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Help! Recrystallization

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doc savant

doc savant

Dennis
tried to recrystallize less than a gram of white/yellow crystals scraped up with light substrate of of yellowish film (after completely dry) which had no apparent crystals. Never got any layering to the hot solvent. crystals/yellow film melted very quickly in bottom of shot glass before added any warm heptane. added a bit at a time stirring often. warm heptane cloudy with a yellowish tint, but no layering, nothing in bottom. Added a little too much heptane in the end probably, trying to see some seperation, but didnt. its still yellowish but clearer than was.

Why no layer? Since i just evaporated the naptha originally without freeze precip, going to try freeze precip now, although not sure if saturated enough to freeze precip. can still evap this obviously, but original naptha was clear and never really got cloudy either, sooooo....
 
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you answered your own question, too much warm solvent = everything dissolved = no separation of goods from impurities. Check the FAQ for exact amount of solvent per gram of impure product.

Now what you can do is just evap a bit your solvent and freeze it to retrieve what you have, and then recrystallize again properly if you want
 
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yes, but added an eyedropper-full at a time; I didnt just dump it. Eyedropper, stir, look, let sit, eyedropper, stir, look, let sit, keeping the hot water replenished every 10-15 minutes. Additionally, this must be less than a gram; only had a 100g of mhrb to start with, plus left half of the plant fat film in pan where there were no crystals. FAQ only gives amounts per gram. not less than a gram. See photo...no layering appeared at any level of shot glass, 1 eyedropper, 2 , 3, etc...
 
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amount stated in FAQ of ml per gram is a ratio, just make proportionally.

I dont know how many mls is a dropperfull, just measure or add slowly till some of the stuff dissolves and an undissolved part stays on the bottom, I think its pretty clear in the FAQ, no?

You should run some warm solvent on that uncrystallized film, there is most likely some dmt there.
 
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endlessness said:
amount stated in FAQ of ml per gram is a ratio, just make proportionally.

I dont know how many mls is a dropperfull, just measure or add slowly till some of the stuff dissolves and an undissolved part stays on the bottom, I think its pretty clear in the FAQ, no?

You should run some warm solvent on that uncrystallized film, there is most likely some dmt there.
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For any other respondents: again, solvent was slowly added in 5 or 6 increments using an eyedropper. Total currently at approximately 20-25 ml as viewed in picture. At no time was any kind of seperation observed. Not a big deal because I can simply, evap again and individually axe out each sea urchin of crystals leaving behind more impurities on each go, if freeze precip doesnt produce anything sufficient to leave behind purer crystals than there were originally. I imagine most of you are used to freeze precip acting as a filter before recrystallization, a stage I skipped because naptha never became cloudy till very small. I believe my crystals are probably reasonably pure, possibly more than would normally be purified by recrystallization? Might that explain the lack of fallout? a fair amount of dark goo stuck to the glass on the first decantation of the original extraction leaving water clear naptha, before ever attempting this recrystallization. Thank you for other more attentive thoughts on this problem, Im guessing Im likely as pure as I can get, this round.
 
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Noman said:
If that's heptane in the top photo and you cool it really slowly, you'lll see some separation start to happen.
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Ah, thank you, sir. That is heptane. I just checked the glass. two tiny dots of red brown have appeared on the bottom of glass, although where that color came from after this amount of time out of the cloudy milky faintly yellow fluid I couldnt say... havent a clue whats going on, what I should do, or what to do about what may or may not be happening. will wait a bit and probably decant it a second time before freezing it. Appreciate it , sir...:)
 

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See, here is why I am completely challenged when it comes to things like this. I think too much. Technically, the heptane was heated so that it can take on more dmt. if it is allowed to cool then the saturated heptane, i would assume, would begin to crash out a bit. As you can see from the photo, more is happening, but this is not as described on the tek, with a neat layered division of dark stuff on the bottom, in what appears to be described as a reasonably short period of time. I was looking to decant this the second time, but more seems to happen across longer periods of time. With the two little dark spots on the bottom of the shot glass, a suggestion of other miniscule red brown deposits seem to be appearing. a shimmery (oily?) look appeared in the bottom section of the glass, but not distinctly. I carefully decanted from the center top middle. It left a ring of orange red. and the shimmery cloudy in the bottom with faint possible small deposits of red brown adhered to bottom glass. If the glass cools from hot heptane, is this shimmery layer precrystallizing dmt, or discardable clear oils/fats? im keeping all of it. the decanted glass is MUCH clearer, but did a large amount of dmt head south to prepare to recrystallize? crashing out of the clearer top stuff. Sorry. Im not very bright.

Thanks :cry:
 

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Sorry, thats basically an empty glass with a little heptane in the bottom with an orangish wet ring where previous level was...dont know if i should go for the little heptane in bottom...thx
 
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No sir! I like explosions, but only on YouTube. It's difficult to find good lighting to take a picture. Stove is off and does not have an open pilot. Those are wet crystals, but vent hood fan is on high, pulling up. Good point, though, thanks...
 
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