How to Wash Harmala Alkaloids ?

[josboaz]

Hello,


I create this post in this subsection of the forum, as I'm qualified as a beginner although I joined back in 2018.


In this thread They write about washing the Harmala alkaloids, I'm curious how to go about this? Just pouring the solvent over it? or re-doing the cycle steps?

 

[merkin]

I'd say the pertinent part is this:

Add more water to the FB and repeat settling and decantation till clear water is all you get. We are washing the solids and discarding the liquids.

Note that he's using caapi here not rue.

Acidifying and basing alternatively is another method of cleaning. Just with this you would decant and filter the acidified liquid and discard the solids. Then you would basify till precipitation is done and filter again, this time keeping the solids, and so on...slowly the liquids will clarify and the solids get cleaner and cleaner. Of course you will lose a bit of product every time so how many times you do this depends on your goals here.

 

[DMT Lexus]

Just add some pure destilled or RO water and let the alkaloids sit.
When it's on the bottom, get the water layer off and add pure water again.
Usually 3-4 times to do it is enough. When the pH is about 8 it's time to stop, let it sit, get water out and strain the alkaloids on a coffee filter, than dry it.

 

[Jees]

If it's harmalas from caapi, the wash water will be clearer than harmalas from syrian rue.
With rue, due to the harmaline content (which is near non existent in caapi) the wash water will start to dissolve harmaline and colour it yellow-ish.

To keep all harmaline freebase, you can add a knife tip of sodium carbonate in your wash water, the pH will be like 9 and the harmaline will not dissolve in your wash water anymore.

In the "VDS papers" he proposed to wash with:

...wash residue with ammonia 3% or Na2CO3 solution 0,5%...

I wash in a big pot with like 5 liters of wash water, just one wash.
I've my freebase filtered out in a coffee filter, add this sludge in the wash water volume, swirl, let settle, swirl, let settle, poor of the clear water and strain the particles trough a coffee filter to catch.

You can however finalize with poring one some plain water over the freebase in the coffee filter, but overkill I suppose. And I've come to the thought that this tiny remainder of dried sodium carbonate trace on the freebase surface keeps it from oxidizing to orange. If I wash with diluted ammonia then I've got the impression orange-oxidizing of the freebase happens way sooner.