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Water/Ethanol mixture crystallization

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The75thFlower

Rising Star
Merits
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Could't find any reference for this, but has anyone done work on the possibility of using a Water/Ethanol mixture such that DMT remains soluble at high temperature but precipitates at lower temperature?

I'm assuming it's solubility increases with temperature too.
 
This is an interesting option, but I am afraid ethanol and water are too polar. Not that DMT won't precipitate, but it might precipitate along with plant oils.

It also depends on solubility curve of DMT free base in that system.

You can do a small test tube experiment: dissolve DMT in small amount of ethanol, filter if needed, add water until cloudy and then put into freezer.

Chances are it will either stay in solution or crash too quickly.
 
I have experimented with this a little. Freebase DMT is extremely soluble in room temperature 90% ethanol and dilution of such a solution with 20% ethanol indicates a possibilty that an ethanol solution around the same strength as normal vodka might be a feasible solvent for recrystallisation.

There seems to be a potential problem in that even 50% ethanol dissolves DMT too readily. On chilling such a mixture to -24°C, it separates into two liquid phases with the DMT present to an overwhelming degree in the darker lower layer. The upper aqueous layer contained only negligible amounts of DMT and may be separated from the upper layer with swift use of a chilled pipette. Otherwise, not much above -18°C the two phases rapidly recombine.

When loosely covered in the freezer for several months the ethanol evaporates from the remaining lower layer to leave yellowish DMT crystals. The only vaguely practical use for this process that I can imagine is perhaps to separate DMT freebase from a water-soluble impurity.

The experiments with normal 37.5% ABV vodka remain to be done. Perhaps you'll beat me to it?
 
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