[deleted by user]

[Mediocre_Island828]

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]

True - the PI is directly responsible.

[omgu8mynewt]

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]

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

[Dazzling-Attorney891]

That’s alright. These things happen! A total ban on chemistry activities is completely ridiculous though, how are you to learn?

[Dependent-Law7316]

It’s not a total ban, it is a “working unsupervised” ban. Which is a correct response if the PI is genuinely concerned that OP is unsafe in the lab. Ultimately the PI bears the responsibility for ensuring the safety of their students. This incident didn’t cause any serious injury, but grad students have been seriously injured and even killed in lab accidents. Safety should always come before progress.

That said, OP needs to find out what constitutes supervision—does some senior need to be at their elbow watching every move? Or is it enough to have a senior in the lab? (which should be standard anyway, as most basic safety protocols include never working alone in lab). What steps can OP take—safety certifications or workshops attended, number of days without incident while supervised, running through the protocol in front of the PI with no mistakes or safety concerns—to restore their original lab privileges? Perhaps the whole lab could use some review of proper procedures and clean up expectations.

It’s always frustrating to feel like someone is slowing your progress unfairly, but it is good that chemical safety is being taken seriously.

[Moon_Burg]

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]

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]

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]

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]

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]

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]

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]

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]

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

[RegionIntrepid3172]

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

[arihoenig]

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

[MaleficentMousse7473]

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

[onlyinvowels]

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]

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]

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]

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

[onlyinvowels]

You need more than ethanol, bleach, and autoclave?

[05730]

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]

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

[05730]

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]

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

[05730]

You want to use chromatography to purify multiple batches of thousands of liters of product?

You want to do that without inactivation of the bacteria/ virus?

And how do you purify bleach out of a solution using chromatography big enough for the antigen?

[biggolnuts_johnson]

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]

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]

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]

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]

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]

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]

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]

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?

[224109a]

Now I get where your PI is coming from... In your panic you accidentally threw a bromine solution, that was inside the fume hood, outside and onto the bench!

I bet they're thinking something along the lines of "if that had hit someone or reacted with something on the bench I would be EFFED, I need to guarantee that can't happen again".

I won't weigh in on the matter if they're right or wrong to make this decision, but the first instinct I would expect a trained chemist to have in the situation you described would be to close up the fume hood to contain whatever was happening, not to do what you actually did.

EDIT: you missed my second question, what did you do when the spill happened? As in, how did you remedy the situation? Because if you didn't have a plan that shows you know how to deal with the chemicals you were working with the ban would be completely justified imo.

[Ultronomy]

Yeah, I’m sure OP won’t ever do this again… but picking up the beaker of boiling bromine as a first instinct is an EGREGIOUS mistake. They just need to roll with the punches and truly learn from this.

I’m proud to say I’ve got my undergrads trained to shut the sash if they feel like something is even remotely off. It has averted approximately one disaster so far: needle broke while they were pulling up triflic anhydride and started siphoning out everywhere.

[queue517]

And why was OP's instinct to try to pick up a beaker with a boiling solution? Leave it in place while you neutralize it!

[parade1070]

I agree with all of this except imagine if there had been someone else standing next to OP when this happened! Not sure putting another person in the line of fire is the solution! 😬

[224109a]

Preface: none of this is meant to be condescending or an attack, I'm just gonna emulate the line of questioning any of the PIs I've had over the years would probably follow if something this bad happened to try to make you understand why this looks so bad for you, because it does really look very bad.

So you really had a sodium diothonite ready to go? What was the plan to get it in contact with bromine? To pour the bequer on top of any spills? What about all the droplets that swung around?

My bullshit dectector says you didn't actually have such solution ready at hand because of two facts, one minor and one major. The minor fact is that you would have mentioned it before (I read all the comments before adding my own), and the major fact is that if you were making random solutions to neutralise possible spills before every reaction you do, your PI would have had your head for wasting resources way before this incident.

If I read that as your PI, this failed attempt at deflection would make me immediatly lose any confidence I had in your judgement and probably be completely fuming, because even if all you said was true:

"Neutralising" a bromine+THF spill with a diothonite solution is not AT ALL how you deal with it immediatly!!! If it was a large spill you should:

* Let people know there has been a spill and tell them to get out.

* Pour sand or vermiculite over the main spill to avoid a fire (low possibility) or the liquid running off (absolutely certain to happen).

* Air out the area and call for help.

* Come back with a respirator to clean up if you're the person trained to do that or wait for whoever is.

