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Solo Chemistry

Many US readers are off today for President’s Day – I nearly did what I actually did do a few years ago, and forget about the holiday entirely. I came in to work that year, noted that there was no one around, and realized that you know, this was one of those holiday things, wasn’t it? Hmm. You can actually get quite a bit of work done under those circumstances – I did for the morning, until my wife and family joined me for lunch and I actually started taking the holiday as planned. But when I was on my post-doc in Germany, more than one German holiday caught me by surprise. Sometimes I would take the day off, and sometimes not.

Bench work in chemistry is not necessarily a good idea under those conditions, though. I don’t see much problem with (say) taking advantage of the NMR machine being totally open and so on, because you’re unlikely to be injured setting those up. But alone in the lab is no time to run that big diethyl zinc reaction (or most any big reaction, come to think of it). This rule is pretty well observed in industry, where chemists are actively discouraged from doing bench work in the off hours, and most especially so when alone. Academia, though, is a different matter.

I well recall being up in the labs at some pretty cruel hours, often (but not always!) alone. Sometimes there would be a Japanese post-doc around who’d never really gotten off JST, or some other night owl several labs down the hall, but if something bad had happened, it wouldn’t have been easy. I think the dumbest thing I did in that line was going in at 2:30 AM to cool and vent a high-pressure reaction. It was a thick-walled glass tube, rather large, and I ended up lassoing it out of a homemade vertical tube furnace with some copper wire, and dropping it after it was pulled up halfway out of the thing. Clang! For some reason, it didn’t actually crack and blow up. I had a safety shield up, but you don’t want to have to test those things, do you? That made it clear even to me that being up there at that hour, alone, messing around with something that could explode (especially if you were, ahem, enough of an idiot to drop it), was not such a wonderful idea.

So anyone out there working solo today, be careful. Save the big organoaluminum workup for when there’s a crowd around to watch it go all over the hood, and postpone opening up that cylinder of anhydrous HBr. A twenty-four hour delay is unlikely to hurt you, but something else might.

35 comments on “Solo Chemistry”

  1. luysii says:

    Back in the early 60s the only time you could hear the Messiah (radio was all we had) was around Christmas, somehow always late at night. Schleyer did have a record player in his lab, but none were around in grad school.

    It was a fringe benefit of working late.

  2. Lab Shadow says:

    That brings me back to the evening I blew up three heavy walled glass pressure vials due to heat shock, at 19:00 on a Sunday. Makes you happy you have a blast shield, heavy gloves, and goggles. Took me hours to find all the pieces. Yeah, maybe working with things that might explode off hours isn’t such a great idea.

  3. Eric W. says:

    I did my first Swern reaction alone, late at night once. I figured if I screwed up and smelled up the whole building, at least I’d minimize the number of people I’d annoy. Thankfully, I didn’t screw up.

  4. Anon says:

    Back in my PhD/postdoc days (or rather nights), I was one of the 3 regular night owls. Generally we’d wake up and get in just in time for lunch at 1pm, and work until the wee hours, 3 or 4am, sometimes until it started getting light outside!

  5. Mark Thorson says:

    I come into work early on a Monday, and my boss says “That chemical you ordered is really nasty stuff. Goes right through gloves. Where’s the MSDS?”. He’d been working alone over the weekend and had some chemical burns on his hands.

    “I didn’t order it. Zlata ordered it. We don’t have the MSDS. If I had ordered it, we’d have the MSDS.” I said.

    If my boss wasn’t a vice-president and co-founder of the company, we could have had a lawsuit on our hands. As it was, he just had some burns on his and after much difficulty we got the MSDS. It warns right in there that it can cause delayed-action chemical burns. (It was a chemical very similar to hexamethyldisilazane.)

    We played fast and loose in those days, to my dismay. I was instrumental in starting up the safety committee at that company, by writing up a memo listing serious safety hazards in every department. Some were minor, but others were mind-boggling. Nobody had ever removed the protective plastic caps from the fluorine sensors in the excimer laser room. There was a volumetric flask being used to store a blue liquid marked (on a piece of masking tape) Cyanide Poison. Nobody knew what was in that flask or where it came from, other than that it was probably left behind by one of many employees no longer with the company. We had equipment that generated hazardous gases that had exhaust ports for those gases which were never hooked up — they just exhausted to the room. Technicians in a couple labs were visibly disturbed when I pointed out the hazard.

  6. Hap says:

    I thought that not having very many people around when she was working (at least when she was doing the ill-fated t-BuLi reaction) was what helped get Sheri Sangji killed.

