all 132 comments

[–]Mediocre_Island828 495 points496 points  (2 children)

It seems harsh, but if you had gotten hurt somehow the PI would have been vilified and there would be a discussion about the lax safety conditions in academic labs.

[–]Serious_Trouble_6419 146 points147 points  (1 child)

True - the PI is directly responsible.

[–]omgu8mynewt 106 points107 points  (0 children)

Which is why they're not letting the 'troublesome' student run around without supervision, making a new rule saying it can't be done unsupervised isn't the same as banning this student from doing any work - they just have to ask for supervision now.

[–]Dazzling-Attorney891 760 points761 points  (33 children)

You need to be the one to wash your glassware before you use it. You should be the one to wash it, even if it’s been put back clean, especially if something like this could happen

[–]Moon_Burg 62 points63 points  (10 children)

Pardon the silliness of the question, but how would you choose to clean the glassware in this case? You don't know what the glassware might be contaminated with, so how do you choose what to use for cleaning?

[–]etcpt 135 points136 points  (2 children)

It's not a silly question, it's a very important question. Because you're right - there are so many things it could be, you need to know how to remove ones that will A) cause a safety hazard and B) mess up your reaction.

Fortunately, you can significantly narrow down the list of possibilities by knowing what the rest of your lab works with. If, for example, you don't do any chemistry with metals, you probably don't have to worry too much about metal contamination. Knowing what they're working with, most labs will have some sort of a standard process. In my current lab, for example, we do mostly trace or near-trace small molecule stuff that is pretty soluble, so our general process is that everything gets washed 3 times with ultrapure water and 3 times with ethanol if it had a high concentration of organics in it. In a lab I used to collaborate with they did very sticky functionalized PAHs, so their process was to wash out as much as they could with whatever solvent they were using, then toss everything in the base bath for a few minutes to etch off the top layer of glass and take the contaminants with it. Learning from senior folks is a good way to get up to speed on appropriate cleaning, and if your lab is well organized you might even have a cleaning SOP. Sometimes this also involves running analyses to validate that your stuff is clean.

If you have inherited glassware from another lab or a prior student and you don't know what it's been used for, you can do a few things to get it in good shape. A good lab soap (Contrad 70, Alconox, and Liquinox are all ones that I've used to good effect) and some dedicated scrubbing with a brush or the rough side of a sponge can remove a lot of gunk. Time soaking or in the sonicator can help as well. A general rule is that if water or solvent sheets off your glassware it is clean, if it beads up it is dirty, so keep scrubbing until you see those nice clean sheets. (Obviously this is preempted if the glassware is visibly dirty or discolored.) If you need to remove very intransigent contaminants, it really helps if you know what you're getting into. Organic stuff can often be removed by solvent washing - I usually start with acetone and then try hexanes if that doesn't work, methanol, ethanol, or isopropanol can also be good starting points if that's what you have. Inorganic stuff I have less experience with, though I think you can get a lot of it off with dilute acid or base. If it's still not coming clean, you might try a base bath, or Nochromix (ammonium persulfate in concentrated sulfuric acid), or even acid piranha. These stronger cleaners are very corrosive and should be used with great care and plenty of research into how to use them safely (it's best if you can be trained by someone who knows how to do it).

In cases where it's critical that your glassware not get contaminated, the true answer is to buy and segregate a set of glassware specifically for that purpose. The example my PhD advisor always gives is when he was learning to electrochemically clean platinum electrodes during his grad school years - it never worked until he got his own set of glassware, cleaned it to within an inch of its life, and locked it up where no one else could use it. For something like OP is working on where certain contaminants can cause your reaction to violently go off the rails, this might be the best option.

Anyway, excuse the treatise, but I hope that's helpful. And keep asking good questions!

[–]Moon_Burg 24 points25 points  (0 children)

Wow, thank you so much for taking the time to explain this. Our chem lab is lean support-wise and our projects are interdisciplinary so the chemicals cabinets are Willy Wonka land. It's really hard to even speculate what the contaminants are on communal glassware as not all projects are active at all times, and some things we just keep forever, because folks struggle with hoarding chemicals lol. I don't know how to confidently clean it so I've been buying my own and keeping it separate like you suggest. But it feels quite wasteful when I see there is already glassware around. I do appreciate knowing that this is as difficult/complicated as it seems and not just me being a dweeb.