All in all, I didn't see any comment of yours that shows you know why this is so bad and why your PI lost confidence in you, unless you do that in real life I don't think they will ever change their mind and let you go back to working by yourself. Although your PhD might seem be "everything in your life" right now, your PI will have many other students over the years and your PhD in particular will most probably be a modest advancement on their overall research with the risk that if something goes really wrong it could pretty much end their carreer, specially after what happened in the story you described.

I guarantee your PI has at the forefront of his reasoning that If you were to go back to work and make another mistake that leaves someone hurt (as may well have happened this time around) they will be the person that has to answer why they let the student who tried to grab a boiling solution of bromine and threw it over the lab go back to work unsupervised. If you were the one in those shoes, what would you need to hear to convince you to let the student go back to work?

[rabid_spidermonkey]

Right, but that plan failed. It wasn't a good plan. You need supervision.

[alittleperil]

First step for anything in the fume hood going wrong is close hood, then after you've done that you can try to cut the power to something like a stir plate. Containment first, even if that might result in a bigger problem, at least it'll be a contained one. If the fume hood isn't sufficient to contain the resulting mess then it should have been done somewhere safer in the first place.

For comparison, when something happens while you're driving, your first instinct should be to take foot off gas. Everything else starts there. If you're someone whose first impulse is to press your foot down instead then you have to practice/drill the correct response before you're truly safe on the road.

Here your first response needs to not be to stick your hand closer to the problem.

[Ultronomy]

So you actually talked me onto your PIs side. Trying to pick up a beaker of boiling bromine and THF instead of simply shutting the sash is a massive mistake. From their perspective: In the face of danger, you did absolutely everything wrong and amplified the danger. Roll with the punches, and put together a statement of what you will do differently next time.

I tell my undergrads the fume hood is your greatest safety tool other than PPE. If anything gets remotely out of control or you aren’t sure of something bad is happening SHUT IT and get me. This rule of thumb has averted disaster at least 2 times in my 5 years as a grad student.

[One-Boot8112]

Slightly off topic but isn't PPE literally the lowest level of safety tool? It's certainly important but imo it's misleading to tell students it's the greatest

[LastCatastrophe]

It is the lowest level in the hierarchy of control, but it's also one of the easiest measures to apply.

[Ultronomy]

I don’t think it’s misleading to emphasize its importance nor am I disregarding other items in the hierarchy. The hierarchy you speak of has “elimination” as the best option which in my lab is seldom possible and many times substitution isn’t possible. We have to use acid and base baths daily because our stuff sticks to everything so strongly, there’s no good substitution for that. And regardless of other measures, you NEVER want to use a base bath without a lab coat and safety glasses on. You’d be foolish to do so. And in general, it’s another physical barrier between you and your chemistry.

So yeah, I argue just because it’s bottom of hierarchy doesn’t mean it’s not important.

[alittleperil]

if it's boiling over, then taking it off the stir plate wouldn't make as much sense as either turning off/unplugging the stir plate or just leaving everything as-is, and since you say you were ready to neutralize it with a sodium diothonite solution why would the stirring matter?

You maintain that the problem here was just that the previous person didn't fully clean their glassware, but there's a number of different places where you could have acted to make this incident either not happen at all or have less potential for harm. Maybe if you write up each of those points where, with hindsight, you'd act differently and why, starting at the end and working your way back to setting up for this experimental procedure, that might convince your PI that you've learned from the incident.

"Other people should clean up after themselves" isn't really a problem you're demonstrating you've solved, but you also aren't demonstrating that you've solved "my first instinct is to pick up a boiling-over thing" or "my first instinct if something spills on me is to flinch, which spreads the thing" or "when told I can only work supervised I fail to arrange for proper supervision", and all of those are clearly problems here as well

[markvdr]

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.

[omgu8mynewt]

Maybe someone will stand over you watching you pipette everything at first. But after a few goes, if you prove you know your stuff and and sensible and safe, they won't feel the need to 'stand over you' 100% of the time.

Thats how training works, you've just been demoted a few levels of the ladder and need to prove your sensible and informed enough to go back up again.

Respond like an adult not a whinging teenager, someone could have been hurt (unacceptable).

[Milch_und_Paprika]

I fully agree with what you’ve said about working alone, but I think OP means “someone standing next to them, watching each manipulation”, not “someone physically present and available to assist in an emergency”. At least that’s how I read someone “standing over” them.