    1. John says:

      From what I understand it was a combination of not being fully briefed on what to expect with the organolithium reagent and not being supplied with proper fire-retardant gear. She was wearing a sweater, no lab coat, that went up in a flash and her coworker tried to smother the fire with a cotton lab coat IIRC. It was a Monday during the winter break as well so I’d imagine there weren’t too many people around. The biggest failing was no fire-retardant lab coats and seemingly no warnings about t-butyl lithium. Sheri wasn’t an extremely experienced researcher but she wasn’t a green lab hand, a small amount of effort towards lab safety and that accident could have been avoided or at the very least minimized.

      1. Piotr says:

        Sheri Sangji was not an experienced researcher. But everybody with a chemistry major should understand the dangers of handling reagents like t-BuLi. According to some sources she was a good student: “She majored in chemistry and by all accounts she excelled, earning outstanding grades and working in the lab of a professor.” –
        Every undergraduate laboratory course at every university I’ve been to has strict safety rules. Nevertheless, she decided not to wear a lab coat when handling a pyrophoric reagent and left open bottles of flammable solvents around. That is against everything she had learned while studying chemistry and she is the one to blame, and to some extent other people present at that time in the lab for not pointing out that a lab coat is necessary when doing organic synthesis.

        1. fajensen says:

          Teenagers, even intelligent teenagers, are just stronger children and being children they will keep doing stupid things – randomly – until they grow up and learn (The cherry on that is that the teenage-hood of today seem to grind on well into the 20’s for most people).

          It is just not enough to have “strict safety rules” for “bum-cover” one also have to keep explaining them and enforcing them until they eventually stick. “She should have known …” will not cover ones ass at the inquest, never mind that an accident like that is something I do not want to see, ever.

          Lets hope they do better than the ritual sacrifice of the supervisor.

          1. DCStone says:

            I’ve read the summary of the health and safety investigation into that incident. Apart from the lack of safety gear (students weren’t apparently provided with lab coats – the Chinese postdoc in the group brought his own in), the biggest issue was that she had been trained to follow a totally incorrect procedure. Not only that, it was completely contrary to the instructions provided by the chemical supplier. And to make matters worse, everyone in that group who used that compound had a reference to the supplier’s safety procedure in their lab notebooks despite the fact that none of them followed it!

            So no, this wasn’t just the case of a rash teenager not following instructions, which is why the supervisor ended up in court.

  7. Mmm…fond memories…early nineties, I was finishing up a PhD in radiochemistry – not your usual, run-of-the-mill 14C or tritium stuff, but shortlived 11C: both high-powered betas AND 511 keV gammas, and multi-Curie amounts at that. Since I was gainfully employed during day-time making nuclear medicine preps for patients, only the 8 pm and onwards shift was available for research, so there I was, running the cyclotron, all alone, dumping a Ci or two of [11C]CO2 into whatever I needed to do, and ever so often making labelled methane by mistake….methane not being a terribly easy thing to contain, it ended up in the giant expansion loop to cool off – with a 20 minute half-life, a few hours of ‘storage’ is all you need for garbage disposal.

    No, this is not large-scale chemistry – at most a few micrograms of labelled stuff (BTW, this makes methyl iodide a brilliant alkylating agent, since you can reach a zillion-fold excess of nucleophile…), but pretty risky nonetheless. Rapid labelling chemistry often means extreme reaction conditions, and use of concentrated and highly reactive ‘whatever’ is the rule, as well as high-pressure reactors (even if small ones…). All in all, we got our GMP certificates, but no-one even brought up chemical safety (radiation safety then was as good as it is today, methinks), and certainly not for late-working research work.

  8. b says:

    I can share a similar experience from grad school. I was in working alone late one night, was very tired and not thinking clearly. As routinely happened, the inner tube of my high vac trap was clogged up with frozen solvent. I closed the valve to the pump, lowered the liquid nitrogen Dewar and began going at it with a heat gun. However, this time I never opened the system to the atmosphere, and eventually the gases created enough pressure to blow the valve at the top of the trap into a million glass pieces all over my hood. My face should’ve been full of shrapnel, but by some act of the chemistry gods, I was untouched.

    It was at that point I decided I would never put myself in that situation again. Doing chemistry while exhausted and alone is incredibly dangerous.

  9. Fluorine Chemist says:

    This is the main reason why I didn’t have to do late hours too many times during my PhD. Fluorine was strictly regulated only to be used during the day on weekdays, the main reason being that the local ambulance service only guaranteed 15 minutes response time during these periods.

  10. CatCube says:

    I can see from reading your blog over a long period that university environments can be rather cowboy when it comes to safety, but I’m surprised that industry doesn’t enforce, rather than encourage, a buddy system. Is there normally building security that they could require you to notify when you’re working alone?

    I’d think that doing a reaction that can evolve something toxic would at least require somebody else outside the room (even doing their own work) who knows what’s going on, so if things go completely sideways and you get overcome there’s someone to a) help and b) knows not to rush in and get overcome with you.

