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Graduate School

Accident Report, or One Damn Thing After Another

I have this from a lab-accidents-I-have-known discussion over on Reddit. It is, of course, unverified, but it’s depressingly plausible. As a chemist, this one is guaranteed to make you bury your head in your hands – it’s the second law of thermodynamics come to take vengeance, with the entropy increasing as you go along:

“A graduate student was constructing three solvent stills (dichloromethane, THF and toluene) inside a hood in Room XXXX. As a final step in this process, the student was cutting pieces of sodium metal to add to the stills. Once the sodium had been added, the student began to clean the knife used to cut the sodium. During the cleaning, a small particle of sodium was apparently brushed off the knife. The sodium landed in a drop of water/wet spot on the floor of the hood and reacted immediately making a popping sound. The graduate student was startled by this sound and moved away quickly.
In his haste to get away from the reacting sodium, he discarded the knife into a sink on the bench opposite the hood in which he was working.. Apparently, there was another piece of sodium still adhering to the knife since upon being tossed into the sink, a fire ignited in the sink, catching the attention of another student in the lab. As the flames erupted, the student noticed a wash bottle of acetone sitting on the sink ledge nearby. He immediately grabbed it to get it away from the flames, but in the process, squeezed the bottle, which squirted out some acetone which immediately ignited. The student immediately dropped the bottle and began to evacuate the lab. As he turned to leave, he knocked over a five gallon bucket containing an isopropanol/potassium hydroxide bath which also began to burn. This additional fire caused the sprinklers to activate and the fire alarm to sound which in turn resulted in the evacuation of the building.
When the sprinklers activated, water poured into the bulk sodium-under-mineral-oil storage bottle which had been left uncapped in the hood resulting in a violent reaction which shattered the bottle sending more sodium and mineral oil into the sprinkler water stream. This explosion also cracked the hood safety glass into numerous little pieces although it remained structurally intact. By the time the first-responders arrived on the scene, the fire had been extinguished by the sprinklers, but numerous violent popping sounds were still occurring. The first-responders unplugged the electrical cords feeding the heating mantles, shut off the electricity to the room at the breaker panel and waited until the Fire Department arrived. Eventually the popping noises stopped and sprinklers were turned off. The front part of the lab sustained a moderate amount of water damage The hood where the incident began also suffered moderate damage and two of the three still flasks were destroyed. The student, who was wearing shorts at the time of this accident, sustained second and third-degree burns on his leg as a result of the fire involving the isopropanol base bath.
There were some additional injuries incurred by the first-responders who unexpectedly slipped and fell due to the presence of KOH from the bath in the sprinkler water. These injuries were not serious but they do illustrate the need to communicate hazards to first-responders to protect them from unnecessary injury.”

I doubt if the sodium was being added to the dichloromethane still; I’ve always heard that that’s asking for carbene trouble. (Back in my solvent-still days, we used calcium hydride for that one). And it would take a good kick to knock over a KOH/isopropanol bath, but no doubt there was some adrenaline involved. I’m also sorry to hear about the burns sustained by the graduate student involved, but this person should really, really have not been wearing shorts, just as no one should in any sort of organic chemistry lab.
But holy cow. The mental picture I have is of Leslie Neilsen in a lab coat, rehearsing a scene for another “Naked Gun” sequel. This is what happens, though, when things go bad in the lab: we’ve all got enough trouble on our benches and under our fume hoods to send things down the chute very, very quickly under the wrong conditions. And were these ever the wrong conditions.

55 comments on “Accident Report, or One Damn Thing After Another”

  1. Josh says:

    Too damn funny. Imagine Kramer (Seinfeld) in a lab. It would play out just like this.

  2. TeddyZ says:

    Its sounds slapstick, but actually its not funny at all…think of what happened at UCLA? I look back on my time in gradschool/postdoc and then back to how I worked in industry: first in the Wild West of Safety (Discovery) and then in a GMP environment. Its amazing how your feelings towards safety evolve.

