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Freezer Precip Problems

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Aeon

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Hi, SWIM has done several extractions in the past with good results, however, he has recently done a recrystalization using the freeze precip method and has encountered a problem he just can't figure out. Swim started with ~2g of fairly clean looking extract (white/off white gummi substance). He then did a normal freeze precip and yielded ~.5g fairly pure looking crystals. He took the left over solvent, evapped it, and got the remaining ~1.5g of gummi stuff back. The next time he tried a freeze precip, things didnt go so smoothly. After several days in the freeze, he noticed a minimal amount of crystals along the side of the glass, and at the bottom, a very cloudy goo-like substance, that no matter how long he waited, never turned to crystals. He then said "whatever" and tried again, evapping the goo to get the waxy extract, then again a freeze precip, but alas, the same thing happened, only goo, no crystals. Has anyone seen/had this happen to them? SWIM is kinda confused and very annoyed and needs help. Thank you
 
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The reason I posted this question is because I have read a lot of the procedures posted in this forum, and they are what I have tried. I followed the instructions exactly, and still with little results. I heated the naptha to near boiling, added it slowly and kept stirring til it had all just dissolved, then covered it, let it cool to room temp, put it in the fridge to chill for several hours, then I put it in the freezer for a few days. Am I doing something wrong? I'm seeing all these pictures of people doing it that way getting remarkable crystals, yet all im left with at the bottom of my glass is white jelly with a little naptha floating on top. Am I freezing it too quickly maybe? or is that a characteristic of water accidentally getting into the naptha?
 
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Thats what I was thinking, thank you. I guess SWIMs freezer has too much water vapor, and his plastic wrap was torn or something. He's trying a new method, just letting it crystallize at room temp as per a thread on here (the guy got fantastic looking crystals.
 
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SWIM has a relevant-ish question..
I hope this is ok Aeon :)

SWIM used a small airtight container to freezer precip.
There was a little bit of water in the lid (5 Drops App.)
SWIM is wondering how that water might manifest itself?
Would it become ice at the bottom of the container?

Thanks for the help.. :)
 
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