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Harmalas Extraction and Separation Guide

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You can, but.. If you start with salt precipitation, it can be hard to filter (sometimes it doesnt settle nicely to decant), so doing a first base precipitation will make the first filtering a bit easier, and once you do the salt precipitation it will be cleaner to filter. I used to go straight for the salt, because I had my filtering tricks (vacuum, being patient, more than one filter/funnel at once, moving the bottom sediments once in a while, keeping a large liquid volume on top of filter to speed filtering due to gravity, etc), but a few people like gibran have brought to the attention that doing a first base precip helps, specialy if its lye, so I added to the wiki. Feel free to do as you please :)
 
reviving this thread unintentionally, but I HAD to thank endlessness and all that contributed for satisfying my craving of spiritual adventures through nature once again :)

Love the nexus and all the nexians!

omega
 
I can't seem to separate the harmine from the harmaline. I want pure(ish) harmaline to make THH. I have extracted lots of harmalas, but when I dissolve them and bring up pH to 8,75 almost everything precipitates. I thought maybe this batch of rue had almost no harmaline, but I tried a new batch from another supplier and still the same problem. I bought and calibrated another pH-meter (100+ euro), still the same problem.. I use NaOH to base, but was careful last time to not overshoot and then correct the pH, and stirred vigorously during the basing.

Anyone any idea what might be wrong? Anyone encountered the same problem?
 
I`d guess both your batches of seed have mostly harmine, then...

You can check out the colorimetric link in my signature and find some reagent that shows different results for harmine and harmaline, which could help you assay them. I don`t remember off the top of my head but maybe they have different color glow with UV light when dissolved in acidic solution, do a little search maybe you can find out.

That would def be interesting for the sake of experimentation but I really do think you have mostly harmine there.

Good luck either way, and let us know what you do and the results :)
 
Luuk said:
when I dissolve them and bring up pH to 8,75 almost everything precipitates.
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this means nothing precipitates from the filtrate of that after being left overnight with...Na/K carbonate or ammonia? (no need to use a meter with those, pH is perfect for harmaline)...maybe there's an extra load of crap in the seeds instead preventing precipitation for some reason...imho bad results should be compared to the outcome of a go with an 1860's tek...

endlessness said:
I`d guess both your batches of seed have mostly harmine, then...
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this is interesting. is there science saying that some seeds with husks have harmine but no harmaline? sorry nothing jumped out from the 554 harmalas thread titles...
 
After dissolving approximately 5g of base into vinegar water and salting, I'm left with about 1g product. Can I do some more heat/salting on the filtered solution and cool/filter more.. I'm worried if I repeat 10-13 I'll eventually end up with nothing
 
Yes, very likely you didnt add enough salt or wait for it to cool enough. You can warm the whole thing up again and add more salt, waiting for cool down again.

If you still dont get more out, you can always add a base again, get whatever precipitates and go from there again
 
EDIT: I had left it in the fridge overnight, and no more salt was dissolving (i think).

Salted it again but just salt precipitated. Tipped solution down the drain (as I'm not going to be using it anyway, just testing the process)


Possibly you use the freeze/thaw technique to separate the base product rather than using filters?
 
Harmaline solubility in ethanol approximately .5mg/ml

Now if only there was a way to extract the tannins from rue seeds first, possibly a long soak in room temp/cold IPA?

Harmine solubility in ethanol approximately 1.5mg/ml
 

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[ removed previous question as CatPharm kindly answered it in PM ]

One thing is still unclear to me - the tek (and CatPharm) advises that I use strictly non-iodized salt. The salt I got is fine table salt with a Potassium Iodide content of 28 to 55 mg/kg. Would that be appropriate for the Manske stage of this tek, or should I look for salt with no Potassium Iodide in it?

Thanks!
 
Nydex said:
[ removed previous question as CatPharm kindly answered it in PM ]

One thing is still unclear to me - the tek (and CatPharm) advises that I use strictly non-iodized salt. The salt I got is fine table salt with a Potassium Iodide content of 28 to 55 mg/kg. Would that be appropriate for the Manske stage of this tek, or should I look for salt with no Potassium Iodide in it?

Thanks!
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I've always just used standard table salt that we get here in the states, it's called Mortons Salt. It's iodized and I've never had a problem.
 
Thanks for clarifying the salt question, paulsage! I have one more noob question... I ended up in a precarious spot at step 12. After dissolving back the now solidified harmalas in water and vinegar, I set up four jars with a double coffee filter and poured in the mixture in the filters so they could filter throughout the night. Approximately 14 hours later you can see the stage of filtration in the below pics... They're barely moving. Also what worries me the most is that the harmalas are dissolved in the water and vinegar mixture, which has now completely soaked the total of 8 paper filters I'm using. How do I get them out of the paper and basically not throw away in the trash paper soaked with a lot of harmalas?