  3. NJBiologist says:

    “When the sprinklers activated, water poured into the bulk sodium-under-mineral-oil storage bottle which had been left uncapped in the hood resulting in a violent reaction which shattered the bottle sending more sodium and mineral oil into the sprinkler water stream.”
    I don’t think our hoods have sprinklers inside them–is that the norm in chem labs?

  4. DannoH says:

    While it sounds somewhat Rube Goldberg-ish, it illustrates an interesting effect of having people as key control components in your process.
    It was my experience back in the day that the first symptoms of an accident at a large scale plant were usually some manner of pressure transient (“did the building just shiver?”) followed by the always fun “WTF was that?!?”
    I will refrain from going off on my fear of bottles left inside hoods, especially those with yellowed old paper labels with typewriter written acronyms on them.

  5. Bear says:

    Naked Gun? To be honest, I was thinking “Three Stooges remake” as I read that.

  6. molecular architect says:

    Not sure whether to believe this whole scenario, just seems to be, as per #4, Rube Goldberg-ish. I remember when solvent stills were a standard part of every organic synthesis lab but I haven’t seen one in an industrial lab in many years. For most uses, the anhydrous grade solvents are suitable. My last employer installed a Grubbs-type system where multiple anhydrous solvents could be dispensed under Argon. For critical applications, we titrated for water with a Karl Fischer apparatus. The Grubbs columns did an excellent job producing anhydrous, oxygen free solvents without the fire danger of stills. Give academia another 75 years and it will be the standard there as well.

  7. nitrosonium says:

    i realize really, really dry solvents have their place but who uses solvent stills like this any more?
    i have not used “freshly distilled” solvents in the last 10 yrs or so. even with tons of organolithium grignard, cross couplings, etc.
    just seems really unsafe and perhaps not useful??

  8. tocket says:

    This is why it’s important to keep calm when unexpected things happen in the lab. Panicking is hardly going to help you come up with the correct way to deal with the situation. Even when your lab is on fire, it usually does not hurt to stop and think for a second before you take action. It is very likely that you will find a better solution to the problem.
    This is of course much easier to say than to actually do. It takes experience.

  9. Pat says:

    Lets review the safety violations (CA law)…
    1. Flammable solvent within 6 inches of a sink
    2. 5 gallon base bath left on the floor, and not in flammable storage
    3. Wearing shorts in lab

  10. Mr. Fixit says:

    While this sounds plausable, does anyone else think it is far fetched. If this did happen, those involved should be kicking themselves, and I almost feel bad for them. Can anyone confirm this story?

  11. opsomath says:

    Utterly plausible and depressing. I’ve always said that one of the biggest safety hazards is a cluttered lab; any time you have a lot of stuff out, any small mistake (such as a startled student making a grab for a falling object) can snowball, particularly when some of the clutter is volatile, flammable solvents.
    Given how good an ignition source alkali metal/hydrides are, if I am ever running my own shop I will be sure to provide specific training for these items. It seems that we hear these stories a lot, Milkshake had a similar one which he contained effectively because he’s not a spaz.

  12. Chemjobber says:

    @8: I agree completely. Yet more evidence that it would be best if safety training incorporated the “panic versus think” process in the live training.
    Instead, we’re out in the parking lot with a fire extinguisher and a pan of gasoline.

  13. Cruel Miracles says:

    “but this person should really, really have not been wearing shorts, just as no one should in any sort of organic chemistry lab”
    In my PhD days (which are only a few years behind me), the safety people, when hearing complaints about the temperature in the labs on hot summer days (30+ °C in real values, not nearly enough in WGBT), told us that as long as we were wearing goggles, gloves and lab coat, we could be naked under there for all they cared.
    Those people were not known for their sense of humour.

  14. CMCguy says:

    I also feel is highly plausible and frankly admit this well could have been me in grad school (except by the grace of god…) including clutter/abundant solvents not stored well plus the occasion shorts in lab. In terms of sprinklers getting into the Na/Oil bottle I would wonder was not likely in the hood but the sash was left totally open (and should have been an auto response by the chemist to pull down) as I believe most people never get trained on how to properly use a hood with closed as much as possible with glass between person and hazards.