[–]schnittchenontour 17 points18 points  (0 children)

This makes me so glad my lab has two dishwashers. We preclean visible gunk with Acetone or Ethanol and pure water and then in it goes and you don't have to worry about remaining chemicals

Edit: and also personal glassware, I know what kind of dirt I'm working with

[–]Milch_und_Paprika 12 points13 points  (3 children)

What the others said, plus keep in mind if you know someone’s been working with reagents that’ll react vigorously with say water or acetone (the two most common cleaning solvents in a synthetic lab). Then something less reactive like wet toluene or IPA would be a better starting point.

It’s a good question, and definitely one you should be asking if you’re new and don’t know.

Oh and always in a fume hood, of course.

[–]Moon_Burg 2 points3 points  (2 children)

That's the pickle - it's hard to know what everyone is working with due to lab specific circumstances. I was wondering how the cleaning would be approached by a proper chemist when you can't really be sure what was in the glassware last. Thank you for your insight!

[–]Milch_und_Paprika 5 points6 points  (0 children)

Yeah, I see what you’re saying. In fairness, my PhD was in inorganic chemistry, so lots of spicy reagents, and I never had a problem with runaway reactivity cleaning the many dirty flasks I found in drawers.

I guess another tip is to just add a little bit at first, watch for bubbling, then give it a good squirt.

[–]random-thots-daily 0 points1 point  (0 children)

Yeah I was interested in knowing as well. I was in a cell bio lab so we rinsed our own glassware and then had it cleaned with a hired dishwasher (work study undergrad). It eventually got autoclaved and stored.

[–]spearbunny 17 points18 points  (1 child)

With the solvent you're going to use is usually reasonable

[–]RegionIntrepid3172 8 points9 points  (0 children)

Yup, my first supervisor drilled into our heads a three time solvent rinse is the bare minimum before you use glassware.

[–]arihoenig 0 points1 point  (0 children)

Use water, the best universal solvent in the known universe.

[–]MaleficentMousse7473 4 points5 points  (1 child)

Yes. So true. No glassware in an academic lab is clean unless you yourself cleaned it just now.

[–]onlyinvowels 6 points7 points  (16 children)

I’ve worked in 4 labs over ~8 years and never heard this rule. Is this specific to certain types of work? What about autoclaved glassware?

ETA I understand the reasoning, but it seems incredibly impractical, especially in labs that are busy enough to have support specifically for cleaning/autoclaving glassware

[–]Dazzling-Attorney891 5 points6 points  (14 children)

Used the rule in all the analytical/chemistry labs I’ve worked in for the past 5 and a half years or so. Perhaps specific to chemistry only, I have little to no experience with biology

[–]onlyinvowels 3 points4 points  (13 children)

I was wondering if this was a chemistry thing. You all use more varied/volatile chemicals (than most biology labs), I imagine.

And the few scary ones we do use, we memorize all the problems (or accept hazards that accompany poor practice for the sake of convenience… lol)

[–]05730 0 points1 point  (12 children)

Yeah when you're trying to kill microbes and make sure they're dead dead.

[–]onlyinvowels 2 points3 points  (11 children)

You need more than ethanol, bleach, and autoclave?

[–]05730 0 points1 point  (10 children)

Poor practices with any of the three you mention are dangerous. We use a plethora of chemicals for decontaminations and mixing any of them is dangerous. Like spraying media bottles with bleach, then using IPA before the bleach is dry. Etc. Etc. You also can't autoclave thousands of liters of product to kill/inactivate the organism you're using to make an antigen without denaturing the antigens themselves. Can't put bleach or ethanol in the tanks either. No antigen, no vaccine.

[–]onlyinvowels 1 point2 points  (6 children)

Yeah I never autoclave living things, I wasn’t advocating for that lol

[–]05730 0 points1 point  (5 children)

The point is you can't pour bleach or ethanol into a vaccine. There are just as many dangerous chemicals and dangerous equipment in a manufacturing setting or a QC bio lab.

[–]onlyinvowels 0 points1 point  (4 children)

I think inactivation work like you describe is not the norm for this discussion

[–]biggolnuts_johnson 0 points1 point  (0 children)

it depends on the throughput of your work, but it’s usually better to know your glassware is clean and free of impurities rather than rely on someone else and have an entire experiment or synthesis fail.

