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Zinc
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Originally posted by Fleaker:
Another thing to watch out for is not touching a bromine bottle that has bromine on it. First it looks like you cut yourself (the blood red color sans
fuming  ), then it feels like it!
Yes I know that. I once got some bromine on my skin.
My finger was brown for 4 days.
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S-Bursic
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I made a mistake, it wasn't a flask it was a beaker. I often mix those two because I don't speak english very often. My apologies.
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UniversalSolvent
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I accidentaly shifted a thistle tube during simple generation of hydrogen using H2SO4 and zinc. A bit of hydrogen shot up the thistle tube and
spattered the acid on my shirt and hands, eating large holes in the fabric. I could feel my skin tingling, but the acid was neutralized before any
bodily harm was done. I'm just glad that this mistake wasn't made during a reaction using heated sulfuric acid. That could be very nasty indeed.
Someone once told me a story of a large quantity of H2SO4 fountaining out of a piece of glassware into their face during a school experiment. He's not
blind though, so it seems nothing overly bad occurred. That would scare the hell out of me, though.
[Edited on 4-6-2006 by UniversalSolvent]
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12AX7
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I know a precious metal refiner who says he once got a drop of nitric in his eye. After a while the top layer of skin flaked off, doc said the body
is more capable of neutralizing acid than base, if it had been NaOH he'd be blind in that eye.
Tim
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ethan_c
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| Quote: | Originally posted by uber luminal
1. moved my arm too close to the upper metallic shell, while arc melting a sample. A wingnut was about 3 inches from my wrist when the electricity
decided my arm was a greater drop. left a sizable scar on my wrist and scared the piss out of me.
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Did I tell you about this- when I was TIG welding the other weekend, I found out that the machine I chose to work on happened to be broken that day
(the grounding wire had corroded away at the machine connection). I was also welding thick aluminum plate, so had it set somewhere between 300 and 315
amps- what's interesting is a day or two later, the initial blister sloughed off, and there was another blister underneath! At this point, a couple
weeks and about four blisters later, this is proving to be a rather interesting injury in my experience. Rather painful at the time, the only
experience I have to compare it to is a cattle prod to the forearm, and they are similar indeed.
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ethan_c
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| Quote: | Originally posted by Zinc
Yes I know that. I once got some bromine on my skin.
My finger was brown for 4 days. |
My chemistry teacher had some extra bromine, and he sure as hell didn't want it around, so I figured, "Hey, I'll add it to my element collection!
Woohoo!" He bottled it up for me and sent me on my way- unfortunately, he put it in a round-bottom bottle, so I just set it sideways on the wooden
table where I keep all my in-use chemicals and experiments in the garage. I figured he knew what he was doing- imagine my chagrin when I opened the
garage door the next morning to the hearty stench of bromine settling over everything. It had literally melted the cap into a little plasticky puddle,
eaten a fair way into the wooden table, and was corroding some nearby transformers at a remarkable rate. So I had the fun of cleaning up bromine
everywhere with paper towels, safety glasses, and a home depot respirator. I set up all the fans we had in the garage, and only felt like I had strep
throat (strep lung? heh) for not quite a week!
Life is full of nice little surprises, eh?
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woelen
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Ethan, welcome to the world of the halogens  . They are like aggressive animals.
Almost impossible to keep in their cage, and while breaking out, they destroy everything on their path. I have had a similar experience some years
ago, with a bottle full of chlorine gas, which I prepared and wanted to store in a fridge for future use. A few days later, the inside of the fridge
was rusted liked hell. The cap was eaten away and the gas had escaped. Just 1 liter of gas, and it was a real mess. Fortunately, the fridge was a
very old thing.
Even iodine is a very nasty little beast, when it has to be stored. It does not eat away caps, but it certainly escapes. I have my iodine stored in a
glass bottle with thick plastic cap, wrapped in tissue paper, and then a plastic bag around it. And this plastic bag in another glass bottle with
plastic cap. Even with this arrangement, there are brown stains around the glass bottle.
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Jdurg
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I concurr that halogens are a BITCH to store. Thankfully, my iodine that is not sealed in an ampoule is behaving. I have it in an amber-glass bottle
with a PTFE cap and NUMEROUS wrappings of Teflon tape around the threads as well as the outside of the cap. The Iodine is then put in a plastic bag
and then put into a metal can. No corrosion or noticeable iodine vapor. Bromine is a different beast altogether. ALL of my bromine is permanently
sealed in a glass ampoule.