  15. The Iron Chemist says:

    Cue the Benny Hill Yakety Sax music.
    Bottom line, clean up after yourself and try not to spazz out if something does ignite.

  16. Honestly says:

    You haven’t really done chemistry until you’ve had a good fire, or so they say!

  17. Secondaire says:

    There’s absolutely no reason why I should find this funny, yet I do, partially because I saw something similar happen in grad school. Basically goes like this: untrained, inexperienced chemist with large syringe of t-BuLi at odd time of evening equals fire. Fire plus paper towels sitting around reaction equals bigger fire, which then meets acetone bottle, which then meets hexanes (or something), which causes bigger fire, which causes uncomfortable visit from the fire department. It’s the butterfly effect, played out to terrifying, combustible reality.

  18. gogoosh says:

    I also find this plausible. Reminds me of the time in grad school when a small sink fire (metal+water+acetone) was made worse when the post-doc ran past not 1, not 2, but 3 fire extinguishers to grab a broom to beat the flames with. Naturally the broom caught fire and created a huge amount of black smoke.

  19. exGlaxoid says:

    I happened upon a fire like this not long ago. I was walking down the hallway and heard noise. There were three people in the lab, one trying to put something over the beaker, one starring at the fire and one yelling. A very large beaker of ether on a stir plate was on fire, some sort of Grignard quench gone wrong. The specific details were vague. But the fire was growing quite quickly in size.
    I asked if anyone minded if I put out the fire and did it with one puff of the extinguisher (hanging 5 feet away) aimed at the base of the beaker. The one person trying to put it out might have succeeded if they had started sooner, but the fire was getting quickly larger and there were several bottles of solvent nearby in the hood, none of which had been removed during the 30 seconds I was approaching. In the end, no real harm was done, the ether might have gotten some yellow powder in it, and the Tygon in the hood was all melted and black, but no real damage. But it could have quickly grown, due to the lack of training and calm in the response.

  20. Mitch says:

    Thanks for a link to the Chemistry Reddit. 🙂

  21. milkshake says:

    @11: I did not contain the fire – my colleagues put out the flames because all the way in the office they could hear the whooshing sound as the acetone-soaked sink + whole bunch of washbottles ignited in hurry. I panicked and did not go for extinguisher, instead was trying to pull flaming washbottles out of fire and unwittingly was spreading the flames. The accident could have gotten a lot worse – out of control in fact if my colleagues did not react as promptly as they did

  22. Rhenium says:

    I am suspicious, this sounds much more like the sort of thing you give students for “mock emergency” training. Any accident of this scale would have an extensive report written up.
    I’d like some more details before I believe it. University? PI? Year?

  23. Nekekami says:

    And this is why in addition to primary training you also perform repetition and repetition and REPETITION, until all safety procedures become ingrained and reflexive. And even then you regularly check on everything to see that the procedures are followed. Though I guess my military background affects my reasoning….
    One of the scariest things to do as a NCO was to teach new recruits to use hand grenades properly. There’s always someone who wants to see the explosion(and they spanned all over the IQ/education scale….Just proves that IQ != common sense and sense of self-preservation) So, what I did was that I’d call farmers or slaughterhouses if I could get a diseased carcass of some kind, and then I’d hang that from a pole above the slit trench they were all huddled in, make sure all of them were sitting down and watching the carcass… Then I’d throw the live grenade and duck down… Nothing like chunks of meat and entrails and blood to make them understand that you don’t toy around with such things…. And even then there were some close calls….

  24. Anonymous says:

    True or not, it is plausible. I have become a big fan of molecular sieves. They work. Use Them. For water they are all you need. For oxygen all,you need is a good sparge with dry nitrogen.

  25. Dave says:

    Actually this happened across the hall from me when I was working in a certain University in a certain city. I heard a slightly different version of what went on inside the lab, but it is also true that the sprinklers coming on burst a pipe in the utility duct, flooding the duct and shorting out main power to the building too. We had to evacuate by the far stairwell because there was a waterfall down the close one.
    The solvent stills were really there. That PI had them in all his labs, on several floors.