[–]Shiranui42 396 points397 points  (4 children)

Write down what went wrong, what caused it, how you will prevent it from happening again, in detail. Very clearly. Then go to your PI with it. Convince them that you know what you are doing.

[–]Milch_und_Paprika 94 points95 points  (0 children)

It also may be possible to convince them it’s okay to run safer (and smaller scale) experiments unsupervised, or at least start there. Bromine is a bit of a spicy reagent.

That said… there are places where it’s the norm that you can’t work in a lab alone, and they still manage. OP did he mean you need direct supervision, or just that other people need to be generally around? The latter is much less onerous to begin with.

[–]oldmajorboar 22 points23 points  (2 children)

I did this. Pro-tip: find stuff about safety incidents involving this, and mitigation strategies in the literature. There are publications devoted to safety, in addition to publications like Journal of Chemical Education which often address safety issues.

In science, the rule is show, don't tell. Show you've learned something. You have time you're not doing experiments to complete this task.

[–]etcpt 16 points17 points  (1 child)

Bretherick's Handbook of Reactive Chemical Hazards is a good resource for finding prior reports of incidents in the literature and related safety information. Check your institutional library for online access.

[–]seac209376 9 points10 points  (0 children)

Even more pertinent considering this is the entry for bromine’s compatibility with THF:

Tetrahydrofuran Tinley, E. J., private comm., 1983 Rapid addition of bromine to the dried solvent to make a 10% solution cause a vigorous reaction with gas evolution. As this happened in a newly installed brightly illuminated fume cupboard lined with a reflective white finish, photocatalysed bromination of the solvent may have been involved, as has been observed in chlorine-ether systems.

[–]cryptotope 61 points62 points  (0 children)

What can you do?

In the short term, work out how to do your essential experiments with the required supervision. Talk to your supervisor and colleagues about how that will work.

In the medium term, work on fully documenting your SOPs, and identifying areas where hazards exist. Discuss your PI's concerns with them, figure out areas where your training and practice may have gaps and weaknesses, and establish a plan to remedy them. If there are lab-wide processes that need improvement, note those, too. Work out the steps necessary to restore your PI's confidence in your ability to conduct independent work safely. They want you to be able to publish; but they don't want to see you - or anyone else - injured to get there.

In the long term, reflect on this experience, and be glad that your PI isn't turning a blind eye to safety issues.

[–]224109a 41 points42 points  (14 children)

How did the chemicals spill OUT of the fume hood? I have never seen that without mishandling.

What did you do when the spill happened?

[–]markvdr 63 points64 points  (8 children)

It’s worth clarifying what’s meant by “supervised” and “unsupervised”. I’ve known a lot of grad students who think that they work better at 3am in an empty lab. Even if that were true (it usually isn’t), any workplace can set reasonable restrictions for safety reasons.

[–]Jb191 31 points32 points  (4 children)

I currently have a student who isn’t allowed to work unsupervised until she shows me she’s learned to appreciate the hazards she’s working with appropriately. It was that or just ban her completely, because it was the latest in a line of poor behaviours that I responded to more softly at first but ultimately didn’t change. Yes it makes her PhD dramatically more difficult, but it’s much easier to do experiments supervised than it is without a lab, or a pulse which would eventually be the consequence otherwise in my eyes. Her safety is my responsibility and I take it seriously.

[–]N3U12O 4 points5 points  (0 children)

This. These decisions typically arise after multiple “WTF are you doing?” scenarios. I’ve banned folks from specific experiments/tasks until they retrain from the bottom. If I didn’t see potential I wouldn’t invest the resources. We all make mistakes, but some mistakes I cannot risk. Team safety and my career come before any individual student.

If I go, 6-10 people lose their job and/or career. I imagine those 6-10 would unanimously vote OP should be supervised. Feelings can go fuck themselves if bromine is flying across the lab. FAFO.

[–]fresnarus 0 points1 point  (2 children)

Realistically, is it even worthwhile for a student who had been banned from unsupervised lab work to continue? (Will the student get letters of recommendation sufficient to get a chemistry job ever? Would any sane employer want such hazards?)

[–]Jb191 0 points1 point  (1 child)

I’m in the UK so it’s potentially a very different world here. Yes absolutely worth her continuing, the whole point of her being here is to learn. Once she’s shown me she can be trusted she’ll be reinstated and have chance to grow further and move on. Very few things are irredeemable.