Now for the accidents/stupidity. 
1): Junior year of college analytical lab. I was determining the metal composition of a US Nickel. The analysis required the use of concentrated
HNO3 and H2SO4 at various parts. So I took the acids and poured them into separate beakers, but forgot to label them. At the end of the lab I was in
a rush to leave so I picked up each of the beakers using my one open hand. Thankfully, I held the HNO3 beaker in the hand, but I grabbed the sulfuric
acid one by just shoving my thumb into the beaker right into the liquid there. I foolishly thought it was water.  I quickly raced to the disposal area praying to god I didn't drop either of the concentrated acid beakers.
Meanwhile, my right thumb was starting to tingle. (Thank god for the presence of dead skin to slow down the "eating" of the flesh). What hurt more
was when I finally put the beakers down and washed my thumb in water. Got some nasty thermal burns there, and at the same time wound up moving my
forearm over a spilled HNO3 puddle. Skin turned yellow for a few weeks and made a nasty little scar. (Though the scar is mostly healed).
2): Sophomore year of college in my organic lab I did a REALLY stupid thing. At the beginning of lab, I accidentally knocked over an open container
of diethyl ether onto my jacket. I went and hung my jacket up near the fume hood so that the ether could evaporate away during the 2 hour long lab.
The fumes were making me a bit funky, but I figured the fume hood would take care of everything. After lab, I grabbed my jacket and put it on. I
went outside but didn't notice any odors. (Probably because I had gone numb to them after being around them for a few hours). I lit a cigarette and
heard a VERY loud "WHOOSH!!!". I then felt very warm and realized that when I scratched my forehead little black flakes fell down. Then I smelled
the odor of rotted eggs. I guess there was enough ether vapor coming off of my jacket to ignite and instantly burn the hair off of my face. I looked
like an idiot for quite a long time, and my eyebrows still haven't fully returned. Heh. I guess smoking really is bad for you.
3): A few years ago I wanted to make some chlorine for my element collection. Up to that point, I had heard that chlorine was a green-yellow gas but
never had a chance to see it in person. At that point in time, the only colored gas I had personally seen was NO2 which is pretty darkly colored, so
I figured the yellow-green color of chlorine gas would be just as intense. WRONG!!!! Cl2 is pretty faintly colored and unless you are looking
through a very large amount of it, or a very high pressure of it, it's not instantly visible. So I had a small glass jar and had some calcium
hypochlorite powder and some acidic drain cleaner I had bought which had HCl in it. I knew that if I mixed them some Cl2 should be generated. I
added a slurry of the hypochlorite and the HCl drain cleaner. It bubbled up a bit, but not too intensely. I didn't notice any green color in the jar
so I put it up to my nose and inhaled deeply to determine what was going on. A few things I can tell you is that yes, it did produce chlorine gas,
and yes, my lungs and nasal passages hurt for weeks. It also showed how brain farts and chemical reactions are not a very good combination
\"A real fart is beefy, has a density greater than or equal to the air surrounding it, consists of the unmistakable scent of broccoli, and usually
requires wiping afterwards.\"
http://maddox.xmission.com. |
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The_Davster
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Let me just say, kimax is not invincible, I was boiling a KClO3 solution after running a cell, the bottom of the 2L beaker broke, and the hot chlorate
solution containing what would theoretically be almost a pound of potassium chlorate went everywhere. As my hotplate needs some fixing, I was doing
this on the kitchen stove, which only magnified the mess as having several hundred grams of KClO3 precipitate in the space between the stove and the
counter was a bitch to clean up. It even got inside the oven somehow.
And I needed that chlorate, the first is coming up
I will also be taking a brief international flight soon, I am hoping chlorate isent one of the things swabs for explosives pick up......not that Im bringing it with me, just crosscontamination I am worried about.
[Edited on 25-6-2006 by rogue chemist]
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dejitaru
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I was making nitroglycerin.
And I added the glycerin too quickly. I felt the beaker get warm so I rushed it to the deep freezer and thought nothing of it. Seconds later, a thick
orange fog comes billowing from the chest and rapidly fills the room. I open the front door, put on my shoes, and get the hell out of there. The
novelty subsides. Holding my breath, I step in and drag the freezer (still containing the nitroglycerin) inch by inch out the door. Mild nausea sets
in.
