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DBL%20Hendrix%20small.png College chemistry, 1983

Derek Lowe The 2002 Model

Dbl%20new%20portrait%20B%26W.png After 10 years of blogging. . .

Derek Lowe, an Arkansan by birth, got his BA from Hendrix College and his PhD in organic chemistry from Duke before spending time in Germany on a Humboldt Fellowship on his post-doc. He's worked for several major pharmaceutical companies since 1989 on drug discovery projects against schizophrenia, Alzheimer's, diabetes, osteoporosis and other diseases. To contact Derek email him directly: derekb.lowe@gmail.com Twitter: Dereklowe

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« Getting Real With Real Cells | Main | Day Off »

February 15, 2008

Putting Out the Inevitable Fires

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Posted by Derek

Lab fires don’t happen as often as you might think, at least to hear the way organic chemists talk. We all have alarming stories of alarming reactions (often set up by some rather alarming labmates), but these things are harvested over a fairly broad range of experience. It’s a familiar enough topic that I can remember someone sitting down at lunch while we were swapping lab stories and saying “Oh, this conversation. . .”

But happen they do, and it’s always worth taking a couple of minutes to think about what you do in such a situation. That depends on the fire, of course. For starters, a small one burning out of the neck of a flask can be put out quickly just by slapping a beaker over the top of it. Never neglect that possibility, because it’s fast, effective, and (truth be told) if no one saw you do it, no one necessarily has to know that your (minor!) fire even happened.

Larger ones aren’t going to be so easy, but there are some potential ways out of those, too. My wife had a labmate in her molecular biology department who was always setting off blazes with the ethanol she used to wipe things down with. (This person neglected to turn off the Fisher burner used for sterilizing wire loops, etc., before she started sloshing the alcohol around). A fire like that will just burn itself out if you close the hood sash and let it rip for a few seconds, as long as you’re sure that there’s no fuel source (like the wash bottle of ethanol you might have chucked in there in a moment of panic, for example).

Most chemistry hoods, though, have all too many sources of fuel in them, so you probably won’t be able to put out a blaze through benign neglect. If it comes to a fire extinguisher, make sure you already know where the nearest one is, for starters. You'd be surprised how hard it is to find one of the darn things when you really need it. And once you've found it, make sure that you know which kind you’re using. The carbon dioxide ones don’t make the horrible mess that the dry-chem ones do, which is one thing in their favor, although I think in general they’re a bit less effective. You can tell the difference immediately – the carbon dioxide ones have the big nozzle on them, while dry-chem is a short, plain hose. My lab is outfitted with the latter, which makes me wish more than ever that we never have to use them.

And if you happen to have halon extinguishers (are those still around?), make a note of that, because the technique you may have learned for using the other ones won’t work. Instead of coming in and aiming at the base of the fire, with halon you have to stand further back and let the stuff shower down on it. A colleague of mine once blew the contents of a flaming oil bath all over the lab because he hadn’t been trained in that distinction.

The safety people always tell you that if you’ve used up one extinguisher and the fire still isn’t out, to head for the door rather than reach for a second one. That’s probably good advice (although I’ve seen it disregarded), and I’d advise you to take it. Actually, I’d advise you never to have that decision to make at all, but that’s not always up to you. You may be doing nothing but adding sodium sulfate to a bunch of dichloromethane today, but who knows? The guys next door might be gearing up for Trimethylaluminum Fiesta Days. You never can tell.

Comments (33) + TrackBacks (0) | Category: Life in the Drug Labs


COMMENTS

1. TNC on February 15, 2008 8:52 AM writes...

Weirdly, as soon as I read "AlMe3 Fiesta Days", the strains of "Ring of Fire" started up in my head. Strange.

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2. Don B. on February 15, 2008 9:32 AM writes...

Watch out for tri-ethylborane coming up the syring and out because of the way it wets glass.

Little green flames~0))

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3. Chronic Complainer on February 15, 2008 10:37 AM writes...

Comment Submission Error
Lately, I have been getting this when trying to comment: (and I have not been submitting comments in days and days)


Your comment submission failed for the following reasons:

Too many comments have been submitted from you in a short period of time. Please try again in a short while.

Please correct the error in the form below, then press Post to post your comment.

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4. VRD on February 15, 2008 10:44 AM writes...

