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The Volatile Chemist
International Hazard
Posts: 1981
Registered: 22-3-2014
Location: 'Stil' in the lab...
Member Is Offline
Mood: Copious
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Yesterday I tried to condense a solution of stannous chloride in HCl, forgetting there was still a good bit of HCl left...Got a good cloud of HCl
before I caught my mistake...
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aga
Forum Drunkard
Posts: 7030
Registered: 25-3-2014
Member Is Offline
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Today a 'simpler' synthesis of sodium nitrite using CaSO3 and NaNO3.
It sounded stupid because CaSO3 doesn't dissolve in water.
It is stupid - doesn't work at all.
Dump the results, then on to boiling down some ferric chloride.
Hmm. It's a bit bumpy. Best let it cool a bit and add a stirbar.
Maybe add a stirbar earlier next time, right after repainting the new 'hood, including the ceiling.
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Sulaiman
International Hazard
Posts: 3558
Registered: 8-2-2015
Location: 3rd rock from the sun
Member Is Offline
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well, the SM badge survived, and you've "baptised" your new 'hood,
now photo's will look like they are from a true experimentalist, which you are .
I don't trust clean fume hoods.
Imagine the mess if you hadn't got the 'hood working
EDIT: maybe some extra splash-guarding for the ac plug/socket ?
[Edited on 27-6-2016 by Sulaiman]
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The Volatile Chemist
International Hazard
Posts: 1981
Registered: 22-3-2014
Location: 'Stil' in the lab...
Member Is Offline
Mood: Copious
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Ouch...
Today I just *could not* get a 'pulver' from what chemicals I had to burn. Did various AN/sucrose mixes, tried to melt some into a paste and ended up
with charcoal that looked like chocolate. At least I know the Maillard reaction works with sugar and ammonium nitrate... Big I think everything I
tried was just too wet, I couldn't grind the AN enough, or I didn't have a proper way to ignite the junk. Was trying to use a match. It was also very
humid. Whatever. Might try Ammonpulver tomorrow, but I don't know how I'll get it to ignite.
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Procrastinium
Harmless
Posts: 8
Registered: 8-9-2016
Member Is Offline
Mood: In an excited state
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To add my contribution to this beautiful thread, a friend and I decided to melt some copper using an arc furnace constructed from a refractory brick
and an arc welder. Having succeed in producing a glowing red puddle of copper, we the attempted the most moronic experiment we could devise: we poured
it into a bucket of water.
I estimate we had about 20 grams of molten copper (mp = 1085C) and on contact with water, a steam explosion of such magnitude occurred that the 20L
bucket was ruptured. The sound was akin to that of setting off a milk bottle of hydroxy gas. On reviewing the video footage, most of the copper was
blasted vertically up, but lucky we were wearing welding gloves and masks anyway. Occasionally I still find splatters of copper around the place.
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NitratedKittens
Hazard to Others
Posts: 131
Registered: 13-4-2015
Location: In the basket with all the other kittens
Member Is Offline
Mood: Carbonated
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Wow, thats 912dm3/liters of beer breath at RTP, but what is the concentration of EtOH. 
Basket of kittens for you ........BOOM
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
Member Is Offline
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I recently discovered that my overhead stirrer, which I bought used, had a crooked chuck. I followed the instructions in several YouTube videos on how
to remove chucks, using a hammer and an Allen wrench... unfortunately, the chuck turned out to be a collet chuck with a bent shaft, and in hammering
on it, I managed to crumble part of the vinyl worm gear on the shaft. It will still run if I put it back together, but now it doesn't run smoothly
*or* have a straight chuck. So it looks like I'll be calling the American office of the Japanese manufacturer to see if they'll sell me a shaft and a
new worm gear... I have a feeling this is going to cost a lot of money....
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TheNerdyFarmer
Hazard to Others
Posts: 131
Registered: 30-9-2016
Member Is Offline
Mood: No Mood
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I have a couple actually.
1. Not that bad but could have been. I was new at chemistry and was attempting to make sodium silicate. Pretty straight forward synthesis, but instead
of using borosilicate glass I decided to use a soda glass vial long story short the glass ended up breaking and unreacted sodium hydroxide got
everywhere on my workbench... Use proper glassware.
2.Probably my worst accident. Also new to chemistry (not long after the previous accident) I decided to attempt the synthesis of nitric acid. Little
bit more dangerous than sodium silicate. I had finally gotten all of my equipment and chemicals together to make it and so I mixed them. Not much was
happening so I grew impatient and simply left to do something else. When I came back the stopper had popped off of my vacuum flask and there was
hydrochloric acid everywhere not to mention the toxic gasses that where released in my shed. What happened is I forgot to dilute the HCl and when I
left the reaction took place and it happened fast. More gas was being produced than gas being released thus leading to the stopper coming off aswell
as the contents of the flask spewing everywhere. But in the end I did in fact make the nitric acid  . Moral of the story is always follow directions closely if your new and don't try and speed reactions up by adding
more chemical to the mixture.