It took an hour or so to ventilate the house and clean the freezer.
I set it on a towel to dampen the shock. The stuff boiled over and disintegrated everything.
[Edited on 2006.07.03 by dejitaru]
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hinz
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Last weekend, the same shit with chloracetone as Reverend Necroticus Rex happened to, happened to me.
I learned on the painful way that it isn't possible to scale up a well working test-tube reaction to an amount that reacts in a 1000ml RBF.
The acetone trichlorisocyanuric acid mixture in the test-tube only boiled after adding some sulfuric acid as acid catalyst. (acid catalysed enol-aldol
reaction).
So I thought if it's only boilling a bit in the test-tube, it works also under reflux. I put 120 g C3O3N3Cl3 (0.5 mol) in the flask, connected the
joint, put the cooling water on and begann to add 600ml (appr 10 mol) of acified (10ml H2SO4)acetone from the top of the condensor. I expected the
mixture to boil and the evaporation heat to take away the excess heat, for this purpose I used the large excess of acetone (1,5 mol of 10 mol gets
(mono) chlorinated).
But I thought wrong. First nothing happened but then the temp. rised, it begann to boil and the bubbles climbed in the condensor. After this I went
instinctifly backwards and a few seconds later the flask exploded to quite small pieces of glass.
Afterwards taken for your amusement:
http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...
http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...
Later (after cleaning my lab) I tried it aggain, this time I preheated the acified acetone to boiling and added the TCCA in portions of a few gram a
time. This time it worked perfect, on each addition of TCCA, the mixture boiled of it's own, so it was not necessary to heat it.
http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...
http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...
BTW. Does anyone know if this reaction is possible:
CH3COCH2Cl + CHCl2-CONH2 + NH2-CH3 =triethylamine=>
CH3-CO-CH2-N(CH3)-CHCl-CONH2
If I condense the product later in alkaline solution, does it give a useful yield as a heterocyclic ring by condensation of CH3 from acetone with the
CONH2 from acetamid or give it just a polymer?
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Nicodem
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I can't believe you added 10ml H2SO4 when a couple of drops is enough! Neither can I believe you used no ice bath!
And you actually dripped the highly acidified acetone onto the full batch of solid TCCA! You just called for a disaster. You are lucky there was only
little chloroacetone formed before the flask blowing up or else you would be in dip shit.
I’m glad you are OK, but let this stupidity be a lesson to you.
To all that are about prepare chloroacetone:
STICK TO THE ORIGINAL PATENT PROCEDURE AND DO NOT FUCK UP WITH STUPID AND IRRATIONAL MODIFICATIONS!
How many times must this be said? Chloroacetone is something you really don’t want to mess with. The TCCA chlorination is very exothermic and MUST
BE COOLED with an ice bath or else it will runaway. No more than the needed amount of H2SO4 must be used. Don’t add more if the reaction seams slow,
rather have patience and wait. It can take one hour for all the cyanuric acid to precipitate but at least you will avoid such disasters.
Remember that here you have a very concentrated solution of a powerful oxidant with a fuel, which is technically speaking an explosive mixture!
Besides if one wants a pure product the reaction must be conducted in an ice bath anyway, and the amount of acid catalyst minimum. Otherwise you get
more overchlorination products.
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garage chemist
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Adding acidified acetone to solid TCCA will produce no chloroacetone and only polychlorinated derivatives, since you have a large excess of
chlorinating agent at the beginning.
If the flask wouldn't have exploded, you'd have been left with a solution of polychlorinated acetone in excess acetone, i.e. no yield.
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Zinc
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Yesterday I was making a mixture of KBrO3, S, Fe powder and paraffin oil. I started adding the paraffin oil with a dropper that I used before for
H2SO4 and I didn’t wash it. The mixture ignited in the mortar. It burned fast and the mortar survived unharmed.
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dedalus
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Grignard rxn
The second worst thing in chemistry is when the reaction doesn't go.
The worst thing is when it goes just a little too well.
I was attempting to make a Grignard reagent from a lacrymatory halide that shall remain unnamed. The reaction wouldn't start. Add Iodine Crystal.
