Dec 19
Fark
I am currently pumping hot water backwards through an upside-down Friedrich condenser full of aqua regia because a suckback accident with refluxing hydrochloric acid got antimony powder lodged between the walls and the inner spiral. The hot water is because it’s 3°C out, which is apparently too cold for the aqua regia to do much of anything. FML.
No commentsFeb 26
Research. whoop dee doo.
For a quarter of a million dollar piece of equipment, the NMR is mighty finicky some days. Wednesday is my longest lab day. I have a 4-5 hour period where I am confined to the lab, elevator, and NMR room. I probably spend at least 20 minutes out of that time using or waiting for the elevator, which runs from the lab on the third floor to the NMR in the basement. At least it interests me. And at least I’m seeing some results.
Well, after spending the better part of an hour running a H1, P31, and C13 spectra on my reaction product (should take 1, 3, and 10 minutes respectively, but all sorts of adjustments are made for the different spectra so it takes a good deal longer), I checked the graph of the P31 spectra, which is particularly indicative of reaction progress. Nothing. Flat line. No peak at all. I’m pretty sure I didn’t transmute the P31 into a non spin-active nucleus (although think of the consequences), so I assume something is up with the NMR. I also check the C13 spectra. One big fat solvent peak and what might be peaks in the mess at the bottom, but too small to be distinguishable. So, I went and got the guy who’s job it is to do maintainance on the NMRs. He opens his username and checks everything. It’s all a little off. Needs some calibration. The P31 seems way off. So, he calibrates it and runs one of our samples. for P31. The spectra looks fine now. There’s the nice peak at 21.5ppm from diphenyl phosphine oxide and two downfield, one larger from the product and one small one that is a side product. So, he leaves and I reopen our research group’s username. We run the sample again. I did the phosphorus first this time, just to make sure. It looks fine. So, I run the H1. Looks fine at first glance. So I run the C13 spectra…..nothing. flat line. Not even a solvent peak. I look at the H1 spectra again. Something is off. Things are definetly shifted. So, we found the poor guy again and this time he starts working on our username. The NMR is calibrating for H1 for all the spectra, it seems, and the H1 is not right anyway. He opens a command box instead of working through the software. Half an hour later, he wipes out a huge list of files and replaces them. Turns out our directory was completely messed up (sometime in the last few days) but not for any of the other users. He blames the fact that we’re running linux on an ancient Dell computer and the two don’t play nice. It’s now time to leave and go eat dinner.
Is it just me, or do you think they could splurge a bit on the computer running the $250,000 piece of equipment. They’ve got piles of tuition rolling in. Yeesh. At least I got a single sample through the microwave reactor between all the mess. Otherwise, it would have been 4 1/2 hours of my life down the toilet.
1 commentFeb 4
Testing. Testing. Is this thing on?
Hey look guys, I’m on the intarblag!
I always decide to write something for this just before I get extremely tired. I’ve been too lazy to get some amusing pictures off my camera to share. I usually end up just going to bed without typing anything or after typing a little and closing the window.
Nitric has been pestering me about why my blog is blank. Anyone got a good ol’ fashion’ pokin-stick that’ll reach Texas from Pennsylvania? Them whippersnappers…Get off my lawn!
For those who don’t know, I’m a junior B.S. chemistry major. I love chemistry. Well, organic chemistry mostly. I was a chemical engineering major, but switched majors after talking to a senior ChemE who wouldn’t know the difference between a ketone and a ketene. I know they aren’t all that bad, but they don’t learn much actual chemistry and use far too much physics and math for my tastes. I have been hanging around chemistry forums for years. Sciencemadness.org is the original one I joined. I don’t know if it’s gotten crappier and a bit sketchier with time or if I’m just more aware of it now. Still, practical chemistry getting done by amateurs is quite a feat. This isn’t something you see much of on scienceforums.net or just about anywhere else online.
From all of this, I am somewhat self taught. Classes are organizing the semi-random facts and snippets I have about reactions, even though my self-taught material goes far beyond the course material. I love a good synthetic challenge and they can and have kept me up for hours. I could definitely be the unlucky chap in this comic: http://xkcd.com/356/. (xkcd = awesome)
I am currently doing research. I have learned how to operate the $250,000 300MHz NMR in the basement of the chemistry building. This is the small one of two. The big one in that room is twice as large and is a 600 MHz. It strikes as funny, borderline hilarious, that there are cameras in the student computer labs. What, is someone going to steal outdated desktops? Meanwhile, beyond the door lock, there is no security protecting what is likely a million dollars or more of NMR machinery. Not that you could run off with an NMR or something, but still.
Peace out, folks.
2 comments