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Dissolving freebase in acid? Options
 
kinkyking
#1 Posted : 4/19/2011 9:57:52 AM

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Goddamn freebase Harmalas don't like to dissolve in acid. what to do? here's the full story:

1- Added lye to Rue soup, freebasing all of the alkaloids.
2- Siphoned and discarded everything except the alkaloids at bottom.
3- Added water and repeated #2 five times until a crystal clear liquid remained with freebase alkaloids at the bottom. then siphoned and discarded the excess crystal clear liquid.
4- Now with pure wet freebase alkaloids at hand, added straight pool acid (without diluting), a nice red crystal clear formed, but with some of the freebase alkaloids still sitting at the bottom.
5- No matter how much acid SWIM added to the solution, the remaining freebase alkaloids just don't like to dissolve.

What the hell is this remained stuff? is it really freebase harmalas? or some junk that was clotted when SWIM added lye?

SWIM dabbed his/her finger in the solution and tasted it, very very acidic! so this excess acid would have salted any remaining freebase alkaloid in theory, what's wrong?
 

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endlessness
#2 Posted : 4/19/2011 11:07:06 AM

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what is 'pool acid'? How concentrated is it? Sometimes alkaloids may dilute better in dilute acids than in concentrated acids. How warm is it? Maybe warm whole solution and mix well, break the precipitates appart/press them, etc.

If after all of this some doesnt dissolve, I would guess its impurities. You could decant/filter, keeping impurities just in case, then add lye to your solution again and see if your alkaloids are there and precipitate.
 
kinkyking
#3 Posted : 4/19/2011 11:21:46 AM

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By pool acid I meant hardware-grade HCL acid.
I didn't add dry and rock hard freebase chunks, the freebase I tried to salt was still wet and soft like cream. I added room temperature hardware grade HCL acid and the color turned red instantly, a little stir and everything was gone, then after a while clouds began to form and then settle (exactly similar to when you stir a freebase solution and then clouds form and settle).
I thought maybe the acid is not enough to neutralize all of the alkaloids, so added more, more, more, more, then was like "WTF! this stuff is eating all of my acid!" then tasted the solution to see if it's acidic or not... wow very acidic! I could feel my teeth began to turn into calcium salts!

So it is impurities? I guess these were proteins or god knows what that sticked together and clotted solid when I added lye.

 
Crystalito
#4 Posted : 4/19/2011 12:39:03 PM
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Hydrochlorides may precipitate in HCl solutions...try adding water and heating up a bit with good stirring. It goes without saying, watchout for HCl fumes.
 
endlessness
#5 Posted : 4/19/2011 12:49:04 PM

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Idea: Next time use an acid like vinegar, theres no need to use HCl for this.

Also wtf, tasting concentrated hardware-grade HCl solution?! Please be more careful next time, thats what pH papers or pH meters are for, dont use your tongue Confused
 
gibran2
#6 Posted : 4/19/2011 2:30:28 PM

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Your original rue soup no doubt contained some insoluble impurities, as it always does. These impurities will settle with the basified alkaloids and will not dissolve when the cleaned alkaloids are acidified.

Take a look at this thread (it shows what to do with insoluble impurities from caapi brew) to learn more.
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kinkyking
#7 Posted : 4/19/2011 3:00:21 PM

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Gibran2, the impurities (or possible freebase alks??) I'm talking about look exactly like this:
https://wiki.dmt-nexus.m...API_EXTRACTION_05_01.jpg

Same color, and same distinctive form. So these are impurities?
 
kinkyking
#8 Posted : 4/19/2011 3:03:34 PM

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What I'm saying is I had lots of these freebase alkaloids https://wiki.dmt-nexus.m...API_EXTRACTION_05_01.jpg then added acid, 70% of those dissolved and turned into a red solution, the remaining 30% doesn't want to dissolve no matter how much acid I add. So basified impurities and freebase alkaloids look similar?
 
SnozzleBerry
#9 Posted : 4/19/2011 4:00:25 PM

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kinkyking wrote:
What I'm saying is I had lots of these freebase alkaloids https://wiki.dmt-nexus.m...API_EXTRACTION_05_01.jpg then added acid, 70% of those dissolved and turned into a red solution, the remaining 30% doesn't want to dissolve no matter how much acid I add. So basified impurities and freebase alkaloids look similar?

No, you now have acidified impurities, which could be said to look similar to freebase alkaloids, but not really, only in that they are solid. If you have solids that refuse to dissolve in acid, even when heated or exposed to large volumes of water, they are not alkaloids. They are most likely various plant compounds that will not dissolve in acidic solutions. This is why, after acidifying your freebase, you should run it through a filter, to separate your water-soluble harmala salts from your water-insoluble unwanted products, further cleaning your material for the next basification, yielding cleaner freebase than your last precipitation.
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endlessness
#10 Posted : 4/19/2011 4:04:23 PM

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^ Snozz is right. But do note that these solid impurities may also be trapping a bit more alkaloids inside so its recommended to break them up and insist on mixing a bit before filtering.
 
gibran2
#11 Posted : 4/19/2011 4:32:51 PM

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kinkyking wrote:
What I'm saying is I had lots of these freebase alkaloids https://wiki.dmt-nexus.m...API_EXTRACTION_05_01.jpg then added acid, 70% of those dissolved and turned into a red solution, the remaining 30% doesn't want to dissolve no matter how much acid I add. So basified impurities and freebase alkaloids look similar?


In my experience, the insoluble impurities are usually much darker in color than the freebase alkaloids. With caapi, the impurities are often dark reddish-brown, and with rue they are often brownish-black to black.
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kinkyking
#12 Posted : 4/19/2011 6:48:57 PM

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Dagger wrote:
Have you tried adding more water? Maybe the harmalas has a relatively low solubility in hcl salt form.

Hmm but HCL salts look yellow/orange not cream/white.

SWIM will filter the mystery soon and try to dissolve it in some vinegar in a separate dish to see if it dissolves or not, if not, then that's just some junk mimicking the appearance of freebase alks (case closed).

I personally guess they are some denatured protein clots. Rue soups always look dirty and not clear, (lots of small proteins and other junk floating around) but upon basing the soup, suddenly the solution becomes transparent after letting it sit for everything to precipitate. so it must be the proteins that get denatured and settle at the bottom together with freebase alks.
 
 
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