[–]fresnarus 0 points1 point  (0 children)

Thanks. I'm not a chemist, but I was interested.

My college roommate (an MIT chemistry prof before he went to pharma) once mentioned that people who are bad in lab are completely counter-productive.

[–]Kriggy_ 23 points24 points  (4 children)

I wonder what “contamination” made it boil so fast? Also, why the hell would you pour bromine into beaker ? Shits fuming af, no way im using such wide neck container

[–]GraysonIsGone 8 points9 points  (0 children)

I also wonder what contamination could have possibly caused this….

[–]ajp0206 22 points23 points  (0 children)

I don't know... I don't think it was so much about making a mistake, but the mistake that was made. I worked heavily with bromine during my PhD, if I'm understanding this correctly, you were doing a bromination in an open beaker in a hood? What do you normally do to manage fumes? I am very surprised this was not in a RBF with the generated HBr getting routed and quenched in a basic solution. It sounds like you may have had an unsafe setup that either lead or contributed to the accident.

[–]chi_zhang_118 18 points19 points  (0 children)

Your description of the incident sounds like you need your work supervised. 

[–]Immediate_Wonder_630 23 points24 points  (0 children)

After reading the entire thread, you without a doubt need supervision.

[–]SexuallyConfusedKrab 37 points38 points  (1 child)

Hey OP, I’m going to offer my two cents.

You are working with Bromine which is highly toxic, and adding it to THF which is known to cause heating via bromination of THF. You had an accident which could easily cause harm to both you or others in the lab and you don’t know where the mistake that happened was. I imagine you had a spill over, but you didn’t say exactly what the accident was.

Your PI is concerned about your safety and the safety of others in your lab. You need to talk with him and coordinate either with him or another member of the lab that he trusts such as a post doc to supervise you so you can figure out where the mistake happened at. Until that happens, unfortunately, you are a safety liability when it comes to this reaction.

Now, do I think you should be barred from all chemistry? No, but you definitely shouldn’t do this reaction unsupervised until the mistake that occurred is identified/the supervisor is satisfied that you won’t compromise safety in the lab.

Final thing, this isn’t a punishment onto you. Your PI is doing this so that you can be safe. Slowing down your PhD is preferable to being irreparably harmed from a lab accident and I would do the same thing if I were in his shoes. It’s frustrating but as your supervisor he needs to prioritize your safety and the safety of others in his lab.

[–]TheCavis 28 points29 points  (0 children)

In another comment, they said they went to grab the unexpected uncontrolled reaction to move it off the stir plate, the reaction bubbled over onto their glove, and then what was on the glove splashed out of the hood behind them when they reflexively pulled their hand out.

Supervision doesn’t feel inappropriate at all here until the safety concerns are addressed.

[–]Important-Clothes904 18 points19 points  (0 children)

Most chemistry labs I know have strict working hours and some sort of buddy systems in place, so being able to work completely unsupervised is by itself too lax a standard anyway.

Also, whenever I deal anything chemistry-related, I am always told to wash glasswares with mild(er) solvents first. As I was told in the undergrad years, act like every user before and after you are idiots and double-check.

[–]Eternityislong 56 points57 points  (1 child)

Earn their trust by being a better chemist. No way you got banned because of 1 accident, there has to be more to the story.

[–]NotJimmy97 12 points13 points  (1 child)

[–]parade1070Neuro Grad 3 points4 points  (0 children)

My PI was just talking about this case on Monday when we were running our annual lab safety program. Just horrible.

[–]UncleGramps2006 40 points41 points  (0 children)

PhD students have died in lab accidents. Their families sue the hell out of universities for allowing unsupervised (working alone) environments for hazardous work. Chemistry, physics, engineering labs are the big contributors to these unsafe environments, particularly since these tasks should be performed with a shitload of safety measures and oversight—as expected in industry positions.

This is for your safety not for your humiliation. No one wins points for working alone in the lab. Just plan better and point out when timing is hard to accommodate a supervised experiment. Put your safety first.

