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Author: Subject: Sublimation
enkephalin
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[*] posted on 20-4-2006 at 07:53
Sublimation


I was wondering if anyone here had any experience with the vacuum sublimation purification of gram quantities of organic materials. More specifically what kind of apparatus works well, other than a dedicated sublimator. I had wanted to use a coldfinger condenser inside a side-arm filter tube, but i cant find one that has a socket connection. Any help would be very much appreciated.
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Magpie
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[*] posted on 20-4-2006 at 10:11


I have used a 20mm test tube with side arm equipped with a 13mm test tube as cold finger. The smaller tube is sealed to the larger one with a rubber adapter. I bought the adapter from a scientific supply house. But IIRC it was hard to find and a bit expensive.



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The_Davster
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[*] posted on 20-4-2006 at 12:29


I sublimated napthalene or camphor, I forget which, in a uni organic lab. I believe I used a 100mL RBF with ice water suspended over a 250mL beaker in which the compound was placed. Glass wool was stuffed inbetween the flask and beaker for a better seal.



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leu
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[*] posted on 20-4-2006 at 17:18


Quote:
I bought the adapter from a scientific supply house. But IIRC it was hard to find and a bit expensive.


One can freeze a rubber stopper and then drill it out using conventional drills and a drill press instead of paying such prices :cool:




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