Maybe someone can check my tek for errors...
In summary, I performed an A/B extraction on 100g ACRB, using citric acid, NaOH, deiodized salt, and heptane for nps. The initial dry result was 3.5g of material, fluffy white stuff and goo. Mechanically separating the nice stuff, I opted to try dry ice to clean up what was left. I decanted the solution off some brown gunk that wouldn't dissolve easily, then treated 5x with dry ice (rewarming in between), yielding some yellowish gunky chunks. Poured the clear nps solution off into another jar and chilled in the freezer for a couple days. Instead of crystalizing, its just a sort of white sludge (a bit poached eggwhite looking). What the heck is this stuff? It was in solution when it was pouring into the jar prior to chilling, so it can't be the NMT carbamate right?
Detailed what I did:
Day 1: - made up some acidic solution 40g anhydrous citric acid + 4L distilled water (pH ~2.2)
- Chopped bark with shears, and ground it to a coarse coffee grind level in a blender. Added 250mL acidic water and froze/thawed 15 times over the course of several days
Day 4:- Did 4 acid boils. 1L of acid solution diluted by a half, light boil for 1:45 per boil.
- Strained contents through cheeze cloth in between boils.
- gently reduced to final volume of 750mL
Day 5:- Slowly bassified with 80g NaOH (temp rose to 50C)
- Did 4 pulls with +30mg heptane +1-2tbsp kosher salt
- Pull procedure: 2mins agitation/swirling. ~5mins (or until separated) rest in warm water (45-55C) 10X per pull
- Collected 111g yellowish opaque nps liquid and froze overnight (-20C)
Day 6:- Decanted nps off jar and dried 1h under fan to a weight of 3.5g
- Mechanically separated white fluffy crystals (0.5g)
- Readded nps, warmed and dissolved most of the goodies, brown sludge would not easily dissolve. Decanted nps to another jar.
- Treated with dry ice 5 times: Added 5-10g chunk, swirled the bubbling chunk to ensure saturation with bubbles, final temp ~5-15C. Warmed back to 50C in bath until most precipitates were redissolved and repeated.
- After last dry ice treatment, decanted rewarmed solution off yellow sticky gobs into another jar for chillling
- After several days in the freezer, fluffy white sludge has come out of solution, but is not crystallizing like DMT normally would.
EDIT:
Attatched photos:
1. Dried crystals from combined pulls
2. Dried crystals from combined pulls
3. Mechanically separated fluffy crystals
4. Weight of nice xtals
5. Left over goo
6. Immediately after dry ice stops bubbling, everything is out of solution
7. Warming it up, most stuff goes back into solution
8. After all dry ice treatments just yellow gobs left, clear nps poured into another jar for freezer
9. Sludge that precipitated out in the freezer, but didn't crystallize
10. Poured off sludge to another jar, only an insignificant mass of crystals seem to have formed from 3g of initial goo material
TxRx attached the following image(s):
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