  26. BCP says:

    OK, I’ll admit that I LOL’d after Derek wrote exactly what I was thinking “Poor Nordberg”

  27. jbosch says:

    well that’s exactly why I ban flip-flops in the lab. We don’t have as exciting hazards but even a broken glass can hurt or spilled acid etc.

  28. Colonel Boris says:

    We’ve still got five still between our two labs and I’ve been trying to get rid of them since I arrived. Also trying to get my lab mates to not wear shorts is difficult. They’ve finally relented on the subject of having reaction tags, at least for overnight reactions.

  29. processchemist says:

    Many years ago I (young and stupid) was helping my boss in loading palladium on charcoal (anhydrous) for an hydrogen transfer hydrogenation in methanol performed in a 12 l flask. After obvious problems in dealing with the powder he decided to switch to a suspension of the catalyzer *in methanol*, made in a 500 ml single neck flask. So he charged the methanol, then the Pd, and a flame immediately ignited from the neck of the flask. Instead of putting the flask in a corner of the hood, he panicked and started running around the lab, with the flask in his hands, searching for a way to extinguish the flame. I was running after him, with a stopcock in my hand, and eventually I succeed in stopping the flask with a fast move. Problem solved, but when I recall the episode I always think about Shere Khan in the Book of the Jungle, that running with a burning piece of wood tied to his tail spread the flames all around…

  30. London_chemist says:

    I read this and thought of Norman Wisdom: which will only mean something if you’re British or Albanian…..

  31. sean says:

    Before I was ever allowed into a Lab at UMIST. we had a lecture and 3 points were etched into out minds:
    Accidents such as this meant automatic expulsion from where I studies – not temporary – for ever – no degree of pHd EVER. You just got thrown out. Reflux benzene when student didn’t know it burnt?
    More subtle and less destructive accidents resulted in suspension but the articles on refluxing benzene and distilling HPMA would have got the student out of lab in 30 seconds and out of school within 12 hours.
    How many innocents die because of the numpty in the next fume-cupboard refluxing HMPA.
    I studied 20 years back at UMIST and it was made clear 0 fuck up = expulsion.
    There seem a lot of these dangerous stories. These people go on to research labs???
    0/10 for weeding out incompetence.
    I would like so see how long they lasted at and Oxbridge uni!

  32. Anonymous BMS Researcher says:

    My doctorate was in Biology rather than Chemistry, but the rules can be just as important. At the institution where I did my postdoc, one of the slides in a safety training session my wife and I attended showed what was left of a lab where somebody had stored volatile solvents in a regular fridge. One of my neighbors was the Medical School Fire Marshall (we often took the same city bus to campus); he had vivid memories of that incident!
    Also during my time there, a centrifuge rotor failed, creating an aerosol of very dangerous tropical viruses that infected one researcher. I think that researcher recovered after being quite seriously ill for some time.

  33. ScientistSailor says:

    Totally Plausable. I had an incident in grad school where I was starting a hydrogenation, adding MeOH to catalyst (yes wrong order, I know now) from a graduated cylinder. The thing caught on fire, scared the crap out of me, I dropped the cylinder, now I’ve got 100 ml of MeOH on fire in the hood, with the 4l bottle that I just poured from right next to it. I thought about grabbing the big bottle, which probably would have sent things down hill quickly. Instead, I closed the hood and grabbed the fire extinguisher, luckily, fire burned out w/o big bottle igniting. Could have been really ugly, still gives me chills today.

  34. Jordan says:

    Undergraduate student weighs out potassium permanganate with a metal spatula, then lays spatula on a nice clean paper towel and proceeds to squirt ethanol all over it (from a plastic squirt bottle) to “clean” it. That was a fun one.

  35. London_Chemist says:

    I would agree with some of comment #31–especially UNDERSTANDING. There does seem to be a lack of understanding of the basic principles behind a lot of accidents/incidents. From my post-doc: a PhD student got an undergrad to do a prep for him. Birch reduction and quench with electrophile. Written prep given to undergrad used octyl bromide but PhD student told him to use benzyl bromide. No change to temp or rate of addition. Result? Benzyl bromide all over lab and floor, entire building evacuated, student in hospital, because PhD student “forgot” (or never knew!) that benzyl bromide is considerably more reactive than octyl bromide.

