Started with acacia of unknown species but most certainly DMT bearing. About 2kg of bark was finely divided, and qpprox 500g was added to a large saucepan. To this was added 3L of tapwater that had been made to a pH of about 2-3 by the addition of concentrated HCl.. The bark was simmered for about an hour and a half, and the aqueous solution drained off. Additional acidified water was added, simmered, and then drained, and then once more, to give three acid washes. these were gently simmered in seperate pots until reduced to about 1/3 in volume, and combined in a glass jar. an equal volume mineral turpentine was added and agitated for the purposes of defatting.
A thick, sticky froth formed which I initially took to be an eumsion but soon realised it was what appeared to be a conglomerate suspension of waxes or resins in a coherent jelly-like layer floating on top of the aqueous phase (resembling many tiny droplets of stuff in a fluid layer of turps). This made seperation difficult, necessetating the use of a seperatory funnel as the gunk was clogging my burette and made decanting an absolute nightmare. So, 6 hours later (the only sep funnel available at the time was a tiny 100mL ^^), I had finally seperated all the gunk from my aqeuous layer. I added a second volume of turpentine to the aqueous phase and again, a layer of gunk developed but noticeably less then the last time. having refined my technique a little, seperation was much quicker this time but still frustrating.
With approximately 2.5L of acidic aqueous solution now remaining, I added first 1L of a solution tap water/NaOH at pH 12-13 slowly with stirring, and got a total pH reading of ~11, another litre took the overall solution to approximately pH 13. 300mL Shellite was added and agitated gently, then drained into a glass vessel. A second shellite wash was added to the same vessel, which was then transferred to the freezer.
8 hours later, the shellite was very cloudy white, I took this either to be a) very fine precipitation of freebase spice xtals, b) some quirk of shellite wherin trapped water freezes at low temperatures to give it a c loudy appearence.
Allowing the vessel to stand for ~30min, the cloudiness mostly resolved and I could see small radial clusters of white xtals forming on the bottom surface. I could barely contain my excitement. I returned the vesel to the freezer for 2 hours, then filtered the liquid through a fine coffee filter slowly. At which point, nothing appeared. Nothing was found clinging to the freezing vessel either. had time permitted, I would have air-evapped the shellite to see if it was merely a poor freeze precip.
I suspected one or more of the following occurred -
1. Too acidic/too hot, broke down some or all tryptamines during the aqueous wash
2. Mineral turpentine did something wiggedy-wack during defat and all my alkaloids went with the gunk
3. Too alkaline, broke down some or all of the tryptamines (or pH spikes during addition)
4. Too much shellite, wouldn't freeze precip
Unfortunately due to circumstances I wasn't able to hang onto the gunk, or the shellite for further analysis, and it had to be tossed, with I have prepared another 750g of bark and am currently reducing the 3 acid washes (which I performed at 3-4pH this time) in volume on very, very gently heat, no agitation visible just steaming quietly.