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Extraction, recycling and smoking

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Z

zlatankomplex

Rising Star
Hi

I have a few newbie questions:

When extracting with a basic solution (NaoH) and later on sepation with a unpolar dilution (Naphta, bensen or other solvent) the DMT molecules "migrates" from the polar phase (water) to the unpolar phase following the "equal solves equal rule". Does any one know the equlibrium of this separation? I guess not 100% migrates to the unpolar phase?

Do you fully evaporate the solvent or do you pour of it off when sufficient crystals have been formed?

And finally the question regarding smoking.

I have understood that the dmt crystals are sensitive to heat and thereby a vaporized should be used. Does any one know what the perfect temperature for smoking? From Wikipedia i found the boiling point to be 160 C, is this the temperature I should be aiming for?

BR from Sweden.
 
1) Because not all the DMT will migrate to the nonpolar solvent, you should keep the basic solution around so that you can do more "pulls" with new nonpolar solvent later.

2) When evaporating, you should evaporate all of the nonpolar solvent. This means that evaporating will not leave you with recyclable nonpolar solvent. If you however decide to do a freeze precipitation, then you can recycle that nonpolar solvent when you're done.

3) Not sure on the exact temperature, but assuming that number is accurate, I would assume it would be the one to aim for.
 
Well, if you have the right lab setup, you can evaporate and collect the clean naphtha to reuse it....

When evapping before freeze precip you evap half or more (or until it gets cloudy when you blow on it or w/e)

After freeze precip, you just pour the naphtha out (through a filter if you want to, I don't as even if some of the crystals go with the solvent pour, I'm reusing it anyways to pull more)
 
SWIM's experience with 1 kg MHRB and Noman's Tek was thus:
5 naphtha pulls, combined and freeze-precip - no evap, as she didn't want that crap in the air.
yield was ~1.2%
the freezer has to be as cold as possible and the goods have to stay in for 24+ hrs for max yields.
Generally, she has found evapping to be useful and tolerable only at low volumes, < 50ml
 
Ljosalfar. So you only made a freeze separation? How do you practically do this? When you saw there was crystals in the bottom did you just pour of the solvent and re freezed the solvent again? Did you need to do dry the crystals?
 
With freeze precipitation, once you're sure all the crystals have precipitated out (the naptha doesn't look foggy or cloudy), you pour out the naptha back into the basic solution (and mix it around as you did before) and dry the crystals. Scrape them up as best you can. Often there may be traces of spice you can't seem to get. Don't worry about it. When you're done scraping, pour the naptha back in the container where the crystals were and put it back in the freezer.
 
After 24 + hrs in a very cold freezer, well formed and "slushy" crystals will be clearly visible and the naphtha will be clear.
Decant the naphtha (if one is careful, one doesn't need to filter), warm it, and add some to the MHRB basic solution for one last pull. Or just save it for next time.
The crystal/slush/few ml of naphtha can be:
a) allowed to evap and dry COMPLETELY, then sampled with care and attention... or
b) combined with a few more ml of naphtha/heptane, warmed until all crystals are dissolved, transferred to a smaller glass vessel,
allowed to cool then into the freezer to repeat the precipitation - this will result in purer product, as the oily yellows stay
at the bottom and most crystals will be close to white/clear.
She finds that "Canary" spice (a) is nice, crystal clear is dear.
Glad to help, safe journeys, let us know.
L
 
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