Submitted by Maggie Geselbracht / Reed College on Tue, 02/03/2009 - 01:37
Forums

Looking for advice:

We have a small bottle of VOCl3 that we ordered from Aldrich, and took into our glove box.  We used it very briefly to make up a standard reference solution for 51V NMR spectroscopy (VOCl3 dissolved in benzene).  After a few weeks, we noticed some odd discoloration on the outside of the small bottle, so I had my student put the bottle inside a jar in the glove box.  After a few months, the inside of the jar looks very odd, indeed.  The original bottle of VOCl3 has not been opened since the initial sample was made and yet the inside of the storage jar is now coated with dark orange-red material, and the jar seems to be filled with orange-red vapor.  My student (wisely) decided that this was probably not the best thing to keep in the glove box, and since he no longer had a need for the VOCl3, removed the entire jar and it is now sitting in the back of our fume hood (still sealed under N2 from the box).

My question is this:  What is the safest way to dispose of this jar containing the bottle of VOCl3 and whatever these vapors are?  My assumption is that there is some hydrolysis going on with trace amounts of water.  Any other thoughts?

 

Kurt Birdwhistell / Loyola University New Orleans

Maggie,

We have used V(O)Cl3 after many years on the shelf with various amounts of red/yellow material on the outside of the bottle.  In this condition it stills seems to be fine for many syntheses.  I think you are correct that the reddish vapor is some sort of hydrolysis product. 

If you want to dispose of it, I would drip it into a basic solution (NaOH(aq)). This will probably create quite a bit of Vanadium oxide waste.  If I were you I would leave it alone, unless you just want to get rid of it.  

Kurt

Tue, 02/03/2009 - 18:29 Permalink