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Author: Subject: Bad days in the lab or with glassware?
Pyro
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[*] posted on 5-9-2013 at 11:43


how about those little black dots on wood tables?

Ever had a towel in a certain place inside for about 6 months, and then next time you pick it up it completely falls apart?





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Pyro
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[*] posted on 8-9-2013 at 08:08


Today I used the last of my 1l bottle of H2SO4, so I got a funnel and my big refill bottle (2,5l) and started to refill the small one, everything went well until air started escaping from the funnel, splattering drops of H2SO4, one of which landed on my chin, the other on the tip of my nose. it immediately tarted burning so I quickly wiped the most off with my sleeve, then stripped off my gloves and rinsed it with water.

now I have 2 red blotches on my face, lucky it didn't get under my glasses!




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sonogashira
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[*] posted on 8-9-2013 at 11:05


Goodness. Probably you didn't have a gap between the neck of the bottle and the funnel?
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Pyro
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[*] posted on 8-9-2013 at 12:46


nope, the narrow bit of my funnel has a groove in it for just that, but the bottle opening was too big, so the funnel rested where there was no groove



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[*] posted on 24-9-2013 at 06:25


today at school we had to test different foods for fat content by putting them in a test tube with some ether, then evaporating the ether on a piece of paper to see if it leaves grease behind.

anyway, some idiot girl dropped a pasteur pipette into the bottle! (it was a brand new bottle, just opened) I took a big flask from the cabinet and poured the ether into it, then retrieved the now bulbless pipette, all that was left of the bulb was a little sticky ring of rubber.

I'll tell you, we are very privileged to have our own labs with nobody else! working with 20 uncoordinated people is hard, especially if they are dumbwits!




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[*] posted on 30-9-2013 at 11:57


Yesterday I learned just what happens if you use the wrong kind of vacuum pump for corrosive gases. It stopped working, so I opened it up to find this:


Pump 1.jpg - 56kB Pump 2.jpg - 61kB


Luckily, I was able to scrape the rust off and get it working again.
Also, a bromine burn I got a few weeks ago when an ampule cracked from heat stress as I was sealing it:



bromine burn.jpg - 40kB

The burned area turned brown and the outer layer of skin evenutally flaked off (I'm fine now, no scarring or anything :))




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[*] posted on 30-9-2013 at 12:01


I was making an azo dye today and severely stained my lab floor :( now there is a blood red splat mark...
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[*] posted on 30-9-2013 at 12:01


Damn! Sorry for your misfortune CC. Be careful!

[Edited on 30-9-2013 by Bot0nist]




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[*] posted on 30-9-2013 at 13:04


A few days ago a (lit) alcohol burner broke in my hand, splashing it with ethanol and subsequently setting it alight. There was still quite a bit of ethanol left in the burner so instead of dropping it and putting out the fire on my hand, I walked over to the bench and set it down in a large tub of sand, then put out my hand with a rag. It's surprisingly difficult to quash the instinctive reaction to being burnt, but the thought of starting a larger fire in my newly set up lab was quite motivating.

Earlier today, I managed to de-glove my index finger of the burnt hand while tying my shoelaces. It was/is much more painful than the burn itself was.
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[*] posted on 30-9-2013 at 21:15


I had my virtually unused 1 liter three neck RBf shatter on me



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[*] posted on 30-9-2013 at 21:33


Looks like one of those Harbor Freight pumps( my apologies if this is not the case) but Good Lord, what have you been doing to that poor pump?Yechh!
Quote: Originally posted by Cheddite Cheese  
Yesterday I learned just what happens if you use the wrong kind of vacuum pump for corrosive gases. It stopped working, so I opened it up to find this:





Luckily, I was able to scrape the rust off and get it working again.
Also, a bromine burn I got a few weeks ago when an ampule cracked from heat stress as I was sealing it:





The burned area turned brown and the outer layer of skin evenutally flaked off (I'm fine now, no scarring or anything :))




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[*] posted on 1-10-2013 at 15:48


i just spilled half a kilo of sodium hydroxide pellets, those two and a half hours of cleaning up the whole floor, fridge top, the brand new sartorius scale as well as the refractometer was really fun, gonna do it again that way!
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[*] posted on 1-10-2013 at 16:01


i have a large black blotch on my thumb from spilling AgNO3.
I accedentally spilled acetone/ethanol on a hardwood desk. it now has a horrible giant white mark.





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[*] posted on 1-10-2013 at 17:27


Quote: Originally posted by Funkerman23  
Looks like one of those Harbor Freight pumps( my apologies if this is not the case) but Good Lord, what have you been doing to that poor pump?Yechh!


Yes, it is a Harbor Freight pump. I've mostly been using it for vacuum distillation lately, with some vacuum filtration as well. I think the rust had accumulated over several months, from stray bits of corrosive gases (NOx, HCl, etc.) that got past the trap.




