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Specialty Chemistry Forums => Materials and Nanochemistry forum => Topic started by: Corribus on February 13, 2019, 02:51:32 PM

Title: Heating under inert atmosphere
Post by: Corribus on February 13, 2019, 02:51:32 PM

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.

Title: Re: Heating under inert atmosphere
Post by: hypervalent_iodine on February 13, 2019, 10:13:39 PM

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

Title: Re: Heating under inert atmosphere
Post by: Corribus on February 13, 2019, 10:32:56 PM

Can you get an oven in a glove box?

Title: Re: Heating under inert atmosphere
Post by: DrCMS on February 14, 2019, 11:22:09 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?

Title: Re: Heating under inert atmosphere
Post by: Corribus on February 15, 2019, 12:48:11 PM

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!