Hi

Quick background - to extract crude Harmaloid freebase I followed this tek.

It was brown, powdery & having used it in a Changa blend, worked quite nicely.

I wanted to clean it up a little, so I followed the second part of this tek.

So,I
Mixed 50ml white wine vinegar & 150ml water & dumped the crude extract in it.
Mixed 100ml water with sodium carbonate until saturated
Mixed the solutions together.
Colour changed rapidly, as expected.

Now the confusion.

The tek says "put jar in fridge, wait a couple of hours until the yellow powder falls to the bottom"

The powder that fell to the bottom is still brown. The liquid is yellow. Have I done something wrong, or can I filter the liquid out & use the powder?

Hi

For 1g Harmine HCL, to convert to freebase, I know I need to dissolve it in water, add sodium carbonate, wait for precipitation, filter.

However, my first attempt resulted in using way to much water, too much sodium carbonate, and ending up with a messy kitchen.

So the question is, for 1h Harmine HCL:
What is the minimum amount of water the Harmine HCL will fully dissolve in.
What is the minimum amount of water & sodium carbonate (base solution) I need to pour into the saturated Harmine solution to precipitate all the alkaloids?

Thanks

Yes your alkaloids will be with the brown. I`d add a bit more sodium carb solution to it to see if the solution changes color some more. If not, decant/filter to get them. Personally I`d do a slow manske precipitation followed by yet another base precipitation.

To do the manske, redissolving the freebase alkaloids in vinegar water, bring it to boil and add 100-120g of salt per l of water, put it in a container and let it cool down as slowly as possible (for example submerging the container in warm water). Such slow crystallizations tend to result in cleaner crystals than quick ones, and then alternating with another base precipitation should result in something significantly cleaner than what you have now. You can repeat these 2 processes as much as your OCD tendencies require

But in any case, even as-is it should be just fine to consume, just maybe you need to adjust dosage to account for the higher percentage of impurity (hard to calculate but as a guess you might need 10-40% more brown stuff than light tan/white alkaloids)

Regarding the amount of water to dissolve harmala hcl, you`ll need very little you can just add it very slowly, drop by drop, till you see it all dissolved. Nevertheless having some more water might be a good idea since some impurities will stay dissolved in the water after you add the base. As for the sodium carbonate amounts, just add it slowly till you stop seeing color change, wait a bit and add a bit more, if no more color change is observed you are fine.

Thanks for your reply, but - still confused.

If the alkaloids are in the brown sludge - then how will adding carb / filtering do anything? They'll still be with the brown, no? Or will repeated carb washes leech the brown from the sludge into the water?

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Will the manske turn the freebase back into a HCL (by adding the vinegar)? Does this step pull the alkaloids out of the sludge and dissolve them in the water?

If this is the case (that the alkaloids are now in the solution) - can you filter the solution at this point to remove all the 'brown', then add the salt to the solution again to turn the HCL back into a freebase? (actually just realised I've possibly conflated 'adding salt' and 'base precipitation' (which I assume to be sodium carbonate) into one... are they one, or do these steps have different uses?

Please let me know if I'm misunderstanding these steps!

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Thanks for the info on water to harmala ratios. How much freebase should I get from 1g HCL? (this is a separate extraction to the above (where I had 3g rue extract) - with this one, I had 1g 99.7% Harmine HCL) I think I've ended up with about .3g, which is terrible. It seems I have gifted the rest to various kitchen utensils due to the ridiculous amount of water I ended up using.

Did you filter the solution after you dissolved the crude extract in water+vinegar and before to mix it with the sodium carbonate solution ?

My suggestion to add more sodium carb now is not to clean it up, but rather to make sure the pH is high enough and that all harmalas have precipitated. The filtering is just so you can retrieve the alkaloids from the liquid and then discard the liquid.
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Almost. Actually adding vinegar will turn them into acetates, which will make them dissolve in the vinegar solution. Then you can filter throw funnel and cotton plug to remove some of the impurities that do not dissolve, which will NOT be alkaloids. Then when you add the salt, the acetates will turn into HCl and precipitate since HCl harmalas are not soluble in salty water.



Yes. Except that when I say `add 100g salt per liter of boiling harmala vinegar solution`, I actually mean table salt, NaCl, NOT sodium carbonate. Sodium carbonate is used in another step, when you precipitate the freebase. Check the Harmala Extraction and Separation Guide for more info. Fe

From 1g harmine HCl you should get theoretically 853mg harmine freebase buta bit of loss in the whole process is normal. 0.3g though is too little, either it was very impure in the first place or you made some serious flaw in your method. If you didn`t add enough sodium carbonate to precipitate all your alkaloids, then some are still in solution (unless you threw away the solution, in which case it`s already lost).

I wonder from where the 99.7% number came from. I`m skeptical until I see some quantification analysis to back up.. In case it was more impure than stated, you might get even less harmine freebase at the end. In any case, I suggest next time you do the whole extraction yourself, since you`re already doing all of this work which is basically the same as extracting except you first have to boil the rue seeds to get the harmala solution.

Good luck!

Harmala salts (both HCL and acetic anyway) are very water soluble. 1 gram will dissolve in less than 10 ml of water, faster if the water is hot.


It might force out more alkaloids from the solution. The higher the pH gets, the less soluble the freebase is. Adding ionic molecules to the solution will also decrease the freebase's solubility. It will not "unbrown" the already precipitated alkaloids.


The Manske procedure will first dissolve the harmala freebase in acetic acid (it is then no longer a freebase), then precipitate it as a solid HCl salt through ion exchange with dissolved NaCl.


"Basing" and "salting out" are not the same procedure.

You can remove some of the brown by repeated filtering of the dissolved ionic form of the harmala alkaloids, or by repeated washing (shaking with clean alkaline water) of the freebase harmala alkaloids. You will likely not get a white powder ever, certainly not when starting out with 1 gram of crude harmalas. Even harmala HCl salts that are pure needles and look bright yellow will be off-white or tan when freebased.


The amount of water does look a bit excessive. The HCl salt is usually a monohydrate, so it is the weight of 1 part harmala freebase + 1 part HCl + 1 part H20. -> 214.3 + 36.5 + 18.0 = 268.8. When you divide the two, you end up with a ratio of about 80%. So 1 gram HCl salt should theoretically yield 0.8 gram freebase. In practice you will get less due to mechanical losses (stuff sticking to the filter, the jar, the spoon etc.) and due to the fact that the freebase is still a bit soluble in alkaline water. Using less water will save more product, but will also save more impurities.

(After typing all of this, I see endlessness already answered. He uses a different calculation for the ratio, though. Maybe this can be cleared up.)

The 98.7% figure came from this link on ebay

Thanks for all your help so far... another question When the HCL is dissolved in water - the water should be clear, right?

When not concentrated, yellow and clear.

When concentrated, dark red. The color saturation is so intense that it seems almost opaque.

Hmm...

Yellow or red huh?

When I added water, it went immediately to cloudy white.

I wonder if I've been sold a dud.... (I know the ideal thing to do is to extract your own, but boiling those seeds smells so, so bad... the advantage of buying ready made & thus not having an irate other half is considerable).

I've ordered more, so I'll post some pics this time.