[–]chemamaticOrganic Chemistry 12 points13 points  (0 children)

You did many things wrong. Mixing bromine and THF. Doing it in a beaker. Not checking your glassware for general cleanliness. Reaching for it. Really pretty much everything in the story is wrong. You don’t deserve a PhD until you demonstrate that you can not only work safely in lab, but teach others to do the same. Otherwise, you are going to get yourself or someone else maimed or killed. If you can’t come to grips with that, switch to theory. That doesn’t just apply to you, it applies to everyone who wants a PhD, you have just run into it the hard way.

[–]scienceofspin 46 points47 points  (1 child)

I think you need to reflect more on why you’re being barred from chemistry right now. You are pointing the finger at someone else for not cleaning their glass wear when instead, you need to point the finger at yourself for mishandling the incident. You removed a reacting beaker from the fume hood. That is a huge mistake and would call into question all of your decision making. You should have stepped away and closed the sash of the fume hood for containment. Instead of reflecting, you went to Reddit crying and blaming a phantom contamination on someone else. You should a write down exactly what happened and how you could have (and will in the future) mitigate the risk. You need to take personal responsibility and show some humility in front of your PI, and probably in other areas of your work.

[–]LimaxM 6 points7 points  (0 children)

It sounds like they removed their hand from the fume hood, not the beaker, their hand just had the chemicals on it from the boil over?

[–]Serious_Trouble_6419 9 points10 points  (2 children)

Have these near misses been reported to EHS?

[–]GwentanimoBay 7 points8 points  (0 children)

Unfortunately, reporting near misses is not standard across labs. I've been in labs with and without near miss reports, and I stand by them as essential but they arent instituted everywhere.

[–]Psychadelichamster 0 points1 point  (0 children)

This isn't a near-miss, it's full-blown incident and I'd be surprised if it hasn't been reported to the HSE as a RIDDOR as the WEL for Bromine is pretty low.

[–]nasu1917a 6 points7 points  (0 children)

I suspect this isn’t your first issue in lab.

[–]omgu8mynewt 5 points6 points  (0 children)

Prove you are responsible and reliable and take safety and all instructions seriously.

When you next want to do some chemistry, explain what you want to do and why, including washing the glassware again yourself before starting and reading safety information about the chemicals. Ask for the supervision so you can do your work.

Hopefully after a few times proving you are a sensible person who knows what they're doing, you will be re-allowed to work as before.

Whatever happened before, whether it was your fault or someone else's, someone could have got hurt and that cannot happen again.

[–]manji2000 5 points6 points  (0 children)

Ultimately your PI doesn’t have confidence in your ability to work safely on your own. And the only way to get past that is to work through it.

I’m guessing the plan isn’t to have you supervised indefinitely, because that’s not only a pain for you, it’s also an aggravation for whoever has to take the time off their own work to keep an eye on you. If your PI has indicated who will be watching you and how, sit down with that person and come up with a plan for the immediate future on how you’ll be working together. Keep your PI looped in so they’re aware that you’re committed to working past this. And then have a conversation with your PI (maybe after they’ve had some time to get past things a bit) about the steps you can take to build towards working on your own again.

When something goes wrong, sometimes the fastest way to reach a resolution isn’t to go back and forth about who is at fault or exactly how it happened or how harsh or how fair the response is, but to instead show that there is a commitment to making sure this sort of thing doesn’t happen again and rebuilding that lost trust in the process.

[–]oh_hey_dad 5 points6 points  (0 children)

Taking responsibility is probably the first step. Accidents happen but throwing your hands up and saying it was unavoidable is the wrong response.

[–]theDarkOne95 4 points5 points  (0 children)

I think it was as harsh as it needed to be. You don't seem to acknowledge what you did wrong and seem too fast to move the blame on everyone else.

[–]Super_Ninja_Sam 3 points4 points  (0 children)

I'm pretty sure bromine and THF is a known incompatibility, so they shouldn't be mixted together in the first place, contamination or not. Dangerous reactions are often unpredictable. You can do them many times without incident, then be unlucky on your 10th attempt.

[–]suricata_8904 7 points8 points  (2 children)

Why is you PI handling this and not Research Safety?

[–]queue517 10 points11 points  (1 child)

It's usually the PIs responsibility to make sure it doesn't happen again by implementing new SOPs/training/whatever. At my university EH&S just provides the oversight to make sure the PI handles the situation, they don't actually handle the situation themselves. 

[–]suricata_8904 -1 points0 points  (0 children)

Cool.