First First Year Grad Student: I need to purify by sublimation 200 grams of potassium t-butoxide from this blackish old bottle from 1948 I found in the basement.
Second First Year Grad Student: Well, we don't have an apparatus, but it's just a cold surface over a hot surface. Take a big ass dish and fill it with the stuff, put a bigger ass dish over that filled with ice, put it all on a hotplate, and heat the bejesus out of it.
FFYGS: Poifect! (Proceeds to do just that, and the odd thing is that the kluge is working fine. The fine white powder is actually subliming and collecting on the bottom of the upper dish. But the walls of the lower dish start to get cloudy, so FFYGS LIFTS UP THE TOP DISH to see what is going on. Ball of flame. Massive ball of flame. SFYGS and rest of lab frozen with fear and awe. FFYGS, still holding large dish now full of ice slush, calmly pours this INTO THE FLAMING DISH. Eruption of inferno, volcanic roaring flames, too much light for the human retina to process. Lab filled with red and white glow. FFYGS cooly pulls the hood face down and steps back.)
FFYGS: The experiment is a failure.

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5. Derek Lowe on February 15, 2008 11:37 AM writes...

Gegen den Dummheit kaempfen Goetter selbst vergebens. Anyone who would pour an ice bath into that system deserves what they get.

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6. MTK on February 15, 2008 1:21 PM writes...

Best lab fire story I ever heard:

A friend was working in a four man lab with three Chinese students. He's doing something in his hood when he hears one of his labmates say something in Chinese. All three walk out of the lab. Our friend doesn't think much of it, but after about a minute decides to walk over to the other side. He turns the corner and sees a big fireball coming out of the hood. Evidently, the student was yelling, "Fire!" in Chinese. So all three bolted for safety. He hurriedly grabs an extinguisher and puts out the fire. He then assembles his labmates and proceeds to tell them if that episode ever repeats itself that the beatdown they will receive will render them incapable of saying "Fire" in any language.

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7. Jose on February 15, 2008 2:35 PM writes...

Personal favorite (almost fireball) was a 20 mL glass syringe, filled to the brim with BBr3 (neat). Sadly, BBr3 does really bad things to glass, and fused the plunger! Feck!! Now what?? I stood there yelling curses until my german postdoc labemate came to my aid. We carefully put a 22 gauge needle through the Leuer and got 90% of it out, so the resulting fire was small and happily contained!

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8. Aspirin on February 15, 2008 3:53 PM writes...

So how many lab fires have you started?! I say nobody is a bona-fide chemist until he has started at least one.

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9. MTK on February 15, 2008 5:50 PM writes...

Aspirin,

More than I can remember. (I'm counting ones that are very small). I think I've started two that required me to Pull, Aim, Squeeze, and Sweep. Whatever that number is I know that I've put out one more than I've started. In that case I used a halon extinguisher. If you've never seen one of those in action, their ability to put out a fire is truly awe inspiring.

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10. Polymer Bound on February 15, 2008 8:19 PM writes...

I've only had little ones from quenching things, but I've had the opportunity to put out other peoples' fires. Derek is right... those powder extinguishers work well, but the aftermath sucks.

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11. Jan on February 15, 2008 8:30 PM writes...

I just started one fire (not counting the fires I started with several nice chemicals like triethylborane, they were on purpose): Doing a hot column (for solubility reasons) and constantly reheat it with a heat gun works fine with toluene and dichloromethane but don't do it with hexane! It was the hottest column I ever ran. A rack with the different fractions was also involved, ca. 1.5 l of solvent...Luckily I had a carbondioxide extinguisher that left no mess so I was able to isolate my product afterwards after I had some time to calm down.
A fire in a neighboring lab had a different story: A chinese grad student received a writting warning because of some earlier misconduct. He took his lghter and burnded it in front of his professor, his last action at our uni.

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12. Jake on February 15, 2008 9:54 PM writes...

I had the misfortune once of catching an indirect blast from a class D extinguisher, one of the ones that "extinguishes" with powdered sodium chloride. I can't think of many times I've been happier with my goggles and quick blink reflex.

On the plus side, though, people pay big money to get themselves microdermabrasion, and I'm pretty sure a class D extinguisher pretty much does the same thing.