Nothing. Scratch scratch scratch with a glass rod. Nothing. Heat it a little. Nothing.
Finally...a little bubbling. A little more. Now, a lot of bubbling....cut to: boiling reaction mixture spurting out of the top of the reflux condensor
like something outta a John Holmes movie.
OhMan. Thought I was going to die, with my eyes tearing.
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nitro-genes
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When in highschool I found an old dusty chemistry book in the attic that belonged to my father, it mentioned the industrial nitration of glycerine
with 1 part nitric acid and 2 parts sulfuric acid at a temperarure of 0 degrees to produce nitroglycerin. The information about nitroglycerin itself
was pretty limited, but said that it would explode from the least amount of heat or shock.
So I "borrowed" some nitric acid from school and made about 15 ml's of nitroglycerin. After scooping of the oily layer with a spoon I found that it
didn't explode when lit with a match. Well, surely this couldn't be nitroglycerin then. Angry as I was I splashed it all into the sinc of my mother to
flush it down the drain...
I used to make dark aluminium powder from aluminium foil in the ballmill. This took about 5 days to complete, but after several 200 gram batches, I
started to wonder how it would be after 14 days. To eliminate excess oxide formation I decided to make the drum as airtight as possible. After two
weeks I was eager to see the result, so without thinking I opened the drum directly which imidiately burst into flames. This scared me so much that I
dropped the drum, creating a sort of jetengine like white flame that sounded like a freightrain. The neighbours living 200 meters abroad later asked
if we had seen a very bright light as well.
[Edited on by nitro-genes]
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vulture
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I've heard a nice story this week. There is a physical chemistry department at my uni which is located in a different building (fortunately!). Anyway,
these guys use alot of wafers and they clean them using SPM, which is basically 30% H2O2 with conc H2SO4, aka piranha fluid.
They use quite alot of the stuff, about 25-50L per week. After they were done with it, thus when it was nicely contaminated with all kinds of crap,
they had the brilliant idea of storing it in 25L jerrycans to be disposed of later. Unfortunately they screwed the caps on TIGHT and put it in a room
with windows which faces the south. With the extremely nice weather here (30C) it was ofcourse an accident waiting to happen. One of the jerrycans
blew up during the weekend and the other one whilst they were cleaning up the mess. It's a bloody miracle nobody got hurt.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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dedalus
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| Quote: | Originally posted by vulture
I've heard a nice story this week. There is a physical chemistry department at my uni which is located in a different building (fortunately!). Anyway,
these guys use alot of wafers and they clean them using SPM, which is basically 30% H2O2 with conc H2SO4, aka piranha fluid.
They use quite alot of the stuff, about 25-50L per week. After they were done with it, thus when it was nicely contaminated with all kinds of crap,
they had the brilliant idea of storing it in 25L jerrycans to be disposed of later. Unfortunately they screwed the caps on TIGHT and put it in a room
with windows which faces the south. With the extremely nice weather here (30C) it was ofcourse an accident waiting to happen. One of the jerrycans
blew up during the weekend and the other one whilst they were cleaning up the mess. It's a bloody miracle nobody got hurt. |
Merck Index #1851 - Caro's Acid.
H2SO5....the active ingedient. Also called peroxymonosulfuric acid. The Merck entry references two explosions, one at Brown U in 1955, one at Sun Oil
in 1960.
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Nerro
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| Quote: | Originally posted by dedalus
The second worst thing in chemistry is when the reaction doesn't go.
The worst thing is when it goes just a little too well.
I was attempting to make a Grignard reagent from a lacrymatory halide that shall remain unnamed. The reaction wouldn't start. Add Iodine Crystal.
Nothing. Scratch scratch scratch with a glass rod. Nothing. Heat it a little. Nothing.
Finally...a little bubbling. A little more. Now, a lot of bubbling....cut to: boiling reaction mixture spurting out of the top of the reflux condensor
like something outta a John Holmes movie.
OhMan. Thought I was going to die, with my eyes tearing. |
"Out of a John Holmes movie" LOL!
Was it benzyl bromide? I hated working with that.
| Quote: | originally posted by Vulture
I've heard a nice story this week. There is a physical chemistry department at my uni which is located in a different building (fortunately!). Anyway,
these guys use alot of wafers and they clean them using SPM, which is basically 30% H2O2 with conc H2SO4, aka piranha fluid.
