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marți, 8 februarie 2011

This May Be the Last Straw

So I bought this awesome laser pointer/pen/stylus 3-in-1 thingy for $20 from the bookstore, and the douchebag REU student who's too shy to ask to borrow it has both stolen and lost it. That I can deal with; after all, it's just a pen and my mom (via my student ID account) paid for it. But today...I walked into my office to find all my books pushed aside and the REU student's computer (courtesy of UK, the rotten bastards) on my desk.

So essentially, I have no desk. We can't isolate the PCN radical, all the parts for the matrix isolation system are in the machine shop, and now I have no desk.

And I was beginning to think not doing an REU was a good thing. Thanks for proving me wrong UK!

Gems from UK's Inorganic Lab "Lab Safety" Webpage

That's NOT dry ice! I didn't take the picture, but the caption underneath said that these peroxide crystals "autodetonated shortly after this photo was taken." They formed in an old bottle of ispropyl ether.

The page says something about not letting liquid oxygen condense in a trap, which seems odd to me (anything colder than liquid nitrogen seems too expensive to use in an undergrad lab!). It links to a video showing Purdue students lighting a charcoal grill with a lit cigarette and three gallons of liquid oxygen. If we really are going to possess the cooling power to condense oxygen out of the air in CHE 450G, I commend you University of Kentucky.

EDIT: The boiling point of oxygen is higher than that of nitrogen, so liquid oxygen will condense out of a constant stream of air. My bad!
Oh wow, this is a good one. In the spring of 1997 in advanced organic lab (CHE 533), someone dumped methylene chloride into a waste container containing some icky stuff, including nitric acid. He capped the waste bottle, and a couple of minutes later BAM! Shards of glass and chemicals went flying across the room. Miraculously, no one was injured.

Enter the Matrix

My lab's matrix IR apparatus is almost done, and naturally the guy I'm working with just had to have a baby. In the meantime, I get to watch over it and get things ready for our first target molecule, chlorosilylene. It is the silicon analogue of the one, the only chlorocarbene.

Herzberg was the first to investigate this molecule, having produced it in 1964 by flash photolysis of chlorosilane. As research on CVD intermediates picked up steam, a number of research groups obtained varied results on the extent to which chlorosilylene is produced during CVD. The Clouthier group, of which I am a humble member, revived spectroscopic studies of the radical by performing laser-induced fluoresence experiments on it in 1997. They obtained a whole slew of rotational constants, geometric parameters, and most importantly vibrational frequencies exhibited by the molecule. That's right, a whole slew.

Our goal is to observe HSiCl's ground-state vibrational frequencies directly by jolting trichlorosilane in an electric discharge and performing matrix IR.

Pictures of the apparatus to follow soon!

Bromosilane go BOOM!

Well ladies and gentlemen, I've reached a milestone...I caused my first explosion in lab yesterday. I was cleaning out a flask after a cold-trap separation of the reaction products of the bromosilane synthesis reaction:

PhSiH3 + HBr --> SiH3Br + C6H6

I believed that no bromosilane (or perhaps a negligibly small amount) remained in said flask. I was wrong. Set the flask inside the hood, put a little heat on it to vaporize things, took a step back to walk away, and BAM! A huge, quick flame burst out of the flask's mouth, accompanied by a horrible noise like a gunshot. Incredibly, the flask was just fine, save for a few brown spots that 48% HF took care of right away. Nothing got burned in the hood either. It was just a really loud, scary noise and a few flames. Doesn't mean it didn't scare the pants off me, of course.

The picture, for your viewing pleasure, is the LUMO of bromosilane.