Dr. Warfield Teague is retiring this year, which makes me feel old. He was one of the professors who helped make me what I am today – in his case, partly by keeping me out of his chosen field of inorganic chemistry. It was a good move on his part; I’d surely have blown something up good and thoroughly when I got to grad school, such are the opportunities in that area.
Unfortunately for both him and for me, his Advanced Inorganic course ended up scheduled for 7:40 AM back in early 1983. I started out my college career with a barrage of classes at that hour, and made every one of them. My sophomore year, I only skipped one class, and I waited for the lightning bolt to descend even for that one. But my junior year I had a professor or two whose lectures could be safely (even profitably) missed, and I began to get in the habit.
Teague wasn’t in that category, though. His lectures were fine; it’s just that they took place so early in the morning. My roommate David and I, both chemistry majors, found it harder and harder to summon the activation energy needed to make it out of the thermodynamic sinks of our beds. Dr. Teague’s threat to come over and teach the class in our dorm room didn’t quite do the trick (while lying there in bed, actually, the idea had a certain appeal). But his threat to start giving top-of-the-morning quizzes did. I showed up, and kept showing up. First year of grad school, now that’s where I started slacking off in my classes in earnest. But not all of the professors I had that year could communicate the facts of their specialty as well as Dr. Teague could for his.
The lab part of the course, that I would have shown up at 6 AM for. I don’t know how he’s done it in recent years, but 25 years ago (not possible, that), we could do pretty much any lab procedure that Dr. Teague would sign off on. There was a requirement that we do at least one low-temperature one, one high-temperature one, one metal complex, and so on. So the dozen or so of us in the class would root around through Inorganic Syntheses or the like, looking for interesting stuff. And there’s plenty of it in there, let me tell you.
In my case, the most memorable included the preparation of fluorosulfonic acid from scratch. Scratch means you start from concentrated hydrofluoric acid, a fine substance for the spirited undergraduate chemist to become familiar with. I can still hear the peculiar whine that solid KOH pellets make when you toss them into a plastic dish of the acid – they’ve a pretty short half-life in there, I can tell you. And I also made the magnesium analog of ferrocene – magnecene, I guess you’d call it – by one of those don’t-be-afraid-of-the-obvious routes: heat some magnesium turnings to about 600 C in a tube furnace, and pass fresh cyclopentadiene monomer vapors over them. Works great. And while you shouldn’t be afraid of the paper synthesis, red-hot magnesium metal is something else again.
While I was thus engaged, my classmates were setting off thermite reactions, making phosgene from carbon tetrachloride (chromium trioxide, five hundred degrees, nothing to it), and preparing titanium tetrachloride from the ground up. (I can’t recommend that particular prep – the liquid “tickle-four” comes out bright green from being around 1 molar in dissolved chlorine gas, so you’re going to want to redistill it, most likely). We learned a fair amount of inorganic chemistry, and more than a fair amount of lab technique. As evidence for that, we all survived.
Whether the latest generation of undergrads will get these kinds of experiences, I don't know. But I'm glad I did, and I'd like to thank Warfield Teague for providing them.
1. milkshake on April 28, 2008 10:04 AM writes...
I have seen preparation of ZrBr4 from elements and I never forget it - a quarz tube filled with Zr shavings, neat Br2 poured on top, the whole thing glowing red hot, brown-red fumes everywhere...
(That was done by a sugar chemist who has been doing lots of levoglucosane cracking from starch also - he was not faint-hearted man.)
I worked with FSO3H and that stuff is a very nasty smoke. And it ate a hole in sheet metal, about 2mm thick, on the lip of my hood because I spilled it as I cracked the ampoule. Triflic acid does not come anywhere near to nastiness of FSO3H.
We did only ICl3 in inor lab, by feeding I2 into condensed liquid Cl2 - and sure enough some dumb students handled the stuff without glives and ended up with blisters all over. But without care you can have a nasty mishap even in anlytical lab, one classmate has proven that sodium uranyl acetate solution poured into eye does indeed produce a nasty lid swelling and eye inflammation...