Edit: Also it completely destroyed my hotplate and actually managed to trip a breaker that powered the shed. When the chemicals got under the surface
of the hotplate it must have brought many wires in contact with each other causing lots of sparks and a tripped breaker.
[Edited on 2-1-2017 by TheNerdyFarmer]
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Geocachmaster
Hazard to Others
Posts: 146
Registered: 5-3-2016
Location: Maine, USA
Member Is Offline
Mood: Corroded, just like my spatulas
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Recent: Attempting to make hydrochloric acid via sodium bisulfate and chloride. My hotplate is probably hot enough but I added some water anyway to
help HCl being driven off (this was the problem). I usually do stuff like this outside but it was raining and I figured with the inverted funnel trap
I'd be okay. After a few minutes of heating up the reaction mixture started bubbling and the HCl starting bubbling through the water in my receiving
flask. This all works for about 10 seconds until water that condensed in the tubing runs back towards the flask. It leaks out of the tubing connection
and starts dripping on the hot plate, instantly vaporizing and putting HCl into the room. As this is happening the flask on the hot plate, now too hot
to hold, starts bubbling out of control. The panic as you rush to find tongs as HCl is coming into the room... Complete failure and only .05 M acid
was the result
A while ago: It was about 18 months ago when I started getting interested in chemistry. I spent around $200 on basic glassware and chemicals, which
included some 98% sulfuric acid and potassium permagnante. Being stupid and unaware of risk, my first idea was to prepare manganese heptoxide . I then went on to make some (without any research other than NileRed's video)
wearing shorts, a tee-shirt, BARE FEET, and NO SAFTEY GLASSES (makes me sick thinking about it). A garden hose was my only safety. It was going so
well, until disaster struck. I was having fun dipping some paper towel in and watching it burst into flames seconds later. I had just dipped some
paper in when a mosquito landed on my arm. I swatted at the mosquito with the manganese heptoxide SOAKED paper. An area of skin of ~2Cm squared got a
nice bit of the chemical on it, along with the excess sulfuric acid. It instantly burned and ran to the hose. I sprayed it with water after for about
10 minutes before I decided that was enough water. I then thought I should dispose of the rest before something else went wrong. I dropped the
container holding it into some water and it splattered getting a bunch on my arm. Some more hosing down and a shower later and I was okay except for
few raw wounds on my arm. To this day I still get scared thinking about how close I came to getting some in my eyes when it splattered and how I would
have very probably gone blind. That scared me into wearing safety goggles always, so maybe it wasn't all bad?
[Edited on 1/2/2017 by Geocachmaster]
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
Member Is Offline
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Today I tried extracting around 700 mL of solution with 30 mL of ether, only to see the organic layer disappear with shaking. I added my other 30 mL
of ether, all that I had on hand, to see a tiny organic layer form. Unfortunately, it didn't appear to contain much of the product.
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charley1957
Hazard to Others
Posts: 137
Registered: 18-2-2012
Location: Texas
Member Is Offline
Mood: Extracted
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My greatest mishap was when I was about ten years old. Was melting lead tire weights to make fishing weights with on a wood fire out in the yard. For
some dumb reason I decided I needed to cool the pipe cap I was using as a form for the weights. Without drying it I made another pour, standing right
over it. The small steam explosion sent molten lead all over my face, ears and scalp. VERY lucky I didn't lose my sight. Lucky too I didn't drop the
crucible on my feet when I dropped it, pouring molten lead all over. I still have the scars on my cheek, near the inside corner of one eye and on my
ear and forehead, and that was 50 years ago this year. Oh, the stupidity of youth. A very significant amount of money has gone into goggles,
respirators, face shields, gloves of various kinds and other personal protective equipment for my lab. I never forgot that instant bewilderment at how
incredibly quickly something so unexpected could happen.
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Geocachmaster
Hazard to Others
Posts: 146
Registered: 5-3-2016
Location: Maine, USA
Member Is Offline
Mood: Corroded, just like my spatulas
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Uhg... Remind me not to fill the flask more than halfway, especially when a lot of gas is going to be given off...
 
Why I filled it all the way, I'll never know.
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
Member Is Offline
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Never, ever wash your mercury thermometer in cold water when the temperature on it reads in excess of 300 C.
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woelen
Super Administrator
Posts: 7977
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
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A little disaster occurred in my lab. I had a big plastic container full of calcium hypochlorite (swimming pool shock treatment). Last few weeks I
have been very busy with studies and hence I did not open the big cupboard in my lab. In the meantime, the plastic of the bottle became brittle and
fell apart, exposing the calcium hypochlorite to the air in the cupboard. The chlorine coming from this hypochlorite has destroyed many things in my
cubboard. Now, looking back, I can explain the faint chlorine smell in my lab of the last weeks.
