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Author: Subject: When Chemistry Goes Wrong
ave369
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[*] posted on 18-9-2015 at 14:10


A particularly minor blunder, but still: preparing a chemical that loves to form colloidal solutions, then feeling all butthurt because it does not want to be filtered out. Happened today with sulfur. In my country, an "ersatz solder" is commonly sold, which is made by melting sulfur with powdered aluminium. It is cast into sticks and used by setting the stick on fire and sticking the burning stick into a hole, which makes the melted mass of sulfur, aluminium and aluminium sulfide to fill the hole with a metallic glossy mass.

What did I do? I ground this ersatz solder with a mortar and pestle and dissolved it in KOH. Aluminium dissolved, and sulfur formed a colloidal solution, which I failed to filter out.




Smells like ammonia....
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[*] posted on 6-10-2015 at 18:14


today decarboxyating in a 50L glass reactor at 180c. glass/PTFE tap underneath decided to crack, we were only a few feet away when this happened and bolted out of there. we were lucky that the contents were essentially chemically innocuous, although the resultant thick white aerosol that quickly filled the room appeared somewhat disturbing. thankful for no burns or fire. tomorrow will be a better lab day.
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[*] posted on 6-11-2015 at 06:59


Oh I have a nice example!
Once, in the lab, whole class being there, a girl put a beaker full with diethyl ether on the magnetic stirrer, turned on the heating... thinking it was the stir control...
She turned around to the teacher and claimed her stirrer didn´t work...
Just in this moment the beaker had started to boil vigorously and splashed on the heating plate (which was indeed turned to nearly full heat)...
It was not very loud, a "whoosh" sound, as the fireball was nearly at the (very high, around 3 and a half meters) ceiling!
No one got hurt, well, except the teacher was angry at her so you could say he was butt hurt :D
We made fun of her being that stupid for a whole year.

Edit: Damned, I´ve just read Bromic´s stories!
Some of them caused me to hold my breath, for having situations nearly that worse... on a much lesser scale, but anyway...
Phew! Luckily you didn´t loose an eye or else...

Once got a splash of lye in my eye, reading your lye story reminded me much of it.
Had to get ascorbic acid solution dropped in my eye every half an hour for two days... even at night(This is the treatment for lye burns in the eyes).
Lost a good portion of my sight on that eye because of this.

[Edited on 6-11-2015 by karlos³]
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hyfalcon
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[*] posted on 6-11-2015 at 07:11


Was she blond? I can legally ask that being a male version. Thank God I don't all take after that trait, though I have run across a couple male iterations.

[Edited on 6-11-2015 by hyfalcon]
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Schleimsäure
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[*] posted on 6-11-2015 at 13:55


I just ruined my 1l chrystallising dish as I cleaned 500g of sodium and got a nice fire in the bathroom sink.

Because I needed to heat the sodium in 3 batches after the first one I emptied the dish and on the bottom some very small beads of sodium were left in the dirty slurry (the sodium was very dirty). After collecting the somewhat bigger beads out of the slurry the remaining sodium crumbs were very small, below 1 mm in diameter.
I wanted to go on with rest of the uncleaned sodium and therefore wanted to use the dish again. So I put in some ethanol into the slurry and waited half an hour for the sodium crumbs to react and neutralize. Of course much to little. As I thought there is no more hizzing from H2 production I went to the bathroom with the dish and wanted to free it from the brown mess in order to go on with cleaning of the remaining 300g of sodium afterwards.

But just after the water contacted the slurry in the sink - poof. And the ethanol was burning. The flame was firstly like 20 cm high and grilled my water tap of the sink :)
I deceided not to use my CO2 extinguisher and let it burn down - like 10-15 min. A fair bit of smoke and stinking in the bathroom and after 2 min or so the boro dish cracked. The watertap was unharmed.

Lesson learned: Even with smallest amounts of sodium one should wait a day or so after adding ethanol and before adding water.






[Edited on 6-11-2015 by Schleimsäure]
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[*] posted on 6-11-2015 at 23:42


Quote: Originally posted by Schleimsäure  

Lesson learned: Even with smallest amounts of sodium one should wait a day or so after adding ethanol and before adding water.
[Edited on 6-11-2015 by Schleimsäure]


Another lesson, get a fire blanket. Your crystallising dish would have been saved had you draped a fire blanket over it. (MAKE SURE YOU GET ONE WITHOUT ASBESTOS)
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[*] posted on 7-11-2015 at 16:07


I just dropped a fairly expensive assembly composed of an addition funnel, a 3-neck flask, and a drying tube onto a test tube rack and came away no more damage than with 2 broken test tubes, neither of which contained anything at the time. They were cheap flint glass tubes I bought locally at a craft store. I consider myself lucky.
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[*] posted on 8-11-2015 at 03:27