Permalink to Comment2. Tipstriflate on April 28, 2008 11:00 AM writes...
Impressive! The most complex experiment we were allowed to do as undergrads in Inorganic Synthesis was the prep of a quadruply-bonded Mo complex and that usually ended in disaster (cracked glass vessels!) Any other interesting experiments were discontinued by budget cuts...
Permalink to Comment3. processchemist on April 28, 2008 12:22 PM writes...
For sure this kind of chemistry is educationally useful (together with a solid preparation about chemical safety). But I know of some people that charge a 8000 lt glass lined reactor with acetic anhydride , then a sugar... then BROMINE and RED PHOSPHORUS... the "best" way to produce a bromoacetosugar, I suppose...
Permalink to Comment4. psi*psi on April 28, 2008 12:50 PM writes...
My undergrad inorg lab can only be described as LAAAAAAME. Then again, the room we were stuck in didn't have the capability to let us run a glovebox and a vacuum pump for a Schlenck line at the same time--not without an electrical fire, anyway--so there's a lot we couldn't do.
Permalink to Comment5. suicyte on April 28, 2008 1:33 PM writes...
Please excuse my (transatlantic) ignorance, but is 'Warfield' really a possible choice for a given name? Is it really 'Warfield' as in 'Battleground' or such? Come one, what kind of person would call their boy like this?
Permalink to Comment6. Derek Lowe on April 28, 2008 1:45 PM writes...
It's an uncommon first name - I think he's the only one I've met. But if I'm not mistaken, it actually goes back to Middle English.
Permalink to Comment7. Matt on April 28, 2008 3:25 PM writes...
My inorganic lab course had us prepare Nitrogen Triiodide, a contact explosive. This was only a few years ago. It was a strange feeling having something in our hood detonate into a hazy purple cloud and then have our professor be proud of us for it.
Permalink to Comment8. Petros on April 28, 2008 4:02 PM writes...
7.40AM. And I thought lectures 6 days per week at 9am was bad!
Permalink to Comment9. sroy on April 28, 2008 5:53 PM writes...
The gods have turned against Merck, either that or they have lost credibility.
______
Merck Cholesterol Pill Fails to Win U.S. Approval (Update1)
By Shannon Pettypiece
April 28 (Bloomberg) -- Merck & Co.'s cholesterol pill Cordaptive failed to win approval from U.S. regulators, less than a week after it was recommended for marketing in the European Union.
Merck plans to submit more data to the U.S. Food and Drug Administration to demonstrate the effectiveness of the drug, known as MK-0524A, the Whitehouse Station, New Jersey-based drugmaker said today in a statement. Cordaptive, the trade name for the drug, is a combination of the vitamin niacin and a new drug called laropiprant.
Permalink to Comment10. Ron on April 28, 2008 8:07 PM writes...
I would say that the most dangerous reaction I've done in my inorganic chemistry lab was the preparation of BF3-NH3. Nothing like what you've experienced, though!
I've always wanted to run a reaction with nickel tetracarbonyl, but no one will sell it except in massive quantities with an unreturnable lecture bottle.
Permalink to Comment11. NHchem on April 28, 2008 8:52 PM writes...
Congrats to you. I happened to be in the area where I received my degree and stopped by to see my old professor who has retired and is having some health issues. It was great to see the man who helped me become a chemist. He was my second father.
Permalink to Comment12. Jim Hu on April 29, 2008 2:41 PM writes...
I love the idea of the "thermodynamic sinks of our beds".
Permalink to Comment13. Sili on May 1, 2008 11:00 AM writes...
And yet again I despair at my lack of lab prowess (I was bad in org. too).
Had one day with classes from eight till six and by then I was nodding off. 6am sounds utterly ridiculous to me.
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