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Floating preciptiate crashed out after salting? Options
 
IridiumAndLace
#1 Posted : 5/30/2021 7:44:23 PM

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Hi friends!

I'm trying out Cyb's Max Ion Tek, using MHRB powder, citric acid, NaOH, and Bestine. I froze/thawed; acidified, cooked, and decanted (x3); and finally filtered. I got 1L of tea from 50g of MHRB, to which I added 70g of pickling salt.

As the salt dissolved, a light-colored precipitate crashed out of the tea. I let the mixture stand for a bit, and the precipitate gradually floated to the top of the liquid to congeal into a semisolid mat. I was able to skim this off with a fork, and I set it aside.

I continued with basifying the tea, and in the process, the remaining floating bits of precipitate redissolved. My pulls so far have gone as expected.

I also did a mini A/B on the floating sludge I skimmed off. When I basified it, all the precipitate dissolved, other than a small amount of tarry sludge that I also set aside. I did a couple pulls on it, and yielded a lot less spice than I might have expected if the precipitate had been mostly DMT. (The first pull produced crystals in the freezer, the second just turned slightly milky.)

My question is, what was that floating precipitate? It dissolved into the acidified solution, crashed out with the addition of salt (carrying some DMT but not a huge amount), and then redissolved with the addition of NaOH.

My best guess is that it's medium-chain fatty acids that were able to dissolve in the acidified solution, then "salted out" when I added the NaCl, then saponified with the addition of NaOH. I suppose the tarry sludge is probably polymerized tannins and/or jimjam, but I don't know for sure and I'm not entirely sure what to do with it.

Follow-up question: is it better to remove the precipitate like I did, or just leave it in the tea to redissolve? I imagine I don't want to leave anything even remotely lipophilic in the tea when I'm doing my extractions, but does that small amount actually make a difference?

Or: am I the first person in the world to observe this strange precipitate?? 😯
 

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downwardsfromzero
#2 Posted : 5/31/2021 10:37:10 PM

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That is odd. The solubility profile doesn't sufficiently correspond to that of a fatty acid. Those would not be water soluble under acidic conditions, or at least, those that do are liquids. Besides that, there should not be a significant amount of free fatty acids in MHRB.

If you hadn't done the acid boil I'd be wondering if that was yuremamine. Maybe it would separate out in the Manske-like conditions, only to be decomposed on the addition of base. Seems a bit unlikely though.

Best thing to do would be to repeat the experiment exactly and send the precipitate for analysis.
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Sakkadelic
#3 Posted : 5/31/2021 11:04:53 PM

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Was your solution crystal clear after filtration? If not then there might be stuff suspended in solution and not really dissolved, they might coagulate under some conditions like adding salt or basifying and float or sink. I don't know what it could be but if it doesn't behave like alkaloids then it's not alkaloids and you can discard it, you can wash it with water or something to retrieve any alkaloids that got carried with it.

I notice something similar in rue extractions, there is stuff that make the tea cloudy and once based they coagulate and sink like harmalas and the tea becomes crystal clear, but when the solution is acidified again they stay coagulated but refuse to dissolve and so it's easy to let them settle and discard them, i am curious about what they are as i am curious to what the stuff you got might be.

I isolated mine and cleaned it but i don't know how to test it further. It's also what makes rue tea hard to filter by simple gravity filtration.
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
downwardsfromzero
#4 Posted : 6/1/2021 7:25:47 PM

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Having considered this overnight, I'd say protein is a likely candidate with that kind of behavior.
Ora, lege, lege, lege, relege et labora

“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
IridiumAndLace
#5 Posted : 6/10/2021 9:36:44 PM

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downwardsfromzero wrote:
Having considered this overnight, I'd say protein is a likely candidate with that kind of behavior.


Ohh, I didn't think about proteins!

So if the acid denatured the proteins, and the salt crashed them out of solution, how did the base cause them to redissolve?
 
downwardsfromzero
#6 Posted : 6/12/2021 8:23:25 PM

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Either because the proteins are acidic or by hydrolysis to soluble peptides and amino acids. Maybe both.
Ora, lege, lege, lege, relege et labora

“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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