    1. Mark Thorson says:

      I’m sure that would happen at a big company like IBM, but at a small start-up it would depend on management. Corporate culture flows from the top down, and if the executive suite cares more about getting the job done quickly than safely, safety may fall by the wayside.

    2. Some random chemist says:

      That would not be an issue at academia. When I was in grad school in late 80’s (chem. dept. in an Ivy league school), we had about 20+ people in the lab. With exception of a few senior postdocs, everybody (certainly all grad students) worked until 12mid-1am anyway. There was no need to enforce a buddy-system, lol. Your buddies like yourself were always there.

    3. One of the Cowboys says:

      I work nights and weekends alone because that is what it takes to get publications and grants: time away from the trivial bullshit that makes up 80% of an academics life. My former colleagues were always on my case about how that was dangerous but, since they couldn’t lucidly explain what I was doing that was dangerous, I concluded the just didn’t like to be made to look bad.

      This country was built by people taking risks, some reckless but most calculated. Putting rules that eliminate all lab work alone is a good way to get rid of the movers and shakers. I suppose my former colleagues are happier now that the lab is dark and lonely, the better to match their pathetic little lives. I left after my 10,000 hours without having had an accident. On to bigger and better things.

  11. Nick says:

    I think in Europe and Australasia, this type of thing is being heavily cracked down upon – both working late and working alone. I know at my Australian department, swipe card access stops at 9 pm weekdays and 6 pm weekends, meaning people physically can’t get into the labs. Similarly, if you were caught working alone, you’d be in trouble.

    My experience of North America says that safety (in academia) is taken far less seriously, especially working late/alone. (Most) Professors in North America seem to expect their postdocs/grad students to work far far more hours, so these things are probably linked.

    1. SSG says:

      I straight up wouldn’t take a job in a department that didn’t allow 24/7 access to my own experiments. Would not work there.

  12. Ed aka swampyankee says:

    RE: Industry.

    I have a story about that.

    I once worked for a major aircraft manufacturer. One night a guard were doing a walk-through and found a light on where no one was expected to be working. At the desk, he found an engineer, slumped over. The engineer was non-responsive, so the guard called for assistance and started CPR. Didn’t help: the engineer had died of a heart attack. Shortly after that, a rule came down that no one was allowed to work past a certain hour without explicitly being directed to do so by management AND at least one other person had to be in the same area AND security had to be informed.

    Yale had a recent fatality where a student was killed while operating a lathe while alone in a campus machine shop. (; this is not problem limited to chemistry labs. (She was strangled when her hair caught in a lathe; had somebody else been there, she probably would have lived).

    1. Design Monkey says:

      Sloppy work habits by said student. Long hair and lathes don’t mix. Not alone, not in group, not at night, not at day.

      If one has long hair and has to work on lathe – tying hair and hiding them in cap is mandatory. More freaking mandatory than safety glasses on chemist.

      1. Ed aka Swampyankee says:

        Yep; long hair and lathes don’t mix. Nor do lathes and rings and wristwatches. If your parent had been, say, a machinist (my father was a toolmaker), you would know that. If your father was a lawyer or a tax accountant, you wouldn’t. Unless the school made a serious effort to inform the students of this, Chances are that none of the student population at Yale would know this — children of factory workers aren’t well-represented in the school’s demographic — and unless the safety issue was really hammered home, they wouldn’t get it.

        I also knew an engineer who managed to cut off half his thumb (long sleeves while working on a car with the engine running) and two of his fingers with a circular saw (actually, he cut the same two fingers off *twice*; they were re-attached and he cut them off again, after which they were reattached again. The surgeon advised he stay away from power tools)

        The dangers of machinery are not known by instinct. Show a kid a snake or a big spider, and they’ll pay attention to the potential danger. Show them a lathe? The caution has to be learned.

    2. Isidore says:

      I wonder where you draw the line. It’s one thing to recommend or even require that people carrying out “dangerous” experiments not be alone in the lab, but makes no sense to prevent someone, who wants to spend an hour or two doing paperwork at one’s desk after everyone has left, from doing so. And how about Dereks’s point using an NMR or other instrument during non-busy hours? Surely, one could die from electrocution from a power supply or even the AC outlet if nobody is around to help.
      Some years ago a former colleague, who had a mid-level managerial position with a major pharma company, had traveled from the US to the UK for a meeting. In his hotel room during the night he suffered a stroke and was found dead the following morning, after he failed to show up for a breakfast meeting and his room phone did not answer. I was told by one of his family that if he had been taken to hospital as soon as he had the stroke he might have survived. Should companies require employees who travel on business to share hotel accommodations to prevent this sort of thing? Your employer cannot be your nanny,

  13. Chimaera says:

    Here in Ireland, my university has pretty strict protocols for out of hours working. You need to apply for a permit, signed off by your supervisor and the chief technician for the department, before you can even think about working after 18:00. On top of that you must have a buddy and you have to sign a security log.

