody know what might have happend there?
- does anybody know the exact pH-level at which the freebase should dissolve?
- can anybody help me?

Thank you very much for you attention and I hope there's somebody out there that might be able to help.

 

[3rdI]

maybe whats left is not harmala's but other substances you dont want. filter them and keep them, then try to base your acidic solution and see if the alks drop out.

what tek you following?

 

[Huxley]

I'm following the TAO of Rue Extraction and the Extraction/Seperation Guide. To filter and process further was my idea, too. But i can't really imagine that it should all be impurities, as it looks very nice yellowish just like the alkaloids should and when I took some of the precipitate and put a little into vinegar/water it dissolved very good. :?

 

[3rdI]

ok im not sure i completely follow, which of these is it

But unexpectedly it didn't work: after adding lots of the acid (3L+) there was still a lot of yellow precipitate that didn't dissolve.

or

when I took some of the precipitate and put a little into vinegar/water it dissolved very good

?

 

[Huxley]

Yes, this is what I also don't really get...
When I tried to dissolve the base-alkaloids-mix in hot water/vinegar there was still a lot of yellow precipitate that didn't dissolve. When I later took some of this precipitate and tried to dissolve it to proof for freebase alkaloids, it dissolved fine. Does this mean I just need to add more acid? But this doesn't sound logic as the solution is pretty much acidic now....

 

[3rdI]

have you got ph tester?

when i redesolve harmala's freebase i just filter the alks then put them in a pint glass and fill the glass with vinegar(5% acetic acid) this always seems to work fine but i use the Gibran2 caapi tek on my rue.

im not sure if its neccessary to use hot water as i aint used this tek but im sure someone will come along with a bit more knowledge than myself.

im sure you wont, but dont throw anything away.

EDIT- i forgot to say welcome to the Nexus Huxley.

 

[Huxley]

I don't have an accurate pH-tester already but I'm gonna get one soon.
Of course I won't throw anything away.
Thank you very much for welcoming me to this great forum! :thumb_up:

 

[Infundibulum]

Hi all,
I'm doing my first rue extraction right now and after days of filtering the liquid looked very fine. First freebasing with Soda went good and after decanting most of the basic liquid I tried to re-dissolve the alkaloids-base-mix (around 0,5L) in a hot vinegar-water-solution.
But unexpectedly it didn't work: after adding lots of the acid (3L+) there was still a lot of yellow precipitate that didn't dissolve. The liquid looks dark reddish now as it should, but the alkaloids didn't dissolve.
What went wrong?
Maybe the Soda wasn't converted well and the Bicarbonate is still buffering the solution (which is not really possible as I put so much acid into it).

So here are my questions:
- does anybody know what might have happend there?
- does anybody know the exact pH-level at which the freebase should dissolve?
- can anybody help me?

Thank you very much for you attention and I hope there's somebody out there that might be able to help.

If you have a 0.5L of freebase harmalas/aklaloid, then you must have done a truly huge extraction or must have had a very generous yield.

Your alkaloids do not dissolve because there is not enough acid to do so. The fact that you take the undissolved precipitate and you can dissolve it in fresh vinegar supports that. So, collect it and salt it with more acid.

 

[Huxley]

Thanks for your post!
The extraction was done with 200g of rue seeds. I now filtered the solution and will try to dissolve the precipitate in vinegar. The filtered precipitate is looking much darker, maybe it's really a lot of imputities...