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Re-X fail: no precipitation?! Options
 
Bud Shizzler
#1 Posted : 2/23/2013 11:36:57 AM

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hi nexus,

yesterday i scraped all my freezed and dried dmt into one container and warmed it with !USED! naphtha, slightly, to dissolve it all, but i took to long all in all and now there is no more precipitation happening after i put it back in the freezer some 20h ago. All there is is an oily film at the bottom and the dmt still seems to be in the naphtha cause it gets cloudy when swirled etc. or looks like it cant form large crystals.

can someone tell me what happened? i had this problem before, it seems to be either
-taking too long with the re-x, so other fats/lipids came over
-warming the whole solution instead of the naphtha alone before


i would be very happy if someone has an idea of how to rescue that spice. Evapping all of it and do a correct re-x seems the only option i got.

thanks in advance

update below
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Miracoulix
#2 Posted : 2/23/2013 12:25:15 PM
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I often red somethin about fast rubbing with a glass rod at the inner wall off your (glass) container helps the cristals falling out, even if it was in other contents. Never done this before, but may you´d give it a try.
 
Ambivalent
#3 Posted : 2/23/2013 12:37:31 PM

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Bud Shizzler wrote:
All there is is an oily film at the bottom and the dmt still seems to be in the naphtha cause it gets cloudy when swirled etc. or looks like it cant form large crystals.

thanks in advance


as i understood you dissolved your dirty spice in some warm solvent, but you skipped the step of decanting the warm naphtha and separating it from the yellow oil on te bottom.

it is possible that part of your dmt precipitated with the oils on the bottom. i would warm the solvent again, swirl to dissolve as much as possible, let it cool a little on room temp, and then decant. after that let the solvent to evaporate till it gets cloudy and put in freezer again.
 
Orion
#4 Posted : 2/23/2013 2:34:52 PM

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My philosophy is that when it all comes apart, put it back together.

Take all the solvent, oil, separated oil from the other jars etc, and combine them once more. Evaporate down till cloudy at room temp when you blow on it, then freeze precipitate that again, and re-x that again with CLEAN solvent one or more times.
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Kash
#5 Posted : 2/23/2013 6:30:58 PM

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The best way to recrystallize is to dissolve your spice in a MINIMAL amount of warm/hot clean naptha. If the solution is too dilute crystals wont crash out. SWIM says he likes to use zippo fluid better for recrystallizing.

To get the spice back just seperate out that yellow oil, and then reduce the naptha a bit, then stick it back in the freezer crystals should crash out.
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Bud Shizzler
#6 Posted : 2/24/2013 5:33:53 PM

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Thank you all!
Just warming that naphtha wouldnt've been a good idea, because that would have also made the gunk redissolve like before.
Precipitation did in fact happen, but as a white/yellow mixed film at the bottom. I was able to dry that again, and will now perform a correct re-x.
So for everyone who has screwed old naphtha that is filled with other oils or that laid with MHRB/Ac-Soup too long, this way should work for them too:

A1.) Freeze
Decant liquids (Pipette and Pipetteman*google-translate* are your friend)
(Fan-)Dry the precipitated film or crystals; put the liquids back in the freezer (if it, like mine, still holds spice that couldnt precip).
B1.) An Alternative Way would be direct evaporation of all solvent
--Both ways keep an eye on it for the right time its dry, because at full ventilation it goes wet->dry->gunk --

2. Whatever solids you recover, you perform a correct re-x on. What i did not get here before is that you only put the solids in for about a minute (and consequently that the naphtha is pre-warmed and fresh)
Then decant the Liquid within this short time range, because after this the naphtha also starts to redissolve the impurities. If your Naphtha is still yellow after this step, you just repeat from start, one more time was enough for me to get the best quality out of the worst gunk Drool
As long as the colour is clear it can be evapped with low air stream to perfect fluffy white xtals.

I also kept the fatty gunk from the bottom (because much), collected and dissolved it in lye and am planing to pull from it with another solvent, that gets jungle alkaloids.


thanks very much for your help, i hope my experiences help others with a bad naphtha problem
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