Ok, complete success. Here's what was done:
Initially, no precipitate was seen, although it may have been too dilute to see.
Those crystals that formed I mentioned above were most definitely dmt.fumarate. Anyway, the entirety of the acetone (initially containing 500mg of dmt freebase and 500mg of fumaric acid) was allowed to evaporate.
There was an obvious mixture of components after evap. They were scraped up and found to be noticably wet (even though 50mL of the acetone does evaporate to dryness and there was no scent of acetone remaining).
The crystals were placed in a jar, covered with 100mL of fresh acetone and agitated in attempt to remove any excess fumaric acid. The solution was let to sit for an hour which allowed all the precipitate to fall to the bottom. The acetone was poured off being careful not to let any of the precipitate come out. The precipitate was allowed to 'dry' (evaporate the rest of the acetone until no scent remains). This took about half an hour. The powder was scraped and found to be completely dry, weighing in at 648mg !!!! That's bullshit accuracy if you ask me, but I'm not complaining. The powder is visibly a single component, water soluble, and extremely tangy on taste.
Ronue.. dude
Fyi,
By calculation, the amount of fumaric acid needed is 0.31 x the amount of dmt freebase used. For good measure, a 0.4 is used:
Future (and in progress) experiment:
-Dissolve 500mg of dmt freebase in 10mL of acetone (2mL/100mg)
-Dissolve 200mg of fumaric acid in 50mL of acetone (25mL/100mg)
-Add the the fumaric acid soln slowly(ish) to the dmt soln
for curiousity, pH was measured and found to be just slightly acidic - good!
after combining the two solution, a single solution which looked like milk was formed (dmt.fumarate precipitated). Within 15 minutes it can be seen that glass shard type crystals are forming. The jar is allowed to sit (covered) overnight to afford the crystallistaion ample time to complete.
-once crystallisation is complete, the acetone is poured off and the crystals are allowed to dry
-once no scent of acetone remains, the crystals are scraped up, powdered and added to 25mL of fresh acetone. Stirred well, allowed to settle for an hour or so, and then the acetone poured off, the crystals dried, scraped up and weighed. They should weight approx 1.3 times the weight of the dmt freebase used