If it's any consolation, the goo
can turn to crystals, especially if you store it in a desiccating chamber of some sort. Unfortunately, even then it's not as lovely as precipitated sparkles. Something you might want to try is
recrystallising DMT fumarate from boiling IPA.
Besides moisture, having taken a look at the method you outlined, Levanah, the fact that it says to evaporate all the solvent is kind of a red flag as far as purity goes. The point of FASA precipitation is that the DMT fumarate is insoluble. The fumarate crystals settle out of the mixture and can be recovered by decanting or filtration.
When you evaporate all the solvent two or three things will occur. Firstly, any soluble impurities will be deposited on the fumarate crystals instead of being washed away like if you had removed the crystals from the solution. And then it comes back to moisture: the residual water will become concentrated and eventually soak into the fumarate - and IPA is fairly hygroscopic so it's pulling water out of the atmosphere as well.
One other factor to consider is the differing solubility of fumaric acid in various solvents. There's
the FASIPA Method, but that goes nowhere near quantifying the solubility of fumaric acid in IPA.
Benzyme estimates it as being "difficult" - again, no quantification.
This post by Luz brings us a little closer to some numbers: "As I understand it, the solubility of fumarate in acetone, in water, and in IPA are all very similiar, between .6 and .7 gr per 100 ml". Then here,
some one has made a nice generic explanation of the FASX process and mentions, "The solubility of FA in Acetone and water is 6mg/ml and in IPA 5mg/ml" - but I'd say that IPA figure is on the low side.
While going through the search results,
this also came up in a post by Luuk: "A good method for purifying is to dissolve freebase in IPA, add straight fumaric acid (no FASI!), and stir good. This causes an instant precipitation of small but pure DMT fumarate crystals. The DMT fumarate formed is contaminated with fumaric acid but this can easily be removed by dissolving the DMT fumarate in water." So, no need to worry about the precise figures after all, perhaps. Except
Endlessness provided a link to some definitive data here. It turns out that the solubility in various solvents increases in the order: water, acetone, n-propanol, ethanol, IPA.
Dang et al. wrote:Propan-2-ol
T/K x1·10³ 100(x1 - x1calcd)/x1
279.00 10.92 -11.1
285.00 13.78 -3.90
291.00 16.85 0.30
297.00 20.23 3.05
303.00 23.59 3.42
309.00 27.25 3.38
315.00 30.97 2.17
321.00 34.92 0.56
327.00 39.10 -1.33
333.00 43.48 -3.58
342.00 53.79 -0.81
351.00 65.62 1.27
Temperature in K in the left column, solubility is presented as a mole fraction in the middle column. Converting mole fraction solubility into more everyday kind of units requires a bit of basic arithmetic and the MW of fumaric acid and IPA, plus the molar density of IPA. I'll leave that one as a challenge.
Just remember, it's not really recrystallisation in the strict chemical sense if you evaporate all the solvent.
“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli