October 24, 2007

More crystals, and a picture

As per recent comments... no, the lab does not have a camera. When pictures appear it is only because I happened to have my camera with me what a particularly photo-worthy event was happening in the lab. If I ever continue the saga of the Ir recycling there are more pictures which go with that. I must admit the whole process was so frustrating I'd rather not relive it, but perhaps... someday...

In the meantime... In a previous post I displayed the raw difraction data from a crystal I had grown. It was difficult to tell that this crystal was of poor quality just from the picture, but it was. I have grown the same crystal via another method and this is of much better quality. I'm including the diffraction pattern of this one to show how much better it is than the one previous. (A clue: those big white dots means that the diffraction of the crystal is better.)

X-ray quality crystals were grown from a slow evaporation of a THF solution under Argon.

October 12, 2007

cobalt is cheap

Since the Ir has been going so awfully terrible I've been looking into other metals. For those of you familiar with the periodic table you'll notice that iridium metal is in group 9 of the d-block, along with Rh and Co. These are typically metals of similar reactivity (Ir and Rh closer to each other than Co) so its common to look at the same molecules with a different metal. Reason being, Ir is the sort of thing in which the global production is measured in ounces, whereas Co is measured in metric tonnes.

The more interesting part to me, since I don't personally pay for the metals I'm using, is that Co chemistry produces some of the deepest blue and green complexes that you'll come across. Look up Cobalt Blue in wikipedia and think, prettier than that. I made my first green complex ever, which completes my personal chemical spectrum. My better half does seem to believe me, so perhaps I'll have to document that in the blog. I'm pretty sure the only one I wouldn't be able to get my hands on immediately is red. Green is one of the less common colors in the lab though.

I digress. True to the title of the blog, I made the new Co complex and got crystals on the first try. High fives were distributed throughout the lab on the way down to the crystallographer, and it seems that the crystals are well behaved (not twinned) and diffract well. Sweet.

Neon yellow/green needle-like X-ray quality crystals were grown from a solution of pentane chilled to a temperature of -40 C overnight.

Ir recycling step 5.2

I have become seriously delinquent in the updates. That's what happens when you get busy with real work I guess.

The muffle furnace was a disaster. I was able to fire the IrO hot enough, but since I let it go for so long, the salt vaporized and formed a glaze on the inside of the furnace. Jason explained to me (rather after the fact) that he wasn't surprised in the least that this had happened, and it was actually a pretty common problem they had to deal with when he was taking a ceramics class as an undergraduate. Basically what happened was this... There was a crack in one of the shelves in the furnace, and one of the three crucibles was set directly over the crack. This allowed a hot spot for form and the crucible broke, leaking molten salt onto the ceramic. The hot salt fused with the ceramic and lowered the melt temp just enough to make the crucible, shelf, iridium residue, and heating element meld together into one big block of solid meteorite like material. I'm really just about done with this whole process. I'm going to take on what I've got for the iridium and call it good enough. Pictures soon of the muffle furnace disaster. I'm really really busy with real chemistry.

October 5, 2007

organization

I walk into Prof. Heller's office to chat about some chemistry that's going on. On the way out I notice that there was a piece of paper with a yellow post-it note lying on the floor. I picked it up and placed it on Prof. Heller's desk. (Or rather, on top of the collection of papers, books, articles, and other things sitting on top of his desk.) An hour later I go in to collect the papers students turned in to him earlier so that I can begin grading them. I notice that the paper I had placed on his desk earlier has fallen off again and is on the floor in front of the door. I pick it up and place it on the desk heap again, this time closer to the center. Several minutes later I walk back into his office to ask a question about the grading scheme I should be using. The paper has again made its way to the floor. I pick it up on my way in and sit down. Prof. Heller looks right at me, picks the paper up off his desk, and throws it to the floor in front of me. I look at him kind of blankly. He explains... "That's a delinquent form that I need to turn in. If I leave it on my desk I'll never remember to do it." He points to the floor in front of the door. "That's the out-box."