My favorite fire story comes from my boss - when the building he was working in was new, the elevators were doorless while it was still under construction. One day, some genius decided to load up a cart with a 4-liter bottle of pyridine and a freshly charged Na/benzophenone THF still for a quick trip upstairs. He pushed the button without realizing two of the cart's wheels were still outside of the elevator, and the whole mess tipped off into the hallway. All the fire of sodium, now with all the stench of pyridine!

My boss said "some people stayed to fight that one, but I figured I might just as well grab my notebooks and go for a beer."

Can't say I blame him.

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13. jose on February 15, 2008 11:29 PM writes...

Jan, How on earth does one run a "hot column?" I've never heard of such a thing!

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14. 100%rac on February 16, 2008 4:32 AM writes...

jose,

Hot column exist for sure.. I did a couple of them because I tried to column some ungodly insoluble shit. I used an electrical heating filament wrapped around the column (little bit safer then using a heatgun) and around that some cotton wool. The whole thing was packed in alu foil. It kept my stuff from crashing out on the column. It worked so to speak..

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15. milkshake on February 16, 2008 6:59 AM writes...

I started quite a few fires as eager undergrad. One memorable ignition happened in an empty freshmen teaching lab. It involved a half-liter of acrolein and a large quantity of magnesium perchlorate. Amazingly, heating this mixture did not produce outright explosion but it self-ignited and burned like a rocket engine. Within 3 seconds it was all finished and burned out - it produced like 10 buckets of very fine sooty ash and while making a deep whooosh sound like a jet taking off. The moment I saw the bright orange glare in the flask, I slammed down the sash and run. When the smoke cleared there was a feet high layer of soot in the hood, the soot tongues on the wall indicated where the hood was leaking. I looked up and there was a dark cloud by the celing that was slowly like a pillow settling on the entire lab. I lifted my notebook from the bench and there was a light rectangle left after it - the whole damned lab was like a chimney. I spent one very unprodusctive afternoon and a big bottle of detergent and washed everything, no-one ever found out about the incident.

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16. bob on February 17, 2008 12:34 AM writes...

Good post but you forgot the good old sand bucket. I started more fires than I would ever admit and nobody ever knew about any of them. See fire, walk to sand bucket, dump sand bucket on fire, scoop sand back into bucket, move on without getting hassled by safety people. We were supposed to fill out multiple page incident reports every time there was any fire at all, complete with why it would never happen again. Some of them were so retarded I kind of wanted to fill out the report - "will make sure flask has no flecks of sodium in it before washing with acetone then water".

In this area chinese grad students are a blessing as they'll never rat you out (either that or they can't speak english well enough to rat you out).

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17. Petros on February 17, 2008 9:57 AM writes...

Two of us were chatting to a graduate chemist who had just completed a hydrogenation using Pd/C when we smelt the smoke.

He had tipped the (unwetted) used catalyst straight into the paper bag that was the bin by his becnh!

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18. pharma giles on February 17, 2008 5:28 PM writes...

Have you heard of Firetrace? It's basically a pressurised plastic tube that runs around the back and sides of the cupboard - if a flame melts the tube, a dry powder cylinder vents its contents through the hole. It's amazingly effective. And no, I don't own shares in them.

There's also a new water-based fire suppressant called F500 that's doing the rounds - it's a radical suppressor, like Halon, but without the environmental issues. It's very effective for solvent fires.

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19. gibbon1 on February 17, 2008 9:06 PM writes...

The refrain I've always heard is the size of a fire you can put out with a fire extinguisher is remarkably small. And I having dumped two of them at a fire little larger than the average campfire I'd have to agree. You could get the fire out but it would just start up again. A surprisingly short blast with a hose did it in.

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20. DrSnowboard on February 18, 2008 4:00 PM writes...

Stupid fire during postdoc in Paris. Tried to kill off Buli residues by adding EtOAc (yes, I know, I was hungover). Poof followed by being covered in small burning embers. Cue comedy patting of flaming fragments on labcoat. Alain the technician sighs, puts down his pipe that he's been sucking on thoughtfully, grabs the extinguisher, walks over and hoses me down with CO2. Walks back and sucks on his pipe thoughtfully once more.
Merci Alain! One cool dude.

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21. MTK on February 18, 2008 4:49 PM writes...

