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Author: Subject: Purging your reaction flask of air
CrimpJiggler
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[*] posted on 26-2-2012 at 21:03
Purging your reaction flask of air


In college we purged a 3-neck reaction flask of air by feeding nitrogen into the flask via this glass contraption which had oil at the outlet which served as an airlock. We had a reflux condenser in one of the necks so this piece of glassware somehow allowed nitrogen to pass through but did not allow solvent vapours to escape. This was a few months ago, I can't really remember the apparatus, anyone know the name of this piece of glassware I'm talking about?
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smaerd
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[*] posted on 26-2-2012 at 22:41


A Gas Bubbler?

http://en.wikipedia.org/wiki/Gas_bubbler

I have one from laboy, I bet dr. bob or one of the other people with large lots of lab glass-ware has one of these laying around :).

Of course you need gas in-lets/out-lets as well.




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AirCowPeaCock
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[*] posted on 27-2-2012 at 06:45


Because the nitrogen didn't condense in the condenser. :P



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Dr.Bob
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[*] posted on 27-2-2012 at 10:27


There is also a device called a "Firestone valve" which has a one way design to avoid sucknig oil into the flask, which is really good. They are pretty pricy, but work well. I have been using one for years, work best when pulling a vacuum on a flask, then allowing nitrogen in. They are really useful when doing a hydrogenation or other reaction where any oxygen left in the flask is very bad. (H2 + O2 + Pd = BOOM!)

I do have some of them, but currently all are lacking some piece like the stopcock, and they are a special one that I have to dig through a box of parts to find one. But I will eventually probably find the missing parts for one or two of them. See below for details. Ace and a few others also sell a similar design.

But for most cases a simple oil bubbler works to show the gas flow as well as reduce suckback potential. I just sold one, and have one left for sure, and I think more in another box. They are only $5.

http://www.sigmaaldrich.com/catalog/ProductDetail.do?D7=0&am...
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Arsole
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[*] posted on 28-2-2012 at 17:50


You do not lie those are pricey. :(



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BromicAcid
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[*] posted on 28-2-2012 at 20:33


These are the ones we use at work:

http://www.sigmaaldrich.com/catalog/ProductDetail.do?lang=en...

Basically there is a T at the top, gasses from your reaction come in one side of the T and nitrogen goes into the other side. The bottom of the T terminates in an oil reservoir. In the area above the oil there is another barb for the exit gasses. You always keep nitrogen on the bubbler so if there is suckback in the reaction it sucks back nitrogen.

Still I prefer the valve that Dr. Bob provided the link to, they're pretty awesome for repeated purge cycles.





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leu
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[*] posted on 1-3-2012 at 17:56


Argon works a lot better as far as purging air from an enclosed system :cool:



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