  36. MoMo says:

    Where was the graduate advisor? You dont let rookies play with such dangerous chemicals, and the fact he was wearing shorts tell that he wasn’t properly trained.
    That student was set up to fail by his advisor, and the law should recognize such neglect.

  37. YinzerChemist says:

    I can confirm this story; every word is true. I was in the building at the time, and witnessed the final moments of this as the building was evacuated via an exit that was in view of the lab. The student was/is under an near-absentee advisor who is 95% instructor/5% research.
    There are several advisors in this department who are dead weight and this could have happened in any of those labs. I would say there are at least 5 faculty who are completely absentee and simply suck money out of the department coffers to keep their ‘research’ going. It’s a sad situation, as there are several other faculty in this department who are top notch faculty.

  38. GladToMoveToProcess says:

    Reminds me of something that happened in the sophomore organic lab when I was an undergrad. We were doing a careful fractionation of something, with heat supplied by oil, in a beaker, heated with a bunsen burner (this was in the mid-60s). One student filled the beaker too full, and when the oil expanded, it overflowed and caught fire. The TA rushed over with the extinguisher, aimed it at the beaker and let ‘er rip. The blast of CO2 knocked over the ringstand and the apparatus, adding to the chaos. Great fun to watch!

  39. Gaspode says:

    By now we removed all our stills from the Lab due to saftey and this:
    turns out Molecular sieves are better than any sodium/calciumhydride/instantfire.
    For most reactions moisture ist not the limiting step anyway, a very good example can be found here for Samariumiodide:

  40. Dogbertd says:

    I’m a biologist, but back in the day we often had to make our own solutions (including scintillants, etc. – what larks!) I was a technician in a lab where my colleague was making chromic acid for cleaning glassware. Unfortunately he forgot (or didn’t know) about which way round to mix the sulfuric acid to sodium dichromate, and the resulting exothermic reaction sent him off to casualty (aka the ER.) I remember being deeply impressed that the acid had eaten through his leather boots.
    In later years I’m still astonished at the number of students who don’t know that you should add concentrated acids (slowly!) to water, and not the other way around.

  41. Lyle Langley says:

    Sounds like something that would happen in my good friends, Professor John Nerdelbaum Frink, Jr., laboratory. Riboflavin!!

  42. Dr. Demented says:

    @ #40: Here’s a convenient mnemonic (helps if you’re from Boston): Do what ya aught ta, add acid to watta.
    Taught to me by my very first freshman chem TA, and I still remember it 20+ years later.

  43. Derek Lowe says:

    Or, in the Arkansas/Texas/Oklahoma declension, “Do like you oarter, add acid to warter”. That accent doesn’t obtain in the whole range, but you do come across it – one friend of mine described himself as coming from the “Damaged warr can cause a farr” part of Arkansas.

  44. Anonymous says:

    As a polymer chemist, I’m disturbed at how often I see academic papers where someone used freshly distilled methyl methacrylate, styrene, etc. We never try to distill monomers in industry; it’s way too dangerous. I suspect a lot of this stuff is a holdover from the old days when the manufacturing and QC of chemicals wasn’t tightly controlled – in 2012, if Aldrich claims something is 99.99% pure, it probably is!

  45. David Formerly Known as a Chemist says:

    A company I worked at back in the 90s had a very similiar incident, though not quite so cartoonish. A chemist was washing his glassware in a wet sink using a squirt bottle of acetone. A spatula had a small piece of sodium metal on it, which ignited the acetone/water mixture that was in the sink (by the way, it was a hard plastic sink, like the kind you might have in your garage or basement). Attempts to put out the fire with an extinguisher failed, the plastic sink started burning (a very hot fire), the flames quickly spread and nearly a quarter of the building burned. Sounds slapstick, but that was a scary day. Small mistakes can escalate very quickly!