Oh and just now I was removing solvent from an oil that wouldn't crystalize... I tried applying gentle warming and a high vacuum and realized that there was a leak in the apparatus. So I sealed it, and the solvent flashed, turning the oil into a foam that fortunately instantly crystalized almost entirely inside the boiling flask (my Claisen got a little bit of product in it).
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Schleimsäure
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[*] posted on 8-11-2015 at 15:43


Quote: Originally posted by Deathunter88  
Quote: Originally posted by Schleimsäure  

Lesson learned: Even with smallest amounts of sodium one should wait a day or so after adding ethanol and before adding water.
[Edited on 6-11-2015 by Schleimsäure]


Another lesson, get a fire blanket. Your crystallising dish would have been saved had you draped a fire blanket over it. (MAKE SURE YOU GET ONE WITHOUT ASBESTOS)


Yes, with a 6l CO2 extinguisher I just thougt about the "big incidences". Good hint, will aquire one.
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[*] posted on 8-11-2015 at 16:19


I have a fire extinguisher -- powder type. I feel inspired to also get a fire blanket and possibly a CO2 extinguisher as well.
Thanks arky for sharing.
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[*] posted on 8-11-2015 at 17:56


I built an electrolyser with a gas separator and NaOH as the electrolyte. I was using it to fill two balloons (one with hydrogen, one with oxygen). After a while one balloon slipped off the gas exit tube, resulting in a fountain of hot NaOH solution thanks to the pressure from the other balloon. This fountain covered both my lab, and me. Fast disrobe, and jumped in the shower - no damage to me thankfully. But boy did i feel like a twit.
Lesson: secure all fittings in a pressurised situation.

Same electrolyser, new game: making exploding foam by bubbling the mixed gas through soapy water. This time we (had some mates around) thought we'd be cautious and try a lighting a small amount of foam before going large. The resulting bang left my ears ringing for two minutes. Acquired hearing protection for the rest of the festivities.
Lesson: sometimes you can't be careful enough! We should have had ear protection right from the start .

My biggest mistake involves power electronics - not chemistry I know, but I'm sure a few of you play with electricity too. I was running a prototype electric fence energiser, which stored about 50J at 900VDC. I then turned it off, and went to so something else. Half an hour later I came back and picked the PCB up. Blam! 900V, 25J, DC shock from arm to arm (only got half the juice as the energy was split into two banks internally). I think I was lucky to survive that one, took me an hour to stop shaking, and left holes burnt in my fingers.
Lesson : capacitors storing lethal charge should have bleed resistors and a tell-tale (neon or LED) to let you know when they're charged.

[Edited on 9-11-2015 by Twospoons]




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[*] posted on 8-11-2015 at 20:24


When I was young I mixed some bleach and nailpolish remover (acetone) to see what would happen. Having no clue what I was doing, I poured them both some of each into a solo cup. It started getting warm and the top of the cup started tipping over. Not wanting it to spill, I put it into another plastic container. That didn't end up helping. I'm not sure what else I did but I ended up with stringy bits of solo cup all over. I mixed rubbing alcohol and bleach at the same time with similar results. I found out that I made chloroform. That was my first foray into chemistry.

I was screwing around with Bi, trying to grow crystals on the stove and generally screw around with molten metal. I put some back in the pot to re-melt. Usually the re-melting was a trivial process, the water flashed off on the surface except for one time. I put the metal back in the pot and a second or two later there was a pop and molten metal went all over. One droplet got my glasses and some others are still embedded in the cabinet. I think what happened is that when I cooled the metal with water, a bit got trapped subsurface that couldn't flash off when I re-introduced it to the melt. I couldn't repeat the accident, even dropping water directly on the molten metal. Nobody was hurt.

Steam explosions are no joke and are also require special conditions in order to happen.

[Edited on 9-11-2015 by TheIdeanator]
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[*] posted on 8-11-2015 at 21:48


I just started dehydrating some 3A seives that had been used to dry ethanol. I let the seives air dry overnight to remove ethanol and then put them in an oven at around 300 C. They burst into flames! I watched the seives burn for a couple of minutes and then realized that the top of my oven was turning red hot, so I removed them. The flames refused to be blown out; blowing on them made things much worse. I finally just suffocated the flames with a metal lid.

Some of the sieves have lost their wet look, probably due to the high temperatures from the ethanol flames. I'm now drying the sieves at a low temperature and slowly increasing it to avoid any unwanted fires.
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[*] posted on 16-11-2015 at 15:56


Today is a bad night in my lab: I received a sneaky bite from my nitric acid. That polyethylene stopper that I close the bottle with, it was always somewhat fishy: it sits tightly in the bottle, requiring some fingernail action to pull it out, and it is always wet with nitric acid. But before this day, I always managed to pull off the finger acrobatics to pull this bung out safely, relying on my long fingernails: the worst thing I got was yellow fingernails.

