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Author Topic: Heating under inert atmosphere  (Read 470 times)

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Corribus

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Heating under inert atmosphere
« on: February 13, 2019, 08:51:32 AM »

I need to heat a solid sample under fairly inert atmosphere for several days at about 80 °C. Anyone have any brilliant ideas about how I might do that? The sample is too large to fit through the neck of a standard glass flask. I do not have ready access to a Schlenk line, glove box, or anything of the sort, but I'm willing to go look for someone who does if I know what to ask for.
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hypervalent_iodine

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Re: Heating under inert atmosphere
« Reply #1 on: February 13, 2019, 04:13:39 PM »

I think your best bet is a glove box if you can find access to one.
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Corribus

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Re: Heating under inert atmosphere
« Reply #2 on: February 13, 2019, 04:32:56 PM »

Can you get an oven in a glove box?
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DrCMS

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Re: Heating under inert atmosphere
« Reply #3 on: February 14, 2019, 05:22:09 AM »

Do you have access to a glass or plastic screw top jar that the sample will fit in? 

If so:
  • oven dry the jar
  • cool it with a flow of dry inert gas into the top
  • add sample still with a slow flow of gas into the top
  • screw on lid
  • put in an oven at 80°C

It might even work with a ziplok plastic bag?
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Corribus

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Re: Heating under inert atmosphere
« Reply #4 on: February 15, 2019, 06:48:11 AM »

Something like this is kind of what I was thinking. I've tried something similar before for a related experiment and had mixed results, I guess because displacing the air isn't that efficient.

I thought about the problem some more and think another option is to use our vacuum oven. Since vacuum is, in a way, an inert "atmosphere", and I have no solvent to worry about, so it may be easier than trying to displace the air with an inert gas.

Thanks for the ideas!
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What men are poets who can speak of Jupiter if he were like a man, but if he is an immense spinning sphere of methane and ammonia must be silent?  - Richard P. Feynman
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