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(nearly) White crystalline DMT --> yellow Oil when converting to Fumarate ?! : (

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Brennendes Wasser

Brennendes Wasser

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Senior member Chemical engineer
Hello!

My Spice is nearly white, only slightish yellow.

I threw 1 g of this into DRY Acetone (coloured slightly yellow then)

0,310 g Fumarate into DRY Acetone

when both were dissolved, I put them together.



Yep ... instantly clouds crashing out, then I placed a fan on top of it to make it evaporate (as I have no excess Fumarate its no problem to just evap of course).

When checking it halfway done, there was already a niiiice big white Crystal in the solution, which was slightly yellow.



BUT

when I came after 1 hour and I thought it must have been done, the crystal was dissolved again in a TRULY YELLOW liquid. The liquid is not really smelling like Acetone and it is not that much, but still everything but a dry container (maybe I could post a photo).



Now ... what has happened here and did I just wreck my 1 g Spice ?

I placed it into the freezer, but nothing went solid (after 20 minutes, could have been more to test it).

I did a pull with hot Naphtha (as this should pull everything but the Salt) - no Change.

Now I placed it in a container with CaCl2, hoping the liquid is watery stuff, which can be pulled out with this. But I dont know where that water should be from - the Acetone was dried with Na2SO4 definetly!

Any Help? I dont want to be left with that yellow shit instead of that nice crystal I saw in midterm : \
 
Acetone is evaportating quite fast and this is cooling the solution and this attracts moisture from the air (condensation).
Always minimize contact of the solution with the air. Never evaporate with FASA. Just pour off once precipitated. It allows using of more fumaric acid (about 10% more).
Poured off acetone can be evaporated then to ensure there is nothing left
You can evaporate fumarates, but I am always avoiding this, because result is hard to work with, almost impossible to scrape.
 
Thanks, I'm also pretty sure that this must be water which got sucked in afterwards, well what else could it ever be ...

But in this case the CaCl2 should pull it off again, I'm just keeping my fingers crossed.

Yes there was another mention, that I should just rely on the precipitation, but I thought *Oh well I used it 1:1 so why not just evap with a fan*.


Testing this the next time with decanting to check if it's really better than. But I guess it will be :roll:
 
I am minimizing the contact with air as I said. And few hours before the procedure the air-cond is switched on max - lowers temperature and removes moisture from the air.

After pouring off let it sit 24 hours with air-flow. Scraping precipitated crystals is pleasure and super-easy. Then break them up as much as possible (by knife?) and put into oven at 80C for an hour with ocassional movement/breaking. Last traces of acetone are evaporated this way.
 
pete666 said:
Acetone is evaportating quite fast and this is cooling the solution and this attracts moisture from the air (condensation).
Always minimize contact of the solution with the air. Never evaporate with FASA. Just pour off once precipitated. It allows using of more fumaric acid (about 10% more).
Poured off acetone can be evaporated then to ensure there is nothing left
You can evaporate fumarates, but I am always avoiding this, because result is hard to work with, almost impossible to scrape.
Click to expand...
This.

There is no point to evap in open air. Just wait till all dmt fum pricips and decant the aceton.
 
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