[Dastanne]

Hello,

I'm new. I just started a Ph.D. in Montréal in organic/material chemistry and I decided to register to that forum because our group is getting smaller and smaller and my professor is often away. So I often find myself ressourceless when I have to do new (and dangerous...) things in the lab. So I hope I can find help from more experimented chemists here and eventually be able to help others myself

Basically, there's a reaction I want to try and that uses peroxytrifluoroacetic acid. This oxidizing agent has to be made using trifluoroacetic anhydride and hydrogen peroxide 90% in methylene chloride. It explains that the reaction won't be as efficient if made from 30% hydrogen peroxide and that it needs to be waterless.

So, since hydrogen peroxide 90% in DCM is not commercially avaible (I didn't find it on a few suppliers websites I looked at...), I guess I have to make it myself... However, distilling hydrogen peroxide seems like a very dangerous thing to do.

Does anyone have any tips or advices?

Thank  you

[Corribus]

Only authorized people are allowed to buy concentrated hydrogen peroxide. I'm guessing you are not among those authorized.

Distilling it can be extremely dangerous. I'd avoid it if you don't know what you're doing.

http://en.wikipedia.org/wiki/High-test_peroxide

[Dastanne]

Yeah that's what I thought. I perfectly know that I wouldn't know what I'll be doing. X)

Thank you X)

[408]

Clean your roti and flask a couple times with piranha, rinse out with distilled water, and then rinse with 30% peroxide.  Careful evap of 30 or 50% will give the good stuff.
Do behind a blast shield.

Corribus: Show proof that ordering small amount of conc. peroxide for lab use requires authorization in Canada.  I suspect it is just that nobody will sell it due to the hazards. 

[Enthalpy]

"Field Handling of Hydrogen Peroxide"
http://arc.aiaa.org/doi/abs/10.2514/6.2004-4146
just for the fun of nice pictures: shoe autoignition, and more.