Today I completely forgot that I broke a nail on my right middle finger, and started to open the nitric acid bottle the usual way. And got nitric acid on my fingertip, mostly right under the nail.




Smells like ammonia....
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[*] posted on 16-11-2015 at 16:04


Quote: Originally posted by ave369  
Today is a bad night in my lab: I received a sneaky bite from my nitric acid. That polyethylene stopper that I close the bottle with, it was always somewhat fishy: it sits tightly in the bottle, requiring some fingernail action to pull it out, and it is always wet with nitric acid. But before this day, I always managed to pull off the finger acrobatics to pull this bung out safely, relying on my long fingernails: the worst thing I got was yellow fingernails.

Today I completely forgot that I broke a nail on my right middle finger, and started to open the nitric acid bottle the usual way. And got nitric acid on my fingertip, mostly right under the nail.


Ow.

Yesterday I dropped my 105 degree vacuum takeoff adapter on the floor. D'oh.

I temporarily substituted an assembly constructed from a Claisen adapter and gas inlet adapter... it's not an ideal setup, but it will work until I get a new vacuum takeoff adapter.
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[*] posted on 16-11-2015 at 16:10


Quote: Originally posted by JJay  
I just started dehydrating some 3A seives that had been used to dry ethanol. I let the seives air dry overnight to remove ethanol and then put them in an oven at around 300 C. They burst into flames! I watched the seives burn for a couple of minutes and then realized that the top of my oven was turning red hot, so I removed them. The flames refused to be blown out; blowing on them made things much worse. I finally just suffocated the flames with a metal lid.

Some of the sieves have lost their wet look, probably due to the high temperatures from the ethanol flames. I'm now drying the sieves at a low temperature and slowly increasing it to avoid any unwanted fires.
Now imagine doing that but with ether instead of ethanol...



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ave369
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[*] posted on 16-11-2015 at 16:31


Quote: Originally posted by JJay  

Yesterday I dropped my 105 degree vacuum takeoff adapter on the floor. D'oh.


Also today my Vigreux column broke in half out of the blue. Damn Chinese glass.




Smells like ammonia....
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[*] posted on 18-11-2015 at 11:12


A number of months ago (at least 8), before I had the money for proper glassware, I collected a sample of MnO2 from a fairly large oldschool battery I was taking apart for the carbon rods inside. I simply chucked it in a jar and forgot about it.

It was very wet when I stored it so about 4 months ago, at least, I decided I was going to dry it out. I opted to just put the jar on my hotplate and run it gently. What's the worst that could happen? I left the room for a moment to check on something else, and when I came back I noted that there was a small "leak" near the base of the jar.

I tried to grab it and quickly move it into an un-compromised container.
Imagine my surprise when the bottom section of the jar shears clean off, and my arms are covered in a mixture of hot MnO2 and near boiling water!:o

I sure learned my lesson after that. Jars are for storage, NOT heating. :(
One of many of my various poor decisions with experimentation in the past, but at least it was a learning experience, even if there are still MnO2 stains everywhere.....








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[*] posted on 21-11-2015 at 07:26


Well, I just averted disaster....

Last time I tried drying out 3A molecular sieves, they caught fire. I was heating them in a glass beaker in an oven, and they were moist with ethanol (they had been air dried, but they looked wet). The flames were alarming and could have caused damage to the oven but weren't that serious.

Today I spread out a much larger quantity of molecular sieves in a pan and allowed them to air dry until they lost their wet look before putting them in the oven at 300 C. To my surprise, the entire pan caught fire, and when I opened the oven I was greeted with a large blue fireball followed by shooting flames. I immediately closed the oven. The flames weren't extinguishing themselves, and I'd prefer not to destroy the oven or catch anything else on fire, so I grabbed a spray bottle full of water that I had been using on my terrariums and misted the flames until they went out.

I'm not sure why so much ethanol is adsorbed into the sieves, but I guess I'll try heating them gently before hitting them with high temperatures.


[Edited on 21-11-2015 by JJay]
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[*] posted on 21-11-2015 at 07:50


Quote: Originally posted by zts16  
Quote: Originally posted by JJay  
I just started dehydrating some 3A seives that had been used to dry ethanol. I let the seives air dry overnight to remove ethanol and then put them in an oven at around 300 C. They burst into flames! I watched the seives burn for a couple of minutes and then realized that the top of my oven was turning red hot, so I removed them. The flames refused to be blown out; blowing on them made things much worse. I finally just suffocated the flames with a metal lid.

Some of the sieves have lost their wet look, probably due to the high temperatures from the ethanol flames. I'm now drying the sieves at a low temperature and slowly increasing it to avoid any unwanted fires.
Now imagine doing that but with ether instead of ethanol...


