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basifyed harmalas don't disolve with phosphoric acid

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Para

Para

Rising Star
I'm following
Harmalas Extraction and Separation Guide
The Tao of Rue Extraction

I basified harmalas, decanted, siphoned out the solution, then added some distilled water and then phosphoric acid 75%.
I ended up adding a lot of phosphoric acid, several ml, as the precipitated harmalas did not dissolve.
I added water till 2L, some more phosphoric acid, my pH paper is showing pH 4-5.
The solution is in a water bath around 50-60 C.

Is something wrong to use phosphoric acid?
Any idea what's happening?
 
Very strange, I recently used phosphoric acid without problems, just tried it with a tiny sample of freebase harmine and it dissolved well in dilute H3PO4.
Maybe the solids are not the freebase but some impurity that's left or a new precipitate from the leftover liquid and the acid???

I got loads of gooy junk when I did something like you did.. I'd say, try to filter out the solids (or take some with a pipette from the liquid above the solids if youre decanting) and do some tests on the clear liquid to see if there are alkaloids in there (add a few drops to dilute lye or sodium carbonate and see if gets milky).

Anyway, don't throw anything away, the harmalas should be in there somewhere!
 
I put the 2L solution in a pot on stove to increase further its temperature, near to simmering, still for nothing.
The insolubles look very much like harmalas in basic solution,
but instead of decanting at the bottom it seems they will go towards the surface of the solution.

Is possible for the solution to be too concentrated even at 2L, so some of the harmalas phosphate couldn't dissolve? I started from 100g rue very fine powder.
Or should I let the acidic solution several hours for the reaction to complete? I thought this is a quick reaction, no tek specified that we need to wait several hours after acidifying.

I filtered them anyway, and basified again the solution, till it turned milky again, so I still have harmalas here :)

I'll let them decant over night again, will continue tomorrow.
I'm curios if at the second acidification with phosphoric acid I'll have the same issue.
 
Fingers crossed! :thumb_up:

My bet is you got rid of loads of junk that's now stuck in the filter, that's promising.

So, what's the next step? Filtering out the freebase?
I'm now using kitchen paper for filtering, it's fast and the filtrate very clear. Much better than coffe filters.

And are you planning a Manske?
 
I was planning to use it in the first boiling stage instead of vinegar because it's completely non-volatile; acetic acid escapes and stinks. I thought it was a proven method to use phosphoric acid for purposes like this..? I know it can form H2PO4-, HPO4-- and PO4--- ions/salts but is this a problem for a kitchen tek? Correct me if I'm wrong.

As for the second stage in the Tao tek (redissolving decanted freebase in acid to perform a Manske) HCl may be best, why not introduce some extra Cl- ions to help the salt...
 
benzyme said:
phosphoric acid is a polyprotic acid, is has multiple pKa's. you're making things complicated for yourself by using it.
Click to expand...

what will complicate?
the conversion of harmalas freebase to salts (in this case phosphates) ?
can you please detail why the use of phosphoric acid is not adequate?

will manske work with harmalas phosphates?

harmalas teks from wiki recommended vinegar/acetic acid which is also polyprotic, I thought phosphoric will be ok too.


tryptographer said:
I'm now using kitchen paper for filtering, it's fast and the filtrate very clear. Much better than coffe filters.
Click to expand...

I filtered with coffee filters after reducing, when preparing the solution, I tried them again with the harmalas dissolved in phosphoric acid, nothing was caught on them. So I needed to use lab paper on vacuum to catch more the very tiny insoluble particles, filter paper turned black in this case.


The decant is over, all harmalas are at the bottom, now I will siphon out the solution.
I will dilute the harmalas with some distilled water and phosphate them again to dissolve in the water. Then filter with some lab filter paper in vacuum.

I then plan on salting the solution (10g/100mL).
Hope no new mysteries will appear.
 
Para said:
harmalas teks from wiki recommended vinegar/acetic acid which is also polyprotic
Click to expand...

no it is not, whoever wrote that is incorrect.

acetic acid only has one pKa, phosphoric acid has three; thus with the latter, you will see four species of phosphoric ions in solution, depending on the concentrations. it can form monophosphate and diphosphate salts
 
sorry, I was the one that somehow mistakenly thought that acetic is polyprotic :(
damn, I need to buy some acetic acid glacial for next extraction.

Will be any issues with diphospates salts, their solubility or during manske?
I think monophosphate will be behave similar to acetates, so will be ok.
 
Para, you already started, there's no going back, so just go for it.

Next time you can use vinegar to compare, or even do a side by side. Im not sure if anybody ever tried. Sure with phosphoric, things can be more 'complicated' theoretically, but this doesn't necessarily mean in practice it will be bad for you. Maybe for all practical purposes you have good clean equivalent yield.

Let us know how it goes.
 
yes, I had a pH 4-5


so, after decanted the basified harmalas and siphon out the top solution it remained around 300mL or harmalas plus a little solution.

From this I took 50mL with a turkey baster, acidified with phosphoric acid till ~pH 4. Not all harmalas dissolved even after 5 minute of stirring so I had to dilute the solution with 150ml water for all harmalas to dissolve.

On the rest of basified harmalas solution, 250mL, I added vinegar 9% till total solution reached 600mL. All harmalas dissolved very quickly. Super !!

I filtered them both, put in a water bath around 50C, and added salt 10g/100ML. It seems they weren't sufficient hot as harmalas salt started to precipitate.
I left them to cool to room temperature then put them in fridge.
 
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