Concerned about fumarate precipitation

[hydrocarbon]

An individual has 300mL of FASW that he used to pull DMT fumarate from one pull of limonene (yes, I know this is a lot of FASW, but the nexus went down for maintenance in the middle of the extraction and said individual got impatient). FASW is now evapping in front of a fan and a visible whitish precipitate has been observed falling out of solution. Is this excess fumaric acid or DMT fumarate?

I am confused regarding the chemistry behind using FASW, apparently. Does this work similar to the sodium chloride precipitation of harmala alkaloids where the harmine/harmaline falls out of solution? Or does the fumaric acid begin to precipitate as the volume of water can no longer hold it?

If the latter is the case, then should all this excess fumaric acid not be filtered out before completely evapping to leave DMT fumarate? Obviously there would be a lot of excess fumaric acid present in the dry product if it were not filtered out; guess I just answered my own question but can someone clarify for me?

The BLAB tek seems to describe simply evapping all the fumarate pulls without bothering to filter; seems easier to filter first and skip washing with IPA...

 

[hydrocarbon]

Also, individual plans on converting DMT fumarate to freebase. Is drying the DMT fumarate first really necessary? Would there be any reason not to simply reduce down to a workable amount then freebase the solution with saturated NaCO3 solution? Would this result in fumaric acid being precipitated along with the freebase?

 

[endlessness]

I would guess thats excess fumaric acid but its hard to say for sure... DMT fumarate is VERY soluble in water, so when you evap, it doesnt really crash out, it only really forms this harder wax in the last moments. You could filter out these white precipitates and keep them just in case (try redissolving in a bit of warm water, if its dmt fumarate it will dissolve easily, if its fumaric acid it wont. Also you can taste a tiny bit and compare with pure fumaric acid..

As for transforming it to sodium carb, it works perfectly with reasonably clean dmt fumarates, but im not sure how well it works with crude FASW. You could try it out with part of your product (dont do it with all at once), and see what happens... In the worse case scenario, it wont precipitate and you can just pull with limonene and salt it out again, repeating the process. And if it works good and you just want freebase and not fumarates, you can do this with all the rest. And no, fumaric acid wont precipitate with freebase, because fumaric acid + sodium carbonate = sodium fumarate, which is very water soluble so it would stay in solution while dmt freebase precipitates.

In the case that it doesnt work and when you evap the rest of the FASW its indeed very impure, you can re-a/b it or do the clean up process described here: Cleaning up dirty fumarates - FASA/FASI/FASW - Welcome to the DMT-Nexus .

By the way even though you used a lot of FASW, I suggest doing another (smaller) FASW salting on the limonene, to catch any possible remaining alkaloids

 

[hydrocarbon]

Thanks to you, endlessness, for your help again on this process! I had not thought of testing solubility on the filtrate, good to know.

I am thinking that if solution is reduced down to say, 25mL or so, then filtered, the max amount of fumaric acid left in solution would be ~150mg based on fumaric acid's solubility of ~630mg in water. Even so, individual will follow your recommendation and try sodium carbonate precipitation on a small amount of solution first in case it ends up being a waste of time.