Snowboard,

Your pipe-smoking labmate reminded of a time when I saw someone smoking a cigarette while shaking a 1L sep funnel. I was sure that he was going to blow up the entire building.

When I saw him the next day I asked "WTF?" He explained that he was doing some sort of cyanide chemistry and that by the time one smelled cyanide it was too late, but that cyanide does impart a unique taste to tobacco smoke at levels lower than one can smell it. So this was his early cyanide detection method.

Honestly, I think he just wanted an excuse to smoke in the lab.

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22. CatCube on February 19, 2008 5:34 AM writes...

The guidance I've always gotten in our safety classes was, "Fighting a fire is like fighting a person: if it's bigger than you, get out of there."

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23. Paul Norman on February 19, 2008 5:49 AM writes...

Although I've not started any major fires myself, the best one I've seen the aftermath of was a dewar of liquid oxygen.

http://youtube.com/watch?v=pr-rhD6cuhM

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24. mevans on February 19, 2008 9:37 PM writes...

I worked with a lot of pyrophoric stuff in the laser lab, but only once did it blow up on me. It happened after a vacuum synthesis that I knew turned out really nasty that involved making silyl bromide from HBr and phenylsilane...I didn't think there was enough silyl bromide in the reaction flask to explode, but BOY WAS I WRONG! For a split second that vacuum flask was a freakin' flamethrower. Nothing caught on fire per se, but it did char the flask quite a bit.

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25. processchemist on February 20, 2008 4:50 AM writes...

Tert-butyl lithium: if you work on a pilot plant with low pressure steel cylinders, no problem.
But when you need to use a transfer line with needles to put 2 liters of solution in a dropping funnel with a septum, I know no way to avoid a bunsen-like flame when you change the bottle. You can always extinguish the fire with flow of Ar or nitrogen directed towards the needles, but I never managed to avoid any ignition.

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26. milkshake on February 20, 2008 7:32 AM writes...

one solvent that cathes on fire extremely easily is CS2, the vapor self-ignition temperature is about 120C - much lower than with hydrazine or ether. I once made a mistake of putting a Liebigs reflux condenser on a flask with 0.3L of CS2. I took the condenser straight from a glassware-drying oven, put it on and there was a whistle-like shot and flame shot right through the condenser.

Process Chemist: I have done tBuLi canula transfers only on 200mL scale, and sure it catches on extremely easily. It does not help it comes in pentane. I suppose one can blow some Ar through the canula for about 20s after the liquid is transfered, then take the canula out of the septa of the addition funnel while a stram of Ar is stil flowing through it, then pull the canula out of the empty bottle that is stil pressurised with Ar. The solid crust on the tip is likely to glow anyway but at least you wont get a flame spitting out like a red flamethrower. (I acknowledge that many problems - the hazzards, heat transfer, stirring, drying etc - are increasingly more difficult with scale, and the difficulties grow in a non-linear fashion.)

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27. Don B. on February 20, 2008 9:48 AM writes...

In thinking back, I believe I have put out about 3 times as many fires as I have started.

For the younger audience tert-butyl lithium used to be supplied in one gallon paint cans~0))

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28. processchemist on February 22, 2008 4:00 AM writes...

milkshake:

when , changing the bottle, you blow the canula with Ar or nitrogen in a typically assembled system usually the inert gas flow comes from the reaction system. And here's what happens
1) you obtain some solid pyrophoric residue
2) you strip solvent from the system
3) you get your flame

The only way to get out can be to mount the canula like a charging line on a reactor, with a three way valve for nitrogen and a simple valve on the line. Never done that: risks of a clogged valve on a canula are higher than a small (and expected) flame.

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29. Anonymous BMS Researcher on February 22, 2008 6:28 AM writes...


I started my first and only lab fire at about twelve when I was extracting chlorophyll from some leaves, which involved boiling them in ETOH. Fortunately, I was able to put it out myself. Nobody else was home, which was fortunate for me in terms of avoiding parental censure, but could have been very unfortunate had this fire spread beyond my ability to put it out unassisted!

I learned the appropriate lessons about fire safety, and such an event did not happen again.

When my wife and I took the mandatory safety briefing for new postdocs at Yale in the early 1990s, the most memorable slide by far showed what happened about 4AM one night to a lab in which somebody put volatile solvent into an ordinary fridge. There's a reason why certain things must only be stored in expensive fridges that are approved for storing such stuff!

