A friend made some harmala salts, and using the information in the "Harmala Extraction and Separation Guide" tried to convert them to freebase by dissolving the salts in hot water and adding a warm solution saturated with sodium carbonate, adding slowly til the solution would not get any more cloudy. Then he let it cool in the fridge.

Anyways, he was wondering if the alks crystallize like when doing the salt extraction? It has been a few hours and its just a cloudy solution with some dark oily looking residue on the bottom.. Not sure what its supposed to look like. Does this sound right?

Thanks all for the help, I have learned so much since I started browsing these forums!

It looks different than manske crystals growing, in freebase it is powder that has to settle at the bottom, that takes time. Don't forget the water washes of the powder with each time a settling out on bottom.
Before adding the base, it is good practice to poor the acid solution trough a coffee filter to catch some particles who cannot dissolve.

Ah, forgot to mention, he did actually filter it before adding the base. What do you mean by water washes? I'm sorry, I am a bit lost on what you mean with that.. He got some powder precipitated in the bottom, although it seems like he lost a bit of yield in the process. He is filtering now and reading and re reading the tek trying to understand what is meant by washing with water. He is rather new to even basic chemistry but always up for learning a new skill.

Water washing refers to point 6 of this, to get the pH down 8:
https://wiki.dmt-nexus.m...ss_NaOH.2C_Salts.2C_Etc.

For using lye it is a must, but I actually don't know for sure how important this is when using sodium carbonate, some tecs don't mention the water washing indeed. Any input is welcome, thanks.

Ah! Thank you Jees, it seems obvious now; I guess I thought the freebase would just dissolve into the water, like with the salt form. Good to know. Still curious as to the necessity of doing this when working with sodium carbonate..?

Harmalas from vine, mostly harmine, keeps more solid in the water washes, the wash water becoming fairly transparent. Theoretical, at pH 8 then 2/3 is freebase solid.

From rue, it shows that the water washes go yellow, indicating that the harmaline goes back into the water. It shows with my tap water even more than with demin-water. The list says at pH 8 then only 1.5% harmaline will stay solid freebase.
For obtaining harmaline it seems manske is the way to get it solid, so to coffee filter it out at lower pH's.

I've never heard of making water washes salty with NaCl to push the harmalas into a crystaline form, I would like to ask the chemists if this is an valid route, for loosing less harmalas into the wash water.

And yes we both want to know if precipitating with SC really needs water-washes or not

Wide-eyed: check out this one, really relevant info about preciping and washing:
Sodium carbonate for harmala xtraction - too low ph? loss of yield?

About washing or not sodium carbonate preciped alks:
http://www.nlm.nih.gov/m.../ency/article/002486.htm

They mean large amounts pure sodium carbonate.
We filter out the washing liquid, then dry them, much cannot remain on the dryed alks I suppose.

Sodium carbonate remains will be minimum if you filter dry your harmalas after precipitating them. It is certainly not toxic to consume those amounts, even harmalas themselves are nearly a hundred times more toxic than sodium carbonate if you look at ld-50.

To minimize sodium carb in the precipitated alkaloids, mix a saturated solution of sodium carb little by little to change pH of the liquid, instead of adding directly dry sodium carbonate to the harmala liquid.

You could water wash, yes, but there's really no need. and then you'd lose a bit of harmaline specially which is more water soluble. With lye its more recommended to wash the harmalas because it is very caustic, so smaller amounts of it in the product would be more dangerous to have.

You can also use the manske salt precipitation step and keep harmalas in their salt form instead. Just use the right amount of salt and cool it slowly and you'll have nice pure long harmala hcl needles. The main impurity in this case would be salt, but if you filter dry it, impurity is minimized, and if you're swallowing it, no need to worry about ingesting trace amount of salt.

^^^ for the confirmation.

Though, wondering if traces of lye could not be encapsulated within the flakes, and hard to wash away. Probably just another stupid concern.

Sublingual, swims mansked yellow's do not taste even salty and it was grown with 20gr salt/100 ml which is actually on the salty side.

Another option if you don't wan't lye traces is to redissolve with an acid and reprecipitate with ammonia (which evaporates completely ) or sodium carbonate.