Crystallization problems

[crazimunky]

I followed the Nomans tek to a T and have been having the most difficult time with my freeze preciping. I'm pretty sure the freezer I'm using is cold enough and I have avoided contamination. However, I've been pouring out the naptha, then putting my jar back in the freezer upside down so all the leftover naptha settles down for thirty mins and then pour that out. But everytime, the crystals just dissolve away on me. I know they are DMT and not ice crystals because of the way they are forming and if I let it evaporate I end up with residue that eventually turns into a small amount of crystal. Any idea how to get my crystals to stop melting on me?

Or, I am patient enough to do just straight evaporation. Will that give me theoretically the same yield and should I just switch to that if I can't fix my freeze precip problem? Thank you for your help, this process has been one of great hope but some frustration.

 

[Gir]

Okay try this:

pour out your naptha, then take your jars instead of turning them upside down in the freezer, put them angled on a towel, and have a fan blow into it. It will dry them. Keep a close eye on them, they will dry fine.

Alternative method like slow evap is good too, if you are patient enough.

Maybe you might try using less naptha to redissolve them in your precip container. I like to use large open glasses for my drying (eg a martini glass hold the alkyhalls). good luck

-gir

 

[endlessness]

you should let it in the freezer upside down for more than 30 mins, leave for a few hours, and then take it off and scrape.. or do as gir said