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Pyro
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[*] posted on 26-10-2013 at 02:31


2 months ago I did my last Br2 batch, 500ml addition funnel on a 1l RBF, after I added the H2SO4 I got called home.
I intended to come back the next day, but the Romanians came back and I couldn't get in anymore as they changed the lock.

I got back there for the first time since then, Now I have a 1l RBF with a 500ml pressure equalized Add. funnel, and the joint is frozen! whats wore is, I was gently twisting it and I cracked the sidearm! :(

Ideas to separate the joint?




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[*] posted on 26-10-2013 at 03:00


Quote: Originally posted by Pyro  

I intended to come back the next day, but the Romanians came back and I couldn't get in anymore as they changed the lock.


WHADDAFACK?
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[*] posted on 26-10-2013 at 08:53


yep,
I use the cellar, but the Romanians moved in the rest of the building and changed the lock to the outer door.
And they have a key to the cellar! I wouldn't be surprised if they have being stealing my meth! OOPS, I shouldn't have said that :D
but does anybody have ideas to separate them? maybe something to put on the joint?




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[*] posted on 26-10-2013 at 22:54


To separate the ground glass joint:

http://www.sciencemadness.org/talk/viewthread.php?tid=9251




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[*] posted on 30-10-2013 at 10:20


I broke a 1 liter round bottom flask at school today.

We had to determine the concentration of caffeine in coffee with HPLC, we wanted to extract the caffeine out of the coffee with a soxhlet extractor.
My partner didn't add enough solvent to the rbf so there was not enough solvent in the chamber to empty it, when we noticed this we added more solvent(at room temperature).
Dumb, we forget to remove the heating mantle, so due to the thermo-shock the flask broke.

We already had thrown away our stock solutions for the HPLC (don't ask me why), so now we can start al over again.



[Edited on 30-10-2013 by DutchChemistryBox]




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[*] posted on 8-11-2013 at 14:06


I was on my way to an opera and was wearing my favorite suit. I stopped by the lab on my way and decanted some HCl for the following mornings activities. I put on my lab coat and was extra careful. nevertheless I still had to buy a new suit. I usually have some pants in the lab I don't need to keep whole. I just didn't take the time to change. More recently I made an acyl halide but didn't hook up the gas line that goes to the hood for such reax when they're not done in the hood. (an inverted funnel over a beaker of water works too and the funnel doesn't have to touch the water. Indeed it shouldn't.)



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[*] posted on 8-11-2013 at 14:27


Oh no, bad luck.

Just this Wednesday I ruined a nice pair of tan pants.
My partner had just made something using H2SO4. He returned the bottle to the closet.
Later I needed H2SO4 and HNO3 for nitrobenzene so I went to the chemical closet and got both bottles at once (each 1l) and walked to the work table.
When I was nearly there my partner said:''holy shit, there's sulfuric acid all over you!'', it turn out he cross threaded the cap and it had trickled out sulfuric acid. There was a line on the floor from the chem. locker to the work bench. I immediately took off my shoe and sock (luckily it was only on one leg) and rinsed with water, then rubbed in NaHCO3. My shoe survived it and looks normal after a polish, but my trousers have big white streaks on them :(

then later that day we were removing the acid from nitrobenzene by shaking it with water. but when we vented the sep funnel it spat a little nitrobenzene. to stop it getting all over the lab I held a paper towel in front of it. This was while the suction tube was going at full blast, I said to my partner:''oh no, could you imagine if this got sucked up the tube!'' and before I finished the sentence it slipped from my hand into the tube. In building it I had been quite liberal with the tape. I had to remove it all to get out the paper towel.

more coming soon inevitably since I have discovered a way to convert about 100g RP to WP at once




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[*] posted on 11-11-2013 at 07:53
Why the Lab Power Switch Smells like Onions


I was running a routine HNO3 synthesis yesterday with KNO3 and H2SO4. This was on a fairly large scale, to produce 500mL 68% HNO3 starting with 720g KNO3 and 400g 93% H2SO4.

Everything was charged into a 1L-2-neck RBF and heating began. The contents melted into a liquid as usual and I began magnetic stirring as it slowly came to a boil. HNO3 began collecting in the recieving flask.

After about 40 minutes of hungrily watching nothing happen, I (foolishly!) decided it was proceeding predictably enough to go upstairs for five minutes and get a head-start preparing dinner.

Three cuts into an onion, I heard a *thwack* noise somewhere in the vicinity of the lab ceiling which is below the kitchen, followed by a faint hiss. This caused me no small amount of alarm; the hair on the back of my neck stood on end as I dropped the knife at once and immediately rushed downstairs, trying not to touch the walls with my onion-juice laden hands.

To my horror, there was a glass stopper on the floor, apparently having just rolled out of the laboratory door, and it was fuming heavily in the air! I went into the lab to find quite a scene... The contents of the recieving flask were translucent white with K2SO4 or KHSO4 or maybe KNO3. There was a stalactite of this material hanging from the condenser into the recieving flask, and the condenser appeared to be totally plugged with solid white material. Worse yet, voilent boiling was taking place in the boiling flask, sending a volcano of hot foam straight up the still head, past the plugged condenser, and out the hole where the only unclipped stopper used to be, pouring heavily fuming HNO3/H2SO4/K2SO4 straight down the side of it all and right into my heating mantle!

