Author Topic: Lab Accidents  (Read 2280 times)

Vesp

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Lab Accidents
« on: August 28, 2009, 12:02:37 AM »
Well I just got done with one that was pretty exciting. So exciting I'd like to hear your lab mishaps.
Anyways, I was boiling away some remaining methanol, which I figured explained why my 4-methoxyphenol didn't separate with the addition of a conc. salt solution.  It was boiling fine for several minutes, but apparently at some point lost off all the methanol, which caused the bubbles to become extremely stable, and allow for the solution to boil out of the flask and over into the hot oil.

Psshsshh! White death smoke is everywhere. Oil tossed all over the inside of my fumehood, with the heating element on. Yay! I turn off the stove, and go to turn on the fumehood  but people were outside and I didn't want any attention from them asking "wtf happened?" or even worse.. the fire department. So I left it off.


That was nice and scary. I probably lost 50-70% of my product, but it still looks like I have a decent amount in the bottom of the flask, that has solidified.

Anyways, this would be my second, or maybe third horrible experience I've had in the lab.

How about you guys?

PS. I'll add how to avoid what happened to me and some more detail later in the thread. I've got to run
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v16

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Re: Lab Accidents
« Reply #1 on: August 28, 2009, 12:13:45 AM »
open air boiling?  Should of had a condenser on that bad boy....


Vesp

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Re: Lab Accidents
« Reply #2 on: August 28, 2009, 12:34:18 AM »
I had a reflux condenser with out any water running through it, and an  tube sucking the gases that formed via an aspirator at the top that was supposed to prevent this but apparently it got clogged or couldn't keep up with the flow and didn't really prevent anything like I thought it would.  :-X

I guess I should have just distilled the stuff, least it would have been directed into a different direction, but the flask I was using is a 19/22 that only fits a reflux, and a claisen adapter I have.
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poisoninthestain

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Re: Lab Accidents
« Reply #3 on: August 28, 2009, 06:43:10 PM »
Some common mistakes I've made that are really obvious, yet important.

1.) Never heat up a stuck flask...ever. I've sprayed GHB and DCM all over me this way. So dumb.  ::)
    Whenever something get's stuck just use a wrench wrapped in a towel or some cloth, "lighty" twist. Works beautifully.

2.) Sandbaths rule. They don't smell, you can use magnetic stirring through them almost always, they work fantastic for RB and FB. Fuck veggy oil. I love the sand.

3.)Always keep aldehydes airtight. They really enjoy the sweet taste of O2 oxidation(carboxylic acid  >:(   ), which kinda sucks. I've had a few aldehydes oxidize from improper storage.

Vesp

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Re: Lab Accidents
« Reply #4 on: August 28, 2009, 09:57:34 PM »
Yeah, I'm going to start using sand or water now I suppose!
Sand just takes so much longer to heat up vs oil. However, it might be the pot I've used for it, It is dented in on the bottom and so it may not actually be getting very much contact with the element.

How much sand do the flasks need to be in? Just sitting on top, or50%+ covered? I guess it probably really doesn't matter.
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2bfrank

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Re: Lab Accidents
« Reply #5 on: August 29, 2009, 12:50:42 AM »
sand is good. one can have it in reasonably deep, and then if need, remove some of the sand, to somewhat modulate the heat, pending how the reaction is going.

NEVEF EVER, rush setting glassware up, doing stuped things, like, Oh I forgot to put the stir bar in. and thinking, oh well, its only been on for a little while. and dropping one in very gently whooooosh.. TOTALY stuped shit, that happened early on..

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Vesp

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Re: Lab Accidents
« Reply #6 on: August 29, 2009, 01:12:13 AM »
Caused it to flash boil?

Yeah, that happened to me once as well, when trying to distill some alcohol from yeast and sugar a long time ago.
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2bfrank

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Re: Lab Accidents
« Reply #7 on: August 29, 2009, 02:54:30 AM »
Pure luck that I didn't sustain serious injury, it whoooshed.BIG TIME.When I put it in, I saw myself do it, totaly void of thinking, was rushed, and had the good sense though to turn my head, and lucky I did I tell you..The old, shell be right, its just started warming up,  and  the flask content gushed. I cant remember exactly what it was, but remember knowing that if it hit me, with that force and temp, BIG time hurt, id imagine.. I dont rush any chem anymore, and I also always have a reservoir of water to dump, and to flush. and  a fire blanket, Just got to wear those stuped glasses.the other 1% of the time, when I have that attitude of shell be right..If I am serious about wanting home chem to be seen as something a little more than dangerous and illegal, etc, then safety should be right up their, .Nothing can harm the cause more,if another dumbass accident, resulting in damage gets reported... So this thread is important I believe.. Ill be reading other peoples dumbass moments and let it sink in.

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Douchermann

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Re: Lab Accidents
« Reply #8 on: August 29, 2009, 02:57:21 AM »
Oh yes, we've all had some experience with superheated liquids.  When distilling aniline + post reaction mixture, I had a bump so hard, it blew the stopper out of the top and hit the ceiling (10ft).