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30. Canuck Chemist on February 23, 2008 1:21 AM writes...

I haven't actually used this, but I read years ago about a simple device for handling very pyrophoric solutions or liquids with a steel needle or canula. It's simply a short piece of glass tubing which is sealed at both ends with some kind of septa. The interior of the tube is flushed with inert gas, and then it is pressed on top of the container with the pyrophoric material. The needle is inserted through the glass tubing and then immediately into the container. The liquid is transferred (e.g. into the syringe), and then the tip of the needle is pulled out of the container into the middle of the glass tube. In this manner the liquid can be transported without flames.

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31. markm on February 23, 2008 9:32 PM writes...

Gibbon: It depends upon what's burning. While I was in the Air Force, I went through some basic firefighting training where they'd ignite large shallow trays of gasoline or jet fuel (kerosene). One puff with an extinguisher in the right place knocked it right out - all you had to do was to blanket the kerosene to keep out the air for a second and it cooled below ignition and wouldn't relight when the air came back. OTOH, you get quantities of wood, paper, or fabrics involved, and they hold the heat so if you just smother the fire, it will start up again as soon as more air reaches the fuel. Large quantities of water work best, not to separate the fuel from the air, but to cool down the fuel below the ignition point - but a fire extinguisher you can carry isn't going to hold enough water or heat-absorbing chemicals to put out anything bigger than a trash-can fire, so for wood/paper/fabric fires, you move fast and hope to stop it before it builds up too much heat, and if that fails you hope someone else is getting out the firehose while you slow the fire down...

Chemical fires are outside my training. I'd imagine that some chemicals will act more like that kerosene, and others might hold the heat - plus the additional factors of possible reactions with water, poisonous fumes, etc. Which is where it seems the sand bucket would come in handy - there aren't any exothermic reactions possible with SiO2, are there?

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32. Norepi on March 2, 2008 1:43 PM writes...

I've started small sodium fires, but nothing major.

The best one I've seen: My undergrad supervisor is attempting a large-stale recrystallization of some nasty aromatic acid from water, which he has in a 4000 mL beaker. The thing's sitting on a hotplate, boiling away at full power. Next to that (several inches away) is a 1 L sep funnel containing ether, which catches on fire and shatters. Me, standing at the rotovap, hears glass breaking and looks over to observe that supervisor's fumehood is a roaring mass of flames. Fire extinguisher is emptied into mess. Whole incident resulted in the destruction of the vacuum lines, the sep funnel, the 4 L beaker (plus product), two other very large beakers, and a 600 mm Allihn condenser.

Best one that happened in my current group: Postdoc decides to do large-scale LAH reduction early in the morning on a very, very muggy summer day. Is weighing out LAH at the balance when, as he put it, "the whole works went up like a Roman Candle." Postdoc decides best plan of action is to chuck lithium Molotov cocktail into nearest fumehood. Sash of nearest hood (mine) is closed, LAH grenade bounces off and promptly explodes, showering a six-foot radius of the lab with flaming lithium salts.

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33. gm137 on April 21, 2008 2:32 PM writes...

I have started a good many fires in my time as a chemist, and some, I can honestly claim, were accidental...

Funnily enough, one of the most difficult - to -extinguish blazes I created was actually rather tame: simply a short-circuit in one of our microwaves appropriated from the faculty lounge for use in excitation studies.

Halfaw through a long run, there was a brief sputtering, and some small flames puttered up through the vents at the top. "Fair enough", I say, and take the nearest CO2 extinguisher down, PASS, and enjoy a noisy billowing blast or two. Thing is, when I stopped, the microwave was still alight. The vents were not letting in any gas, so the damn thing re-lit like a trick candle whenever you stopped the discharge. With the flames starting to reach distinctly unamusing heights, we decided to crack open the door slightly and blast through the gap, which fortunately worked with no mini-backdraft to enliven our day further.

I like your sand-bucket theory, markm, and subscribe to it myself! Mind you, there are one or two reactions that you can speed up with SiO2; I recall our first college chemistry lecturer mixing sand and finely-powdered magnesium, lighting the lot with a perchlorate - acid "fuse", and spending the rest of the term reassuring us that our sight would return....probably.

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