Luckily the fume hood was on and the air quality in the room was fine despite the clouds of brown NOx rolling out of the top of the still head. I immediately cut the power to the lab and carefully monitored the setup as it cooled. The table gradually developed black spots from spattered H2SO4 during this time.

Much to my further dismay, as the mixture cooled, I heard a really loud *TIC* like cracking glass, causing me to sweat for 30 more minutes as it cooled, wondering what could be broken.

I disassembled everything once cool, except the still head, condenser, and boiling flask which are firmly cemented together by the hard white material. My stir bar is also solidified in a chunk of the same stuff. Hopefully soaking in HCl will remedy this. The worst part is that my fears of cracked glass were realized as I discovered a roughly circular crack circumnavigating the bottom of my 1L 2-neck RBF. :mad:

It could have been worse, though. The mantle appears OK, and at least the flask had the good grace to contain its contents despite the crack. I'm also glad I always leave one glass stopper unclipped on the boiling side of my distillation setup. The otherwise high pressure and weak flask could have resulted in a catastrophic explosion, probably destroying the mantle with hot acid. The blown-out stopper was surprisingly undamaged.

I think the bulk of the HNO3 is recoverable. About 650mL of liquid (now with large chunks of highly crystalline white solid and under a brown blanket of NOx) remained in the recieving flask. Hopefully a little dillution followed by simple distillation at the 121°C azeotrope of HNO3 can recover something of a decent yield.

Lessons learned:
Even if you have run a reaction multiple times, there is NO excuse to leave something like this unattended. Eat before starting an experiment. Bring a book, call your mom, mess with the girlfriend, plot your takeover of humanity... just DON'T leave the lab! Always leave a pressure-release stopper on the boiling side of a distillation setup. Even when no significant vapors are produced, it is a good idea to leave the fume hood running if there is a potential for this to happen.


My best failure analysis estimates that as the HNO3 left the flask, the K2SO4/H2SO4 mixture became increasingly more concentrated, and thereby more viscous, which contributed to excessive foaming. Unattended, the foam was allowed into the condenser. As the foam cooled in the condenser, the K2SO4 and any KNO3 crystallized out, first forming large chunks in the recieving flask, the stalactite, and then clogging the condenser. The pressure buildup behind the clogged condenser then blew out the stopper, and the suddenly reduced pressure violently increased the rate of boiling, causing the foamy "volcano". The *thwack* noise was the sudden pressure release by the stopper leaving the apparatus and possibly striking the ceiling/table.

The crack might just be because this was a cheap Chinese RBF. The flask was cooling in the mantle, nice and slowly.

[Edited on 11-11-2013 by Praxichys]




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[*] posted on 11-11-2013 at 17:25


Ouch Prax, reminder for me to never leave the lab unattended (again, I have had my days, none that bad however). Luckily the worst for me lately was picking up a beaker of re-crystallizing AgNO3 which somehow had found its way all over the outside of the beaker. I didn't notice until washing up a few minutes later that I noticed a long streak of black starting at my first finger and running down both sides of my hand. People at school for some reason thought it was some horrible cut or something :) It took about 2 weeks to finally remove the last traces of the stain.



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[*] posted on 12-11-2013 at 20:34
What a shame...


Had some awful glassware luck yesterday. Along with some other glassware, transporting a brand new Chemglass Schlenk-Line with 24/40 ground joints and stopcocks and a 4-neck 12L RBF and I got into a car accident. Both are toast. That 12L flask was beautiful.... :(

@prax
I did something similar a few months back, left my HNO3 distillation running while I walked to the corner store to get a soda. 'Bout halfway there I started getting a bad feeling about the whole thing so I turned around and started sprinting back. As I was running back I see two fire trucks race past me sirens blaring towards the house. They ended up going past it, but I didn't stop running anyway.
I got back and found that my distillation had indeed popped a stopper and flooded the surroundings with nitric acid vapors, thankfully it had been under vacuum so it wasn't hot enough to produce much NOx decomp.



[Edited on 13-11-2013 by *FWOOSH*]

[Edited on 13-11-2013 by *FWOOSH*]
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[*] posted on 12-11-2013 at 23:21
ruined magnets


I just discovered a very unexpected and stupid thing that I did. I managed to spill a significant amount of ferromagnetic fluid onto an N50 magnet. As you can imagine the fluid is super stuck onto the poles. An N50 magnet is just ridiculously strong. It seems impossible to get the fluid off the magnet. You can't exactly grab onto the fluid and pull it off. You also can't heat up the magnet or it ruins the magnet. I was extremely angry when I first noticed my situation, but after a few minutes I started to cry. :( How fast can a person ruin a very expensive magnet? When I get a good photo I will attach it. Other folks may find a photo of this particular stupidity entertaining. :P
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