Appr. EUR 500 worth of electronics is corroded (e.g. a router with green oxidized stuff on all its connectors, a completely rusted power supply, high
voltage capacitors (5000V / 40uF) with completely corroded screw-connectors, the outside of the big capacitors rusting like hell and full of blisters,
labels of other chemical bottles bleached out and very humid, LEDs, resistors, transistors, inductors, all I have to throw away, they are completely
useless, a pressurized can of WD-40 lubricant broken open and its contents leaked out of it, making a puddle of oil, another pressurized canister with
so-called dust-off was rusted and empty. The cupboard itself also is destroyed inside. All hinges and metal parts are severely corroded, the plastic,
covering the hardboard has blisters all over and feels wet. The iron parts are wet, covered by a mix of rust and wet stuff (probably completely
liquefied iron(III) chloride). I estimate total cost of damage to be around EUR 1000
So, never store calcium hypochlorite in its original container for more than a year. The container may look sturdy, but the slowly released chlorine
and hypochlorous acid vapor slowly make the plastic brittle and then it simply cracks under the weight of its contents. I had the calcium hypochlorite
standing there for nearly two years and only had used 100 grams or so of it. The remaining nearly 1 kg can do a LOT of damage by all the fumes it
gives off.
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Bezaleel
Hazard to Others
Posts: 444
Registered: 28-2-2009
Member Is Offline
Mood: transitional
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Ouch!!! Thanks for the warning.
I had unintended corrosion when I kept plastic bottles containing 36% HCl and 52% HNO3. Labels wet and unreadable, chromed hinges of the cupboard
rusting, white crusts everywhere, and everything that stood in the cupboard felt moist and dirty. Since your advice for red capped glass lab bottles,
this is virtually over.
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fluorescence
Hazard to Others
Posts: 285
Registered: 11-11-2013
Member Is Offline
Mood: So cold outside
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We tried to de-gas Methanol for a reaction in the lab. For non-polar solvents like Hexane you simply freeze them in liquid Nitrogen, then let them
melt again under high vacuum so the gases are removed and then freeze it again, like 4 times.
However you shouldn't do this with Methanol....as I was told too late unfortunately. Apparently it will either go into small cracks in the glass or
the functional group (OH) might have interactions with the polar functions in glass. If you let this melt the normal way, even under high vacuum the
flask will explode like ours....one way to avoid it would be to heat the flask for some seconds so the "ice-block" looses contact to the glass wall.
I guess it's more like Methanol might expand a little and destroy the flask that way...it doesn't matter why it happens just keep in mind that rapid
melting of frozen polar solvents can be dangerous for glass....
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Geocachmaster
Hazard to Others
Posts: 146
Registered: 5-3-2016
Location: Maine, USA
Member Is Offline
Mood: Corroded, just like my spatulas
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I just wanted to use my shiny new Soxhlet extractor. I though maybe esterification with drying agent in the extractor like Nurdrage. 20 Minutes into
reflux for making ethyl salicylate the siphon tube activates. What was left of the reaction mixture had a significant amount of ethyl salicylate and
was boiling at much higher than 78. The ethanol pouring back in boils on contact and spews a bunch out the top of the condenser. The wintergreen smell
was so strong it was hard to breathe. I really need to build a fume hood.
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MeshPL
Hazard to Others
Posts: 329
Registered: 20-4-2015
Location: Universe
Member Is Offline
Mood: No Mood
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I guess you need to use a smaller extractor or a larger excess of ethanol or do the reaction on largere scale with the same extractor to prevent such
an occurence.
This is I an example where the reaction literally failed because the scale was too small... compared to the size of extractor. A smaller extractor
wouldn't hold all the ethanol from ester mixture which would still boil at ca. 78C. A larger excess of ethanol couldn't fill the extractor and without
remaining in a reaction mixture. A larger scale is an equivalent of making the extractor smaller.
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A Halogenated Substance
Hazard to Self
Posts: 68
Registered: 7-2-2017
Location: United States
Member Is Offline
Mood: Oxidizing due to extended exposure to oxygen
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I created some videos (using "lovely" text to speech) about my home chemistry mistakes during my first year of amateur chemistry. Some of these
weren't really accidents and were instead very "potential" for accidents. Some of them are quite horrifying to me today.
I'm very surprised I was not injured more often back then.
https://www.youtube.com/watch?v=s-LFxh_ghLc
https://www.youtube.com/watch?v=jKt4IB4U7dw
Enjoy my early ignorance.