I'm guessing it could blow the door off of the oven... scary stuff.
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[*] posted on 21-11-2015 at 07:56


Quote: Originally posted by ave369  
Quote: Originally posted by JJay  

Yesterday I dropped my 105 degree vacuum takeoff adapter on the floor. D'oh.


Also today my Vigreux column broke in half out of the blue. Damn Chinese glass.


That sucks!

My Chinese kit appears to be a mix of low quality and high quality components. The sep/addition funnel appears to be high quality; the flasks appear to be high quality; the condenser appears to be high quality; and everything else looks like it was picked out of the reject pile. The vacuum takeoff adapter was pretty low quality but I have a good one now, and I figure I'll just replace components as they fail with American counterparts. Vigreux columns aren't cheap....
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[*] posted on 21-11-2015 at 16:37


Quote: Originally posted by JJay  
I just started dehydrating some 3A seives that had been used to dry ethanol....

I'm guessing it could blow the door off of the oven... scary stuff.


From an earlier post of mine:

I had been using 3A mole sieves to dry some 95% ethanol. Wanting to re-activate them I poured them into a 9"x9" glass cake dish and set them on the kitchen counter to dry. They were already mostly dry after sitting in a large beaker overnight. After about an hour on the counter they looked dry so I set the kitchen oven for 500°F (260°C) and placed the sieves in the oven. Some time after the oven had reached temperature I hear a loud bang while sitting in our family room watching TV. I looked in the kitchen expecting to see some heavy object laying on the floor; but there was nothing amiss. I then surmised that the noise must have come from the oven - an explosion of ethanol/air pushed the spring loaded oven door open and then it closed itself with a bang! So I just continued the heating until the time (2 hrs) was up then turned off the oven. A short time later I opened the oven and retrieved the sieves, after assuring myself that the oven temperature was below the auto-ignition point of ethanol.




The single most important condition for a successful synthesis is good mixing - Nicodem
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[*] posted on 22-11-2015 at 16:17


Bromic Acid tells great stories... :)
I once (mind you, before I know how chemistry worked) thought sparklers *must* contain some sort of oxidizer to work. Since I had sublimed sulfur powder, I thought I could make some pseudo-gunpowder. I ground up approximately 10 sparklers, and added all the sulfur I had. I placed this on a very large piece of copper sheet metal I had acquired. Well, thank God it wasn't actually gunpowder, there was a lot of this stuff... I lit a sparkler with a magnifying glass, and carefully placed it on the mix. It flared up with the most intense heat and light I'd ever seen at the time. Great spectacle for a pre-teen. It stayed lit, spewing 'sparks' for a while. The sulfur was obviously reacting with the copper sheet, forming nice blue-green splotches on the metal (in retrospect, it could've been an iron sulfur-oxyanion too). I realized, though, that the flying pieces of metal and molten mix flowing on the copper sheet were a bit of a fire hazard, given the fact the whole thing was sitting on dry grass in our back yard. Trying to stay calm (but still feeling ridiculously cool for figuring out how to do this), I picked up the sheet by its corners with my pointer wingers and thumbs, each corner on a finger or thumb. Now, this plate was approximately 12 inches long and 3 inches wide. And it had been allowing a thermite reaction to continue on its surface for a little while now. So it slid out of my fingers and thumbs, melting four lines down them, one for each corner, one on each finger. It took a bit to feel the pain, but of course it didn't last too long, since I now had to stamp out the fire caused by the fallen sheet and dripping metal. Parents never did hear much about it, though it made a good story at school...
Lesson: 1. Don't be Stoopidd.
2. Know what your reaction is doing, d3on't assume what's in something.
3. Adding sulfur just makes it smell bad. And make clouds of suspicious gas/smoke.
4. Don't be rash, and don't do chemistry if you're just doing it for bragging rights.
Not that chemistry's bragging rights anymore. Heck, the girls in my chemistry class last year probably thought I made drugs due to my 'friends' in the class making loud jokes and statements. This year, I get asked for help by a few, but I've been ostracized from the general social world anyways. If I'd stayed in band I'd at least've had those friends... :/
Chemistry stories, man. They're great. Max Gergel's first novel is my favorite biography, story, almost favorite book.




My write-ups are on here...
http://www.MeltThe.Ga or http://ptp.x10.mx
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ave369
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[*] posted on 1-12-2015 at 06:23


Today, in a break between playing Fallout 4, I decided to test my brand spanking new distillation setup. When I ran it on water, it all did handy-dandy. But then I've run it on Glauber's nitric acid synthesis, and totally forgot about that rubber bung sitting on the top of my Wurtz flask...


Poor, poor bung. It weeps some black liquid into the flask...

[Edited on 1-12-2015 by ave369]




Smells like ammonia....
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[*] posted on 1-12-2015 at 10:49


Just scrap a tire wall and some Nuka-Cola bottles and you'll have a new chemistry station in no time!
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