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Wierd precip from Manske

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FiorSirtheoir

FiorSirtheoir

Rising Star
I will elaborate the full process I have been experimenting with once I get some yield numbers. But, what I ran into was something I thought strange. I had done a couple of A/B's (with lye) on some rue and then did a manske on it. I put the NaCL Harmalas saturated water in the freezer for about 12 hours (it didn't freeze), then collected all the salt, some of it was clear. Well once I had all the salt I dissolved it warm water I then acidified the water, as soon as I acidified it it began to precipitate. I collected it and have it drying, even let the acidified salt solution sit for a few days to get all the precips to settle, and collected them. Any idea what the precip is, and why did it precip when acidified?

Thanks yall!
 
Let me start to dispel some of the mysteries here as best I can :). I like your observations, your picking up on some neat things here.

1) The reason why your solution did not freeze is because of a colligitive property(physical property) called freeing point depression. The more ions in solution the lower the freezing point of the solution becomes. :) This is why if you put salt into ice water, the ice melts(and the water actually get's colder then 0*C/32*F).

2)Now why was some of the precipitate clear. It's salt(NaCl)! It came out of solution because the as the temperature goes down the solubility for salt in water decreases. Or perhaps you poured in a little too much, no big deal.

Now to the meat of it here, what your probably actually wondering about.

Well what the manske does is it forms the hydrochloride salts of the harmalas, ex: Harmine HCl, Harmaline HCl. Keeping in mind Harmala 'salts' are soluble in clean water. So before you added your acid, you already had them in their salt form. So what essentially happened here, this is my guess. You had an excess of salt in your precipitate(#2). Now there is an effect and this is actually how the manske works, when you have a 'salt' of an alkaloid(Harmine HCl) and you put it into a solution with a 'common-ion' in this case Na Cl(Notice the chlorides) the Harmala HCl's become less soluble in solution.

Back to #2, when you raise the heat of the solution the solubility increases(in this case). So your harmalas went into solution in the warm water. Then you added I'm going to assume here acetic acid(vinegar) which was probably room temperature. This cooled the solution, lowering the solubilities of the Harmala HCl's and the common ion(Cl- Chloride's). So I'm going to go on a limb here and say your precipitate is Harmala HCl's, these are generally yellow when fairly pure and brown/yellow when impure.


Now -
What you can do to receive the freebases is add NaOH solution to your acidified solution with some stirring.It won't be instantaneous and it may take a little more NaOH then you were expecting to use, but given enough time with the right amount of base you should end up with a tan to brown precipitate(dependent on purity).

Hopefully this helps!
 
I do appreciate your efforts in dispelling mysreries, however this is not my first rodeo. The precipitate is not salt, it is an alk of some kind. I can tell from the taste, doesn't taste salty at all. It does have a yellow color, none of it was clear. I have done a sodium carbonate to the solution the manske salts were dissolved in, it precipitated, and then KOH, that precipitated too. I will get weights once everything drys out and pictures. It is just strange that it precipitated once acidified.
 
FiorSirtheoir said:
It is just strange that it precipitated once acidified.
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Yea...the stuff that precipitates out when acidifying a basic solution is not alkaloids, but is in fact plant "junk" tannins/oils, etc. This is how a/b's clean up the extract from the crude state post-manske to nice off-white powder (collect based solids, acidify, strain, discard acidified solids, basify, repeat). The precipitate you have is almost certainly not alkaloidal in nature as in an acidic solution, your alkaloids are water soluble, thus do not precipitate. I don't think there's any need to weigh, bioassay, etc. as there's nothing there, imo...but if you happen to turn up anything interesting, please do inform us. 😉
 
I will definately do that, Snozzel. The thing is that I had already done 2 A/B, so the manske was pretty clean - especially for the volume of precipitate, from the acidified NaCl harmalas solution. I will test it's solubility.
 
If it's clear and solid, then I say try and get a little piece of it, as clean of a sample as possible, then try and melt it on tin foil. If it isn't salt it won't bubble/melt.
 
Well the acidification of the dissolved manske causes the harmaline to precipitate. It has to be dissolved and cleaned again afterwards, but it seems to be primarily primarily harmaline
 
A/B once; the color - it is almost white, and SWIM took 300mg oral. I will do another A/B and sodium bi-carbonate, to see what drops out.
 
FiorSirtheoir said:
A/B once; the color - it is almost white, and SWIM took 300mg oral. I will do another A/B and sodium bi-carbonate, to see what drops out.
Click to expand...
This certainly doesn't give any evidence as to the composition of the extract...it just shows that you have an off white powder extracted from P. harmala.
 
Sorry no access to any analysis or analog. SWIM did loose approximately 33% of the manske acid precipitate, when it went through A/B with KOH so there was and only about 68mg of oil residue in the filter.

SWIM USED distilled vinegar on the water dissolved manske salts.

Sorry if my subjective experimentation isn't sufficant evidence; all do respect do what I have and give me some real feedback, or ...open for suggestions.

Peace
 
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