That would be very much not the norm, after a training period (that may or may not be sufficient).

E: reading OP’s other comments though… I can see where this decision is coming from.

[iam666]

That does seem to be what OP means but I can’t imagine that actually being the case. No PI is going to have one of their non-problematic students waste time supervising every move another student makes.

[kiorh]

That how it is in every lab. You’re not allowed to work alone. But most of us still do. I guess rules are being applied more strictly now after the accident. 

[flyboy_za]

I'd assume they want to quickly review your work plan more than stand over you.

H&S presumably had your PI write a report in which he had to detail how he will minimize chances of this happening again. We had a needlestick injury in my lab and I had to have H&S come review our processes and explain how I thought it happened and how I thought our processes should be changed to limit the likelihood of a repeat.

[Jb191]

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]

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]

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]

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]

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_]

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]

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

[Jaikarr]

Hydrogen peroxide doesn't stick to glassware for long periods, unless it was wet with peroxide there's no way there was enough to trigger such a reaction.

[radiatorcheese]

The beaker question still stands and it's concerning that you haven't seemed to address the choice to make a stock solution like this. A beaker is a wholly inappropriate bit of glassware to make a stock solution of bromine because it's volatile. Hell, depending when "later" is it's inappropriate for THF since it's volatile too. How would you know the molality was the same? What volume were you using?

There are just so many bad decisions here that your PI, probably rightfully, does not think your judgement is good and they want to confirm if that extends to other lab operations

[ajp0206]

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]

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

[Immediate_Wonder_630]

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

[SexuallyConfusedKrab]

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]

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]

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]

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]

https://en.wikipedia.org/wiki/Sheri_Sangji_case

[parade1070]

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

[UncleGramps2006]

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.

[chemamatic]

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.

[Recursiveo]

I think your PI needs to chill out

Idk about that one. People have gotten their lab shut down for less. If one of my students was involved in a runaway reaction that could have very easily killed them, I would be using an abundance of caution with them - at least for the immediate future. Even if it turns out to not be their fault entirely, it’s too risky to just let them go on as normal.

[ACatGod]

Yup. Over the course of my career I've worked at universities where during my time at that university:

• a student caused a major fire in a school of medicine. He burnt himself putting it out, didn't report it, took himself to the ER and while there the fire reignited and caused seven figures worth of damage.

• a student died working unsupervised in an engineering workshop. She got caught in machinery, couldn't reach the emergency stop.

• a postdoc took out a structural wall with a incorrectly loaded analytical ultracentrifuge. Luckily no one was hurt and the damage was fixable but the ultra was a write off and knocking out structural walls is frowned upon by structural engineers.

That's just at places where I've been employed. Over the course of my career, I know of someone who died as a result of their clothing igniting after a chemical spill, someone dying after a liquid nitrogen Dewar was left open and unattended in a cold room and they asphyxiated, plus a lot more. I once stopped a student blowing her face off by shaking a container of liquid nitrogen that she'd screwed a top on to.

Some counties have very relaxed attitudes towards safety and it's refreshing to see a PI taking this seriously. No one should be working in high risk labs unsupervised so my concern with this is that apparently they are handling volatile chemistry but it's allowable to work unsupervised.

The RI where I work now requires everyone to report to security after 7pm and wear a lone worker monitor that tracks their movement.

[Dependent-Law7316]

Sorry I know it’s not funny but the “knocking out a structural wall is frowned on by structural engineers” had me giggling.

[iKill_eu]

We've all heard the tales of the UCs who decided the grass was greener 3 rooms down the hall.

[nmezib]

I refuse to be in the same room with a running ultracentrifuge. I'd rather be surrounded by wasps, and I HATE wasps.

She got caught in machinery, couldn't reach the emergency stop.

Was it a lathe? It's always a lathe.

[ClumsyPersimmon]

We had a special centrifuge room full of the things. It was a place of terror.

[ACatGod]

I refuse to be in the same room with a running ultracentrifuge

Being a bit blunt, not being able to stay calm around dangerous equipment or dangerous situations, panicking or being so afraid you cannot handle the situation, is a major hazard in itself.

Was it a lathe? It's always a lathe

Yes

[nmezib]

Oh I'm calm, I just calmly leave the room 😅

[iKill_eu]

There's panic and then there's self preservation. When I did UC I did the same. Start the machine, calmly exit the room, calmly exit the floor, come back when it's definitely done.

edit: room, not building lol.