I've had plenty of accidents in my lab.  If a liquid managed to fill up your condenser to the point where it wont return to the flask, never remove one of the other stoppers to try and equalize the pressure.  It results in a spray of flask contents everywhere hahaha.

I also had iodine crystals lodge themselves all over my face.  A big one went in my eye, and wedged itself deep in my tear duct.  I ended up having to dig it out with a q-tip.  The burn from the I2 still hurts, and it's been two days.

Today, I was venting pure oxygen + a little methanol vapor (not the LEL thankfully).  When showing my friend the power of oxygen + a little ember, the hose actually caught fire, and the white hot jet began shooting up the vinyl hose.  Fortunately, I was quick to flip off the ball valve.

Vesp

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Re: Lab Accidents
« Reply #9 on: August 29, 2009, 04:12:00 AM »
I2 in the eye sounds horrible! is your eye brown? How did that happen?
pics or it didn't happen  ;D

Some things that have happened to me in the past:
  • Cut by a breaking glass bottle of HNO3 - getting some of it on myself but very little.
  • I2 under fingernail
    • H2SO4 on skin - didn't feel it, but noticed the burns, still have the scars
    • Grocery ammonia, from the stores shelf fell onto the floor, splashing into my eyes.
      • Lung full of ammonia
      I think that is about it for now?
      Not much has happened to me.
« Last Edit: June 21, 2010, 08:18:01 PM by Vesp »
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2bfrank

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Re: Lab Accidents
« Reply #10 on: August 29, 2009, 04:22:21 AM »
Ha,, a runway but from the addition funnel.. persulfate, methanol(aq) scaling up, filling it up, enough time to heat it up to the magic whoosh number, caught it as just started reacting,, sort of cool seeing it, but quickly my friend, grabbed it, with a cloth, and raced out, with it gushing all over.re:. the prep for the honey, with the said 95% yields under Nitrogen,, but only got 15, and then 20,, NH4 not good,, converted to Na, slightly better I believe,, not the 95% but, not by a long shot...Better ways He feels..

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geezmeister

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Re: Lab Accidents
« Reply #11 on: August 29, 2009, 04:30:44 PM »
I had a half a liter of naptha detonate on me once when I removed it from the hotplate, where I had let it get overheated as I went out to heed the call of nature.

Cost me two weeks and thirty thousand dollars.

Vesp

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Re: Lab Accidents
« Reply #12 on: August 29, 2009, 07:55:57 PM »
Quote
Cost me two weeks and thirty thousand dollars.

Oh my god, I'm sorry about that!
Glad you are ok though, how is it that it detonated? And how is it that it costed you so much?
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Douchermann

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Re: Lab Accidents
« Reply #13 on: August 29, 2009, 08:27:38 PM »
Quote
Cost me two weeks and thirty thousand dollars.
And how is it that it costed you so much?

Don't be askin that question vesp ;)

I just had an accident of my own about 10 minutes ago.  It wasn't bad, but it was frutrating.  I had a flask full of ketone-bisulfite complex, and when pulling it off the shelf, it hit the top and the bottom slipped out.  2ft fall, and it shattered.  I was sitting there trying to scoop these crystals up into a beaker, all the while being gassed with SO2 from the bisulfite.

Vesp

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Re: Lab Accidents
« Reply #14 on: August 29, 2009, 08:32:43 PM »
SO2 is probably the worst gas to get gassed with, well.. besides ammonia, and it might be equal to HCl though.
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Sedit

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Re: Lab Accidents
« Reply #15 on: August 29, 2009, 08:39:04 PM »
Mild SO2 isn't bad but a strong amount feels like death, some of the SO2 gets auto oxidized and you end up with Sulfurous and sulfuric acid when it hits the fluid in your lungs.
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Douchermann

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Re: Lab Accidents
« Reply #16 on: August 29, 2009, 09:00:24 PM »
Yeah, my main problem with SO2 is the taste it leaves in your mouth.

poisoninthestain

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Re: Lab Accidents
« Reply #17 on: August 29, 2009, 11:05:57 PM »
@Vesp- the amount doesn't really matter I'd say between 20-40% of the container is enough.

I use a little excess to cover the bottom of a steel pot and just enough to immerse a thermometer.

heisenberg

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Re: Lab Accidents
« Reply #18 on: August 29, 2009, 11:22:25 PM »
I've gotten burned by anhydrous white fuming nitric (nice scar on my knuckles), had NOx inhalation, ammonia inhalation, and been sprayed in the eye with boiling acetone vapor.

I also once had a beaker full of partially nitrated cellulose auto ignite on me. It was in a fume hood though, and all it did was seriously alarm me.
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Vesp

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Re: Lab Accidents
« Reply #19 on: August 30, 2009, 06:32:56 AM »
When I began doing nitrations, I some how managed to get a run away with naphthalene. Bubbled a ton, spilt all over the place and made a decent amount of NOx. I just left and waited a while.  No fire or anything though.

Oh also I've made a mix naphthylamines, which one of them is known as a human carcinogen, so that scared me as I didn't realize it and I touched it, and smelt it. eep!
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