i got fumaric acid, did FASA and FASI, and then tried to reX, then freebased, then hexane extracted, at no point even as a fumarate, was i EVER able to obtain a solid. it maintained its goo status the entire time. now however i have an absolutely perfect crystal clear orange oil that drips down the evaporating dish when left at an angle, much like how tar seems to flow like molten glass over a span of centuries.
So, it worked, but, it didnt fix the issue of the extract not bloody forming a solid.
Something interesting did occur though, i accidentally distilled/smoked over DMT out of the raw first NPS extract as i was concentrating it and distilling over like 250ml of toluene. it was so clean though i didnt notice when it turned thick and all the toluene was gone, so then it just kinda started cooking and vaporizing against the glass, but it barely just turned yellow. afterwards i added toluene back and distilled more to rinse the DMT out of the condenser, and later i added FASA to the receiver, and got perfect results. about 40mg of high purity as-described DMT fumarate, formed the right crystals behaved the right way, i have yet to freebase it to see if it crystalizes properly. Just thought id note this. It makes me wonder, what if i tried vacuum distilling raw base instead. at very least it might let me get away from whatever is preventing solid fumarate from forming.
edit- after going back and re-reading the OP which for some reason i havent done at all since trying my own process, i realize something, possibly a method of purifying spice and even seperating them to some degree. My method with IPA was on the mark, although it suffers from a lack of water, and i realized, the OP method here, does just that, they do minimize nasties at first by crashing out undesired gunk. my soup at any given time is like a smoothy its that thick with tannins and such, i just reprocessed the soup before disposing and got more of a yield, and this was after already re-trying yet another time (i think the DMT sticks to tannins and precipitates slowly how readily it touches solvent and migrates, leaving it behind even though theres no bark anymore, thick soup might just be that naughty).
Next though, they do not shake the heated naptha hard on their thinned soup, they dont say why but i bet its just because it has previously formed awful emulsions and they wanted to avoid that. this results in a very gradual dissolution of dmt into the solvent, and this is the key: substances will dissolve slowly, in order, at the interface they might even form supersaturated pockets and crash back out, who knows, molecular physics is chaotic, but, the most soluble things will migrate first and the least soluble things, last.
Having accidentally distilled some of the DMT, entrained in toluene, but distilled nontheless, i note that, the pure crystaline product i got was pure white also while the rest was yellow. so whatever it is causing the coloring is, in some manners or another, heavier.
Because of the controlled manner in which spice dissolved into the solvent, it fractionates, though i think theres probably another word for this since its basically the opposite, its fractional leeching?
anyway, as the dissolution is slow and controlled, and there isnt any extreme forces at play like shaking which can practically FORCE things into solution with mechanical force rather than osmotic/ionic ones, pure DMT is obtained, and its seemingly seperated from whatever it is that encourages the formation of oily polymorphs over crystals. incidentally resins which precipitate out readily even at RT i found, a little, given time, do not enter the solvent at all. shaking can force them in, as can aggressively dissolving into hot solvent which still is nowhere near saturated.
less pure DMT is obtained in subsequent fractions, but this still lacks a critical polymer/polymorphing component, allowing the spice oils to co-crystalize with the dmt, or at least, i assume, form waxes or oils adsorbed/dispersed throughout crystal structures.
The other day i wanted to quickly dissolve my freebase in hexane so i could see if it had been sufficiently purified after being a fumarate salt, i added enough hexane to the evaporating dish i had used, but found it really didnt want to dissolve. it eventually did though with the aid of some stirring and gently heaving the point where the oil was collected, the boiling aggitating it, and etc, but, it really really resisted. under these conditions, it did not want to precipitate, not even close, and it wasnt fogging until the volume was subsequently reduced. but really think about that, i had to force it to dissolve, but then once it was, it would not come out nearly so easily. i know for fact having tried freezing more concentrated, vastly dirtier actual goo, that it would not precipitate out undesirables under the same conditions it was kicking and screaming as i tried to dissolve it.
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So what im getting at if you cant make it through my ramblings is that since spice goo/oil behaves very differently dissolving vs precipitating, perhaps we can exploit this somehow, which is how the thread OP process works too.
I think i at least proved in a simple way, that if you rinse goo with IPA, based on how long it spends in contact, you get totally different compositions oover time while the goo/gum/resin does not dissolve at all until its literally all that is left.
After thinning the base-soup eliminating the floating solids that might radically slow spice mechanically, from reaching the solvent, and just being very gentle, and letting things happen naturally, in chemisties on natural order, pure products were also obtained, much moreso than mine, and i think the difference is the water adds an additional kind of threshhold, adding even more controlled order, maybe reducing what i had, as 5% contaminants making it through, down to 0.1% enough that it finally crystalizes and drove everything to keep on seperating apart as solids and liquids.
So perhaps there is a process we can employ, opposite to fractional crystalization, where we can leech specific portions of available products, at more selective, desirable rates, utilizing the natural ordering of things when left to their own devices, and getting cleaner products based on how the affinity drops off a cliff as a solution becomes saturated. The reason we havent previously seen this is that through shaking, actual water-pressure causes molecules to reach escape velocity, in a manner of speaking, at complete random. very quickly you get 99% of everything in solutionm but then the rules change when its time to do the process in reverse, because a mystery-compound prevents the DMT from assuming a solid form, period, which we rely on to finish seperation during crystalization.