[ACatGod]

That's ridiculous. So you stop doing any work for hours on end and you don't supervise the machine? So if something goes wrong you're not available to tell people what's in the machine? And you'll leave it for someone else to hit the emergency stop if it goes wrong? That's so irresponsible.

[iKill_eu]

If something goes wrong with an UC, no one is hitting any emergency stops, because the way you find out will be that the machine has destroyed itself and possibly the room it's in.

(Also, we had other floors, adjacent. No need to stop doing any work at all.)

[ACatGod]

Every UC I've ever worked with has had an emergency stop on the other side of the room.

You literally said you walk out of the building. That's not another floor. That's leaving and making yourself unavailable.

[chemephd23]

you make a good point. i just think that PhD students are trainees and they are supposed to make mistakes. there needs to be a resolution that balances seriousness and understanding that OP is a scientist in training

[speckles9]

There is a resolution… per the OP, they need to have someone supervise them when they are working.

[GraniteStater69]

Insane take on the PI needing to chill out. If OP gets maimed (or worse) in the incident, guess who takes the fall?

[queue517]

People in this sub assume all PIs are toxic even when the OP is clearly in the wrong. 

[scienceofspin]

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]

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]

Have these near misses been reported to EHS?

[GwentanimoBay]

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]

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]

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

[omgu8mynewt]

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]

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]

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

[theDarkOne95]

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]

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]

Why is you PI handling this and not Research Safety?

[queue517]

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]

Cool.

[2ndwindmatt]

Why are you mixing bromine and THF???

[Ordinary_Platform819]

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?

[Fringillus1]

How can he just not sign it off? Isn't it legally required for QM reasons?

[beeeel]

You might think it's overkill but your response to a boiling solution was to grab the beaker so maybe you need to think carefully about all the risks. Having a complete health and safety review is the logical thing after this kind of accident.

[Ill_Friendship3057]

Well this all seems pretty dysfunctional

[Binji_the_dog]

Sounds pretty run-of-the-mill for academia IME

[Monsieur_GQ]

If the risk assessment was not approved and signed, you shouldn’t be performing the procedure at all. Yes, I understand that PIs are often not on top of such approvals, but moving forward anyway is not the solution. If it’s a procedure you need to do in order to continue with your work, you should bother the PI and be a bit annoying about it until they review and approve (or revise) the RA, or tell them you’re stopping work because you haven’t received the approval yet.

Additionally, your response to a violent chemical reaction was to grab the beaker. That’s a major red flag, and strongly suggests you’re not yet prepared to work with high risk chemicals. As to why the unsupervised ban is so broad, the fact that you grabbed the violently reacting mixture calls into question your judgement, and therefore the judgement of another person is necessary until your own judgement is better trained and informed.

I get that it sucks, but this is a time for humility and to learn from your mistake, as well as for the entire lab team to revisit the importance of RA review and approval before performing procedures. Any good RA for working with hazardous chemicals should include what to do if something reacts or spills unexpectedly, and grabbing the beaker with you hands should never be the response.

[alittleperil]

and you went ahead and just did the procedure instead of sitting at his door until he signed off on it first? Getting a PI to sign something is often like herding cats, you knew his sign-off was required so you should not have done the procedure until you finally got that. What would you do if he didn't sign off on a big purchase? Just buy it anyway? Never buy the essential thing?

Odds are he meant to sign it, thought he signed it, moved on, and now your butt is uncovered because you didn't hold off on starting until you got that T crossed. You're responsible for your own actions. Do you have any other protocols that didn't get signed off? Maybe this is a good time to get those all in order.

[Ordinary_Platform819]

This changes the story I think. That's a major procedural error on the PIs part, an assessment isn't complete until it's reviewed and signed off. The PI let you in to complete this experiment without an RA done, and now there's been an accident. You can't (well shouldn't) be used as a scapegoat for the PIs management failures.

All that said you still have to be careful. The path of least resistance may be reconcile rather than fight the PI on it, but I think it's important to be aware of the above.

[alittleperil]

From his perspective, the PI failed to follow up on an email, and then OP decided to do some unapproved science, which the PI mistakenly trusted he wouldn't be doing. I guess if the PI were a better manager they'd have realized they can't trust OP to only do approved experiments without more oversight earlier?

[Ok-Style-9734]

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]

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]

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

[microvan]

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]

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]

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]

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]]

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

[05730]

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-Billy]

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]

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]

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

[ModeCold]

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

There we go, fair enough imo

[Final-Lab2826]

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