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recrystallization with naptha Options
 
Teller
#1 Posted : 11/29/2012 11:02:38 PM

Blue Electric Monkey

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Ok, I've tried to search for this, but I can't seem to find any posts about re-xing with naptha, as opposed to any other solvent.

What I've done so far:
-Made a water bath for two jars, one with clean naptha and one with dried spice and a little spice oil.
-After all spice melted into liquid and naptha was very hot to the touch, poured naptha into jar with melted spice.
-Liquid turned a yellowish haze, then poured off liquid into a pyrex dish. A pile of impurities remained in the other jar.
-Repeated everything to ensure no loss of active components

So it seems like this worked to some extent judging by the clump of dust, hair and muck that was left behind in the other jar. My question is, do I let the spice infused naptha evap before doing freeze precip again? There's a good amount of liquid in the pyrex, way more than what I use when I do freeze precip from STB pulls. So I'm kinda stuck here. Evap first or go ahead and cool it down all the way, and why?
 

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RustySpoon
#2 Posted : 11/29/2012 11:30:26 PM

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i have re-x'd in naptha before, but usually youll want a small amount of naptha to re-x, about 20ml for about a half gram is what ive used. remember to not throw anything out until you know there is nothing left. i made the mistake of throwing out the yellow goo that formed at the bottom while using heptane to re-x and thought it was inactive plant oils and gunk...i was wayy wrong. *smacks self in face*

why did you use so much naptha to re-x?

if i were in that situation, id put a small fan over the dish and let some evap, or re freeze, if it even will. the higher the concentration(less naptha) for the amount of dmt in it, will freeze easier and faster.
 
3rdI
#3 Posted : 11/29/2012 11:31:00 PM

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I would evap til the naptha is cloudy then freeze precip. DMT will precip better when the solvent is highly saturated which is indicated by the clouding
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Teller
#4 Posted : 11/29/2012 11:37:11 PM

Blue Electric Monkey

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Oh, it's quite cloudy already. It's like a yellowish milk. Should've mentioned there was about 75-125ml of naptha and about 2g-2.5g of spice. I don't really measure these things when I do them, I just use my intuition.

I think I'll try letting it evap down a good bit before cooling it, and post the results.

Thanks guys. Cool
 
Teller
#5 Posted : 12/5/2012 7:50:25 PM

Blue Electric Monkey

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Here's my current "crop" after recrystallizing with naptha. After an evap and freeze precip, the dish had a good amount of oil in it, giving the spice a brown sugar color and texture. Would you recommend I do another recrystallization?
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ArcturianSeeker
#6 Posted : 11/21/2020 8:58:36 PM
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Never, in my experience, have I ever seen an extraction that is so dark. Do you think that you might have pulled somethings other than the typical alkaloids? I have only ever experiences yellow, really yellow, whitish yellow, and white in my pulls. There is a lot of stuff that we can reduce from the solution through the use of physical concepts relatable to that particular set of compounds.

What were you pulling from? I use MHRB exclusively.
 
downwardsfromzero
#7 Posted : 11/22/2020 7:46:42 PM

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Post is from ten years ago, and user was last seen 08 Apr 2013, so you'll probably not get a direct answer. Things have moved on a good deal since then and there is a current thread discussing possible polymerisation of DMT to form the dark goo, and the parameters associated with this phenomenon.

What is your experience, ArcturianSeeker?

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