Edit: There's also a "first bromine distillation" video somewhere on the channel. It's already mentioned in the videos I linked above but if you're
interested in it here's a more detailed video over it...
https://www.youtube.com/watch?v=F7k_svSp71o
[Edited on 2-12-2017 by A Halogenated Substance]
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Rhodanide
Hazard to Others
Posts: 348
Registered: 23-7-2015
Location: Ｔｈｅ ８０ｓ
Member Is Offline
Mood: That retro aesthetic
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When chem goes wrong?
I know a bit about that.
Spilled Chloropicrin on myself, 35mLs.
Thank holy **** I was wearing an EXTREMELY hydrophobic FBCS. (Full-body Chem suit)
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Melgar
Anti-Spam Agent
Posts: 2004
Registered: 23-2-2010
Location: Connecticut
Member Is Offline
Mood: Estrified
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Trying to dissolve palladium in aqua regia, and wanted to make sure that it had dissolved as much as possible, so as to minimize fumes during
evaporation. Put a torch flame directly on the beaker. Not full-blast or direct, but still enough of a thermal gradient that I now have $400 worth
of palladium salts soaked into my carpet and a few other casualties that got in the line of fire. Interestingly, when I started using an ozone
generator in that room to reduce odors, the polyester carpet gradually disintegrated in the areas where palladium salts had been spilled.
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Sulaiman
International Hazard
Posts: 3558
Registered: 8-2-2015
Location: 3rd rock from the sun
Member Is Offline
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if a replacement carpet costs around $400 might it be worth buying a nice new carpet and processing the old one to recover the palladium ?
CAUTION : Hobby Chemist, not Professional or even Amateur
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
Member Is Offline
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I personally hate the smell of ozone; for me, that would be like keeping a pet skunk to mask unpleasant cat odors.
That is interesting, though... I guess it is a catalytic oxidation? Hopefully it isn't generating carbon monoxide.
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Tin man
Harmless
Posts: 34
Registered: 12-9-2016
Member Is Offline
Mood: Gruntled
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This was a few years ago, before I really got into chemistry. So I had been cooking rocket candy( 60/40 mix of KNO3 and sucrose) for a while at this
point, and I was quit confident on my abilities to melt the mixture over an open wood fire without the possibility of spontaneous ignition, and it was
working great! I had made several rockets by pouring this mix into sections of bamboo, coreing a hole through the center, tapeing the top off,
sticking a fuse in the bottem, and ductaping it to a long stick. All this was working fine, but one thing that bothered me was that I had to take the
fuses out of bottle rockets, as I didn't have the wherewithal to buy them off eBay. So to solve this dilemma, I went to the most reputable source of
information I could think of, YouTube! While browsing, I found a great video by Grant Thomson found here> https://youtu.be/w-H02hwvVgI
In the video, he dissolved 60 grams of potassium nitrate and 40 grams of sugar in whateverthefuck much water. He then added twine and boiled the
solution down until he was just left with damp twine. He then spread the twine out on a baking dish and put it in the oven to dry. After watching the
video, my lazy ass came to the conclusion that taking the twine out of the pan, and putting it in the oven was a completely unnecessary step, and that
one could just continue to heat the twine in the pan to drive off the last of the water. So I went outside, started a fire, dissolved everything in
the aforementioned amount of water, added twine and began to heat it. ( keep in mind that I was using a bean can to do this because, well, I use my
pots and pans for cooking food). So most of the water was boild of at this point, and everything was going according to my halfass plan. I had I ball
of damp but loosely packed fuse wire, so I just continued to heat it to drive off the water. As I was doing this I had neglected to put on safety
glasses because, well, only nerds wear those. As it was getting almost dry, I heard some crackling coming from the can. My first reaction was stop
stiring, get my face close to the can, and look in. At that moment, my face was engulfed in a large, purple fire ball, as the hot fuse burned
instantly. I fell backwards and lie on the ground for a few seconds that felt much longer than they were. When I finaly opened my eyes, I was
immediately struck by the fact that, holyshit, I wasn't blind! For this I was very happy (and even more lucky)! I raced inside as fast as my newly
acquired adrenalin rush could carry me, and ran for the mirror to check out my new haircut. I was not in possession of my eyebrows or eyelashes any
more, but I was in possession of a newly found respect for dangerous chemicals, and that's what you should take away from this.
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JJay
International Hazard
Posts: 3440
Registered: 15-10-2015
Member Is Offline
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I just started oxidizing a gooey suspension of metal hydroxides to extract the chromates using calcium hypochlorite at home. This produces rather
noxious fumes (which I assume are chlorine gas). I ended up putting the plastic container I was using for the oxidation in a 5-gallon bucket and
putting it outside, but my entire apartment reeks of chlorine.
I haven't figured out exactly why this releases so much chlorine, but I won't be doing this reaction indoors without a fume hood again.
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