They use quite alot of the stuff, about 25-50L per week. After they were done with it, thus when it was nicely contaminated with all kinds of crap,
they had the brilliant idea of storing it in 25L jerrycans to be disposed of later. Unfortunately they screwed the caps on TIGHT and put it in a room
with windows which faces the south. With the extremely nice weather here (30C) it was ofcourse an accident waiting to happen. One of the jerrycans
blew up during the weekend and the other one whilst they were cleaning up the mess. It's a bloody miracle nobody got hurt. |
PhysChem... It takes all kinds I guess Who was responsible
for the disposal of the Piraña? Was he punished in any way?
#261501 +(11351)- [X]
the \"bishop\" came to our church today
he was a fucken impostor
never once moved diagonally
courtesy of bash
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dedalus
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It was benzyl chloride.
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Nerro
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Come to think of it, I once did an oxidation with pyridinium chlorochromate which suddenly went berserk in similar way. Nothing happened for an hour
so I decided to heat the reaction mixture a little. Once the temperature came above 35 degrees I stopped heating to see what would happen. The mixture
kept on heating up and after a while the temperature was as high as 120°C... (the manual stated that a maximum of 60°C was to be observed!) The
reaction didn't splatter all over the place or anything nasty like that but the products consisted solely of a black smelly tar-like substance...
Still, it beats the hell out of that little LiAlH<sub>4</sub> accident...
[Edited on 4-5-2007 by Nerro]
#261501 +(11351)- [X]
the \"bishop\" came to our church today
he was a fucken impostor
never once moved diagonally
courtesy of bash
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Zinc
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I was once making chlorate whistle mix. I know that the chemicals shouldn't be ground together but I did it. The mixture exploded in the mortar and
slightly injured my hand but the mortar survived unharmed. Before that I was grinding the chemicals together in a glased mortar so it didn't explode.
This one was not glased.
Also I was once making a mixture of NH4Cl, NH4NO3 and Zn. The mixture ignites when it comes in contact with water. The film can in wich I was mixing
the chemicals by shaking them together wasn't dry so the mixture ignited but I dropped the film can imidiently so I was not injured but the carpet on
wich it fell was burned. Before that I made the same mixture and it didn't ignite when I put a drop of water on it.
[Edited on 16-5-2007 by Zinc]
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phangue
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I was trying to dissolve fragmented tire leads in about ½ quart of HCl. I decided to hasten the process by cooking it on a hotplate. Trouble was, the
container was not heat resistant. Then, I had to clean up the hotplate, work bench, me, the floor—the whole room with a water hose. GO FIGURE!
The second most ignorant thing was when I got interested in home-brew munitions years ago. So I nitrated some cotton, put it in a bottle (about ¾”
in the bottom) and forgot about it. Several years latter, a friend and I was discussing munitions, and he said, “Phangue, you realllly should get
rid of that gun cotton—someday it will torch your house.” Several weeks later I took the bottle to the back yard, uncorked it, lit a match and
touched it off--inside the bottle. The resulting fireball took my moustache, eye lashes, and brows. Funny thing was that the mild mannered, elderly
lady over the fence replied, “I don’t know what the shit he’s doing!”
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hashashan
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I think i beat all of you guys with stupidity 
Did anyone was stupid enough to dry TACP over H2SO4? well i think i was stupid enough some time ago.
i accidentaly bumped the beaker and the plate with about 20 grams of TACP just fell into the H2SO4, it detonated instantly opening my hand, tore it
open quite nicely, if thats not enough i was all sprayed with quite hot H2SO4. got about 10% body burns some of them 3rd degree and really deep. it
took me about 2 months to heal from the burns (still have some really severe scars) 2 operations were made to reapir the hand(which i have to say is
almost ok now, almost full movement however the torn nerves are still not healed and the sensation on one finger is dull).
Oh yeah the place was also quite a mess, the beaker blown a hole in my table(i got really lucky that the gasses were blown towards the wall and only a
tiny amount went into my hand, otherwise my hand would be shred into little pieces). Half of my clothes had holes in them, my bed is still holed like
hell(i do have to buy a new one), traces of acid could be found even after cleaning all my room with sodium bicarbonate solution even after 2 months.
So do i get an award?
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Phosphor-ing
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You very nearly got The Darwin Award!
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