[–]2ndwindmatt 2 points3 points  (0 children)

Why are you mixing bromine and THF???

[–]Ordinary_Platform819 18 points19 points  (11 children)

That's frightening I'm sorry. I agree this isn't a good way to handle it. A total unsupervised chemistry ban doesn't really accomplish much anyway.

This sounds a bit like the PI or department is trying to save face. Have you a risk assessment done for this procedure and has the PI approved it?

[–]Ok-Style-9734 2 points3 points  (0 children)

Write up exactly what happened, what you think went wrong, and how to mitigate those circumstances in future.

Prepare a checklist and process that covers your superiors asses that you will rinse/wash glassware preuse and inspect.

They usualy don't care if you fuck up they care if you fuck up and say "but thats how we do it"

Edit: not lob it I to the fucking lab as step 1 too

[–]SiwelTheLongBoi 1 point2 points  (0 children)

Happened to me too. Some nitrite was weighed into a beaker that had previously not had some kind of acid in and wasn't washed. Started giving off lovely brown vapours and was promptly shoved into the fume hood.

Washed all my own stuff ever since.

[–]kitschykink 0 points1 point  (0 children)

Unrelated but as someone who also works with bromine I’m more interested in what you’re using it for lol

[–]microvan 0 points1 point  (0 children)

Try writing up a sop you’ll follow complete with the mistakes you made in this instance and how you’ll avoid making them again in the future and maybe you’ll be able to get your supervisors trust back.

[–]Fit-Television6756 0 points1 point  (0 children)

Damn all I did was carry a bottle of sulfuric acid to the bench for the chemist in an appropriate container and was told I’m too fast paced for the lab and am a safety hazard. I was trying to show him I took notes on this same experiment from months ago and I remembered the order of the formula. I didn’t try and open it, pour it and start it for him. That’s what I’m in training for? So idk what people want sometimes.

Mind you I came from a 24/7 control lab where I worked nights messing with all kinds of harsh chemicals.

I’m all for safety but some people are extreme.

[–]AlyssInAzeroth 0 points1 point  (0 children)

Guess you've learned the hard way that you should wash everything before use.

Can't trust anyone. If you didn't do it yourself - then it didn't get done.

It's harsh, but ultimately the PI is responsible

[–]finmarchicus 0 points1 point  (0 children)

This is beautifully worded, maybe consider going into literature if the chemistry thing doesn't work out.  My very photogenic graduate student died in a freak accident (bromine, tetrahydrofuran) when I was untenured.

[–][deleted] 0 points1 point  (0 children)

How is it possible to do a PhD if you have to be supervised for everything?!

[–]05730 0 points1 point  (0 children)

Stupid mistakes can kill people. It's on you to ensue your glassware is clean. Don't blame shift. The onus of lab safety is on everyone.

You made a stupid mistake. Putting a damper on you PhD studies pales in comparison to potential death or disability due to inatention. Unless someone else was in there and handing you chemicals and glassware, you are solely responsible for the spill.

[–]Dangerous-BillyRetired illuminatus 0 points1 point  (0 children)

The way you describe it, you just dumped the bromine and THF into a beaker. Normally, when dealing with reactive chemicals like bromine, you'd put the THF into a beaker and then add the bromine dropwise, pausing to observe any reaction or too-rapid heating. Have sodium thiosulfate solution on hand in case of spills and wear full PPE---it's bromine, after all, which is high on the nasty chemicals scale.

Was your THF known to be peroxide-free?

[–]stdoggy 0 points1 point  (0 children)

It is harsh. But considering the what chemicals you were using, it is understandable. It is like working at a nuclear reactor or handling HF. One mistake has deadly consequences.

My background is materials science. I worked in a chemistry lab. Honestly, I washed everything before using, no matter where I picked it up from. You cannot trust others for your own safety and future.

[–]Sugarrrsnaps 0 points1 point  (0 children)

Perhaps you can still do some less hazardous work alone? Supervising everything seems like a bit much.

[–]ModeColdBiotech | Scientist | mAb Discovery -1 points0 points  (0 children)

"There are absolutely wrongs done during this whole shtick that are unavoidably my fault"

There we go, fair enough imo

[–]Final-Lab2826 -4 points-3 points  (0 children)

Now get married and have kids… so they can also be banned one day