Sciencemadness Discussion Board

Ampoule sealing inside the glove box

briankim78 - 9-3-2011 at 23:11

Ampoule sealing inside the glove box


Dear all,

I am preparing some chemical which is very reactive to the atmosphere.
Therefore, I am trying to put the material inside the glass ampoule and seal it while it is prepared inside the glove box.
The glove box I use is filled with Argon.
Any suggestions?

ldanielrosa - 10-3-2011 at 01:49

What precisely is it sensitive to? If exhaust from an oxyfuel torch with reducing flame is not an option, then maybe heat the ampule stem on a piece of metal that you play a tig torch on.

Can you seal the top of the stem with epoxy in the glove box, the properly seal it by more mundane means once it's protected?

ScienceHideout - 13-3-2011 at 15:09

I've sealed an apule of sodium, which is somewhat air reactive. I just put the oil in the ampule too. What if You fill the ampule with oil, add the sample in the glove box, and seal it outside the box?

UnintentionalChaos - 13-3-2011 at 15:20

Quote: Originally posted by ScienceHideout  
I've sealed an apule of sodium, which is somewhat air reactive. I just put the oil in the ampule too. What if You fill the ampule with oil, add the sample in the glove box, and seal it outside the box?


Because he doesn't want oil in his laboriously prepared compound?

Arthur Dent - 13-3-2011 at 16:54

It might be much easier to do your ampoule sealing by gently blowing a stream of an inert gas like argon in the ampoule to displace the air as you're filling it with your sensitive compound. Then while the ampoule is still fed with argon, seal it with a small torch.

Or is your compound so sensitive that it cannot even for a brief moment be exposed to air?

Robert



bfesser - 13-3-2011 at 17:45

Put a rubber tube on the neck of the ampoule while in the glovebox and clamp it. Then remove from the glovebox and seal. Simple.

Contrabasso - 14-3-2011 at 01:24

If this is to be a frequent need then look at the hot air guns used in solder rework stations. They are simply an electric heater which heats a stream of gas to a "melts solder" type of temperature. Feed your argon through one and use it as a blowtorch. Use great care because the output IS flame hot but it looks like just a stream of gas('cos it is!).

Heinrich - 14-3-2011 at 02:32

Quote: Originally posted by bfesser  
Put a rubber tube on the neck of the ampoule while in the glovebox and clamp it. Then remove from the glovebox and seal. Simple.


I've done this with highly air-sensitive materials, most recently with TiCl3. Works like a charm, but i have to admit that i was a little nervous carrying at around. Probably the simplest and cheapest solution also.

redox - 5-6-2011 at 10:11

What exactly is your atmosphere-sensitive compound?

quimica - 6-6-2011 at 23:40

Quote: Originally posted by bfesser  
Put a rubber tube on the neck of the ampoule while in the glovebox and clamp it. Then remove from the glovebox and seal. Simple.


I don't quite get it. How can one seal an ampule with a rubber tube atop of it? Wouldn't rubber be in your way or catch fire when you heat an ampule?

Dr.Bob - 7-6-2011 at 07:07

Ampules have long necks, so you can seal the top with a septa or piece of rubber and still heat it below that a few inches and seal it. I did that in graduate school and it worked fine. You can also get ampules with teflon type plugs which can then be sealed in a flame outside of the glove box. There are also sealable shlenck type tubes that work fine for storing air sensitive compounds.

Bob