The exact nature of the substance in front of you is a subject of
current debate. I really wish we could run a bit of that through an LC/MS, an IR spec, and an NMR spec, to try and get a really good idea of what's going on there. Could shed some light on this mystery!
Loveall believes that your DMT has aggregated over time, the molecules having clumped together into a sort of polymer that's hard to dissolve in NPS and even harder to smoalk. If you break up the polymer, it'll turn back into white xtals.
I suspect that some of your DMT has oxidized over time, and what you have now is similar to Loveall's polymer. Except, at the center of each "clump" of DMT is a molecule of DMT-n-oxide. If you reduce the oxide back into DMT, the polymer will fall apart and again leave you with white xtals.
My advice is to do a mini-A/B on it, but add zinc powder during the acid step:
- Dissolve all the powder in a small amount of near-boiling vinegar or citric acid. I recommend citric but I think acetic should work too. This may take a while, but keep it hot and keep mixing it, and it should all dissolve eventually.
- Add a few grams of zinc dust, and continue mixing it for like an hour. Keep it hot, 60-80°C. You should see it change color from yellow-orange to almost clear. Be sure to vent the container to avoid pressure buildup from the zinc reacting with the acid.
- Decant or filter off the zinc, add the NPS of your choice, and keep mixing gently while you add sodium hydroxide solution drop by drop. Wear safety goggles when handling aqueous NaOH!
- When the water layer turns milky and stays that way, stop adding base. Look to see if you have a layer of liquid DMT floating between the water and NPS layers. If you do, just keep mixing until it all dissolves into the NPS. Then pull most of the NPS out and replace it with fresh NPS. Add a bit more base, and mix it a bunch more. (The water layer will stay milky--this is just zinc oxide.) Then pull the NPS, combine it with the previous pull, and put all the solvent into the freezer.
- Freeze the NPS for at least 24 hours, then decant the solvent, dry the xtals, and do a final re-x.
You can buy zinc dust online for cheap, but in a pinch, you can get powdered zinc from fresh alkaline batteries (not ones that say "heavy duty" ). Use a pliers to remove the top of the battery, pull out the anode rod, and carefully scoop out the gray zinc paste. (Be careful not to get any of the potassium hydroxide electrolyte on your skin and try not to get any of the black manganese dioxide out with the zinc.) Rinse the zinc with fresh water 3-4 times, and if you see any globs of gel sticking around, pick those out. One size C battery got me about 10 grams of powdered zinc, before I went on eBay and got 3 lbs of zinc dust for $20.
If you follow Loveall's approach, DO NOT boil solvent in a confined space and DO NOT boil solvent over a flame! NPS vapors are unhealthy to breathe, possibly damaging to nearby surfaces, and
potentially explosive. Either do this in a very well-ventilated area, like next to a window with a fan blowing outside, or use a
reflux apparatus to trap the solvent before it escapes. And NEVER heat anything in a sealed container!
Whichever approach you try,
please let us know what you did and how it turned out! In the absence of conclusive analytical data, empirical tests like this might give us some clues into this phenomenon.