    1. Da Vinic says:

      Here in my building in the UK this would lead to an immediate revolt. There’s a reason us biologists need 24/7 access….

  14. dearieme says:

    Head of Department: are you prepared to chair the safety committee?

    Me: are you prepared to have every lab closed for a fortnight while it attends to my complaints?

    Upshot: go on, guess.

  15. slava bernat says:

    True, official days off in Germany were countless for me and often unexpected, I never managed to take all my official paid holidays in a single year.
    From working alone in the lab the only accident that I remember was force-opening of the old Schlenk flask of oxalyl chloride and spilling it all over my gloves and lab coat accompanied by inhaling a healthy dose of HCl. The regulations about working alone in that lab weren’t very strictly enforced though.
    In the US it’s enforced in a different way: everyone should work crazy ours so nobody ever works alone in the lab!

  16. Bagnar says:

    Second day of my Ph.D, 7 p.m.
    The student next to me splash a certain amount of sulfuric acid on her face. Eyes saved by safety specs… Quite shocking by the way. The syringe had no lock and unfortunately, due to pression, happens what happened.

    Third day of my Ph.D, 8 a.m.
    Fire on the THF distillation upstairs.

    Since then, nothing happened ! I’m glad I survived the first few days :p

  17. Shion Arita says:

    Often times the only reason I know about minor holidays is that the lab building is locked during daytime hours.

    Actually as a general statement it’s pretty hillarious: the university custodial staff keep happily unlocking and locking the doors at like 9am/6pm, even though most of us PhD students follow nothing close to that schedule. Cargo-cult openings and closings I guess.

    1. KevinH says:

      I remember having the same problem with cargo-cult schedules during my PhD. Not only did they lock the doors, but when we moved into a newly-constructed building we discovered that they also had the lighting on automated timers–at the stroke of seven o’clock, the overhead lights in the office and lab clicked off. It took several months of complaints before the timer was pushed back to 11pm. (As an added bonus, the lights were on a poorly-designed “zone” system. Someone trying to save energy by turning off the lights in the photocopy room across the hall would also inadvertently douse the lights in our lab.)

      Meanwhile, I still occasionally made use of an instrument in the old building. I needed long blocks of time, and it tended to be free at night–but the elevators were locked down at 6pm (after that time you could get out but not back in). So I would go on “camping trips”. I loaded up a backpack with all my supplies and notebooks, along with snacks, sandwiches, and caffeinated beverages. I’d arrive and set up my experiment by 5:45pm, put in an 8- or 10-hour “day”, and then head home and sleep until noon.

    2. SSG says:

      I work in the US and actually didn’t know President’s Day had been and gone till I saw Derek’s post today! Or, I saw it on my calendar but wasn’t aware it was a day that people take off (international). Strikes me as funny!

  18. Myma says:

    @Mark Thorson – Speaking as someone who did intern at IBM research, I can confirm that the safety guy there was quite diligent. I was working with 2 known carcinogens, and that guy visited me Every Day to make sure I was using my PPE properly and disposing of everything according to his directions.

    However, my grad school experience in a big research university was decidedly mixed. I managed to explode a glass dessicator, unharmed, at some ungodly hour in the am. But the kids in the next building using HF were under extremely strict rules: in glass, no label, couple other rules = swipe card access off = no more thesis research = no more grad school for you mistah. It only took 1 idiot every decade or so to break the rule for everyone to pass around the story that they really do enforce the rules, and yes you will be kicked out.

  19. Peter S. Shenkin says:

    Then there’s the time the 1/2-inch-thick sapphire window failed on my high pressure bomb at about 3000 atm. However, it contained a liquid system with a total volume of about 10 ml, so it just made a bang. It did scare the s**t out of me, however. I was getting ready to put the bomb into the Cary-14, and the spalling sapphire made kind of a dusty stain on its outer finish. But I was glad it wasn’t in the machine when it blew.

  20. burn-free says:

    Our department were approached by a company selling Diphoterine spray, for use on chemical burns. Eventually it saw use, and proved remarkably effective in completely eliminating the burns from a sulfuric acid splash to a students face, they are unscathed today. It has since been embraced by the department, with a bottle at every first aid kit, and has prevented numerous students from more serious burns. I know I sound like a salesman but I’m just a student grateful for this product, and would recommend other safety committees look into bringing this product to their labs. Link on my handle.

  21. Me says:

    I’ve worked for my share of narcissistic sociopaths (academics) in my time. All those hours I put in for a prof who still hasn’t bothered to publish my nanuscripts >10 years later. Plenty of lone working, the dermatitis on my hands, the frazzled sense of smell, the scars from various burns and deep cuts. And now I’m not even a chemist any more and earning tonnes more than I would as a chemist. Makes me wonder whether I’d do it all again if given the chance

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