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crystals/precipitate disappearing! Options
 
psychonautiloid
#1 Posted : 4/1/2012 11:41:03 PM
encountered a strange phenomena and wondering if others have experienced this. a freezer precipitation with naphtha and crystals were removed from the freezer, the excess naphtha was poured off, then the crystals were left to dry/let excess naphtha evaporate. several hours later, nothing appeared to remain in the dish, and when scraped, there was nothing! this was a second freezer precipitation from an earlier batch.

then, the same thing happened, also with used naphtha in a dish that hadn't been frozen but crystals had formed anyways.


both were in a pyrex container, both were used naphtha, and both had abundant, visible crystals before being left to dry. any ideas?!

thanks!
 
daedaloops
#2 Posted : 4/1/2012 11:54:05 PM
This happened to me too once, and I was just as confused. It seems that sometimes if you leave alot of excess naphtha on the drying dish, the crystals melt back into the naphtha and they evaporate away with it for some reason. (i used to think this was impossible)

What I try to do from now on is to move the crystals around on the dish so most of the excess naphtha stays behind and then I gently blow into the crystals with my mouth, this way the naphtha evaps really fast and you can literally see the crystals drying when you do that. Just don't blow too long or you'll faint lol.
 
InfiniteRegress
#3 Posted : 4/2/2012 12:35:01 AM
What Deadaloops said should work. However, if it continues to dissolve back into solution you may just have to let it precipitate off. What i do is put the naphtha solution in a large glass cooking pan or something and then i put a fan next to it. It should evaporate relatively quickly depending on how much solution you have and there will be nice little crystals waiting for you. Good Luck!
 
wingchun
#4 Posted : 4/2/2012 2:44:28 AM
Had same problem, still working on a best solution....

Things that help - drain the solvent and return the jar with crystals
stuck to sides back into the freezer - let drain upside down for
at least 30 mins - get rid of all the excess shell / solvent.

Otherwise crystals re-dissolve on warming to room temp.

Also - check it wasn't ice... as in cold h20...
this may look like nice crystal in the jar and will evaporate
away to nothing.

I am testing the method of filtering the final shell pulls
through epsom salts or sodium bicarbonate (powder) held
in a funnel by filter paper. I figure the dry powder
will absorb any water in the shell, but not the spice?

Double check your residue / sometimes I get a thin coat of a
yellow like oil, that seems active / just impure....

I don't think spice can evaporate away to nothing at room temp,
at least not that quickly - if you had some spice, at the
very least you should have been left with some oily gunk....


 
endlessness
#5 Posted : 4/2/2012 9:54:10 AM
 
DMT777
#6 Posted : 4/2/2012 6:59:05 PM
This has happened to me a couple of times, i think it was caused by a small amount of water getting into the solvent.
 
 
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