  46. Anonymous says:

    Definitely true. I was friends with the person this happened to while in grad school. The funniest thing about this is that afterwards his feeling was that wearing shorts actually may have saved his legs from worse damage since it didn’t hold the burning isopropanol tight against his legs. I know he had to wear compression bandages for at least a number of months to help minimize the scarring.

  47. sciencemonkey says:

    @44: I also am a polymer chemist, and at least for RAFT and ATRP polymerizations I never bothered distilling monomer. Gravity filtering over some silica gel (or inhibitor removal packing if you are fancypants) was good enough to remove inhibitor.
    On the topic of polymerizations, my supervisor would always remind us of the danger of runaway polymerizations (Trommsdorff effect), and how a gelled 3 gram polymerization may get really hot, but a 100 gram run could blow out a fumehood. I never witnessed such an accident. I did do 20 gram (plus 20% solvent) runs of well-behaved RAFT polymerizations.

  48. Peter says:

    Many solvents can be dried efficiently with a cheap, convenient and very SAFE dessicant: molecular sieves See J. Org. Chem. 2010, 75, 8351–8354. For many purposes this is sufficient. But people tend to think they need dry solvents for every reaction. Unnecessary, waste of time and above all, in inexperienced hands, very dangerous.

  49. Slurpy says:

    So three people claim to know about this, and yet no one is willing to say where it happened? Right. . .

  50. Anonymous2 says:

    I can also confirm that this is truly happened. I think we are all avoiding the name of the school to protect the student.

  51. ech says:

    I’m glad that as a Physics & Astronomy student, the most dangerous stuff I worked with were radioactive sources for calibration of instruments. And we were very well trained on how to use them.

  52. Anonymous3 says:

    dichloromethane+sodium and isopropanol+potassium hydroxide?
    2 possibilities:
    – this is an urban legend described by a NON-scientist
    – the school has major problem with the teaching of basic chemistry: please close the department or change to Biochemistry.

  53. Aston_B says:

    This is not funny but in fact a pity!I think this is the way each and every accident turns ugly. An accident may start with a minor note but turns ugly with human errors. We have that tendency of panicking and making a serious situation more worse. What a pity it is!

  54. Larry P says:

    I was working on an experiment in a college chemistry lab. The lab was set up with eight rows of benches. I was working on the far end and there was an exhaust hood against the wall at the other end. For some unfathomable reason the lab instructor dropped a small piece of sodium into the hood drain and ran some water apparently not noticing that there was an uncapped bottle of acetone and a sealed can of ether in the hood. The acetone caught fire and the instructor shut the hood and yelled get out. Shortly after that the acetone bottle broke and the flames spread to the can of ether. The instructor then yelled get down. I dove past the end of the bench helping a female student to the floor at which time the ether exploded shattering the hood glass which caused some minor cuts on my legs that were still sticking out into the aisle. The fire department showed up and what I remember most was their concern that there was a 55 gal. organic solvent waste drum in the lab. I ran into the instructor a year later and he had cuts on his face. I asked what had happened and he said it had something to do with frozen ozone.

  55. OmegaPaladin says:

    Let’s me honest here. There were safety deficiencies there, but half of armchair quarterbacking here is completely useless.
    I love the comment on MSDS. Assuming the (M)SDS is competently written (which is rare, especially with the pressure to get new GHS-compliant SDS out the door), it only provides you with hazard info. 95% of the time it is just boilerplate that does not address the true level of hazards present. Besides, I don’t think there was a failure of hazard identification here…
    Chemistry laboratories quite often do things that aren’t amenable to drills. Emergency response is more about principles than a specific drill. Contain, Alert Others, Extinguish if Possible. I had an incident where I was cleaning up a sodium spill with ethanol when it caught fire. (Forgot that it was not absolute ethanol – might have also been a water droplet) I told the people in the area to get out, then went for the extinguisher. Took it out nicely. It was certainly a hair-raising experience.
    Also, I recommend full-length aprons for hazardous work in torrid conditions. Give me shorts and a sheet of chemical resistant rubber over long pants any day.

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