Any advice is very much appreciated, I'm such a newbie here... :cry:
 

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Nothing is lost. You can set aside the filtered tea and then combine the unfiltered portions in one container, then squeeze the liquid off the filters, wash the filters with fresh water several times and add all this rinsing water to the unfiltered liquid container.

Then you can basify harmalas in the unfiltered portion, filter, dissolve in minimal amount of hot vinegar and leave the solid particles to settle (overnight). Decant, top up with fresh water and repeat the process say two times. The last time it should filter fine.

From there it should be easier. Filtering off the fine particles and sludge is the hard part.
 
blue.magic said:
Nothing is lost. You can set aside the filtered tea and then combine the unfiltered portions in one container, then squeeze the liquid off the filters, wash the filters with fresh water several times and add all this rinsing water to the unfiltered liquid container.

Then you can basify harmalas in the unfiltered portion, filter, dissolve in minimal amount of hot vinegar and leave the solid particles to settle (overnight). Decant, top up with fresh water and repeat the process say two times. The last time it should filter fine.

From there it should be easier. Filtering off the fine particles and sludge is the hard part.
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Thanks for replying man! So basically when I basify the unfiltered portion the harmalas will bind to the base and form solids, which then I will capture in the coffee filter.

After that I dissolve in water and vinegar and I leave the particles to settle, but what settles are impurities? And if yes - will the liquid I decant contain harmalas?

If yes - do I put that liquid with the other already filtered liquid that I've set aside, or do I combine the decanted liquid form the unfiltered portions in one place and then filter once more, and after it's filtered combine with the filtered harmala portion?

Sorry for making you reiterate but it's somewhat confusing to me :cry:
 
After that I dissolve in water and vinegar and I leave the particles to settle, but what settles are impurities? And if yes - will the liquid I decant contain harmalas?
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Yes, in general terms :
- In acidic, discard solid, keep liquid
- In basic, keep solids, discard liquid

If yes - do I put that liquid with the other already filtered liquid that I've set aside, or do I combine the decanted liquid form the unfiltered portions in one place and then filter once more, and after it's filtered combine with the filtered harmala portion?
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I think there is no rule, it's all depending on how you want to process your extraction.
For my part, i like to put aside all rinse solution and filter, then when my "main" process is finished, i process all rinse solution + filter + another cook on seeds then extract if once more.


This last extraction is a bit dirty as i process all waste and sludge from previous step.
In the pic you can see different rinse solutions, boil 5 & 6 on the seeds, filters cooked. All have been based with NaOH to recover theses precipitate. It contains sludge + harmalas, and then is processed as an usual extraction.
All theses freebase have been decanted and redissolved in dilute vinegar, reduced, then filtered, then based with NaOH, decanting to be ready for mnske step. It represent in my beaker a volume of ~ 100mL of alks.
 
Thanks a lot pastranostra! So basically by now I've filtered all the harmala tea through a coffee filter twice and it looks pretty clean. Now in the tek follows the manske step.

Since time is of great importance here, can I just get the crystallized harmalas that will form on the bottom of my glass jar and dry them up and use them as they are, or do I absolutely have to repeat the basify-filter-redissolve-filter-manske cycle at least three times?

Would only one iteration of this cycle yield a perfectly consumable crystallized harmine+harmaline HCl, or will it contain dangerous chemicals that make it unsuitable for changa?

Thanks!
 
When you have you precipitate in your saline-acidic solution (harmalas hcl), you should pour off the acidic solution and let it in a jar.
Dissolve your dry harmalas hcl in warm water (no acid needed as it's a salt), then do manske.

Doing manske will help purifying your harmalas. Some lye, salt and other can be present after your 1st manske, so it should be better purifying more by doing manske multiple times (i usually do it between 4 & 8 times). Manske after manske, you should see your harmalas needles being longer and longer, brighter and brigther

https://imgur.com/a/P72E8Ap

Advantages of manske is the use of only water and salt, it's worth the effort as chemicals used are very safe :)
If you can, try to keep all your manske solutionn then base it at the end. You should have a bit more alks that precip.
 
Wow those are some beautiful crystals you got there! How much seeds did you use to get that much? I used around 140 grams of seeds and now after I left the mixture after the manske step in the fridge for 6 hours pretty much no crystals had formed. Then I filtered the liquid through some coffee filters and I can see that I actually have some crystals, but doesn't look like much more than a few hundred milligrams. Yours looks like a lot of grams. Would redissolving my crystals in water and doing manske again increase the amount of crystal that precipitates? Or is it purely of a purification purpose?
 
der-seemann said:
does anyone know the solubility of hamala (harmin, Harmaline and THH) HCl's in plain cold water?
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I crudely measured a harmine/harmaline HCl mix from rue to be ~0.1M (~2.5g per 100ml) in 4C water. Not a precise lab measurement at all though, I was just trying to understand manske better and in particular how important the initial Harmala concentration is before adding NaCl.

Details here
 
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