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gatosgr
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[*] posted on 29-3-2016 at 09:55


Wear gloves, chemicals can get through your skins and make you crazy.



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JJay
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[*] posted on 29-3-2016 at 11:00


I had a huge comedy of errors with my tube furnace.

I was having some problems with my power supply, so for troubleshooting purposes, I connected the furnace directly to the wall current. The heating element burned out in about 10 seconds.

Then I rebuilt it twice using a different brand of refractory paper, one that apparently conducts electricity better than expected. Both times it failed at fairly low temperatures.

Then I tried building one out of perlite cemented with sodium silicate. Unfortunately, that composition melts at well under 1000 C, and when molten it etches quartz. So now one of my quartz tubes is damaged (though still serviceable)....

I built one out of stoneware clay last night, and so far it seems to be working OK, but it's going to require some insulation....

[Edited on 29-3-2016 by JJay]
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ave369
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[*] posted on 29-3-2016 at 11:28


Quote: Originally posted by gatosgr  
Wear gloves, chemicals can get through your skins and make you crazy.


You have to work with very specific chemicals to end up crazy (as opposed to burned, sick, ill or dead). And if you work with them, you have bigger problems than lab safety. Problems such as the local law.




Smells like ammonia....
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[*] posted on 29-3-2016 at 12:15


Quote: Originally posted by gatosgr  
... through your skins ...

That's Alien Lizard talk right there.
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[*] posted on 29-3-2016 at 20:21


Quote: Originally posted by aga  
Quote: Originally posted by gatosgr  
... through your skins ...

That's Alien Lizard talk right there.


Damn reptilians eh. I know what you mean. Whenever I see a really hot chick on the bus, I gotta just accept that she's a disguised reptilian lizard, and that its not worth thinking about my chances.

This board looks more like 4chan every day.
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[*] posted on 29-3-2016 at 20:56


My biggest mishap came in organic lab I two years ago. I don't remember what the lab was, but I do remember we were working with a bunch of carcinogenic stuff, pretty sure dichloromethane was in the lab. My lab partner and I had performed several small reactions in test tubes and we were instructed by our TA's to dump everything from our hood into the big 4L waste bottle in the far hood in the lab. When it came time to clean up, I poured all the test tubes into a single beaker to dump in the waste bottle and a 2 foot geyser of liquid cancer shot up from the beaker and sprayed my forearms (hands were safe from gloves). I quickly washed off my arms after (luckily I didn't seem to have any chemical burns). Apparently the TA's didn't know that they should have prepared individual waste bottles for each reaction we had to perform and that the different reaction products were incompatible. Lesson learned, double check the TA's.

[Edited on 30-3-2016 by Alkoxide]
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gatosgr
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[*] posted on 30-3-2016 at 08:36


Damn trolls... :D

[Edited on 30-3-2016 by gatosgr]




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The Volatile Chemist
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[*] posted on 1-4-2016 at 15:06


Yesterday I was trying to ignite a balloon filled with some hydrogen, but I couldn't get it to go off. Turns out a tiny flame from burning the string soaked in acetone won't pop a 1/4 filled balloon...



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[*] posted on 3-4-2016 at 14:12


Quote: Originally posted by Herr Haber  
You've read Urbanski on what industrial accidents used to happen "back in the days?" when making Nitrocellulose?

Well, lesson one: Dont work in a rush, even if you have a friend at home that would like to take home some of this NC.

I was actually trying to compare the différences in nitrating Cellulose both with 68% nitric acid and 92% nitric acid (home distilled). (Same amount of cellulose, same quantity of acids except the concentration).

The first accident happened because the temperature was to high (30c°) in the room and the nitric acid and sulphuric acid were at room temperature.
Maybe there were some organics in the cellulose too. Who knows... This ended with me and my gasmask on, extractor at full speed, window open and calling my friend: "Hey, if you wanna see what a runaway reaction looks like, now is the time. Just stop breathing". There was a beautiful column of NOx angling right where the intake of the extractor was ;)
Yield was obviously low even though I caught the beaker with pincers and put in in ice.

The second accident happened shortly after finishing nitrating the cellulose with stronger acid (cold this time!). I drained most of the excess acid as I usually do and dumped the whole mass into a big sink full of cold water. As I had quality gloves and there were less than 10 grams of NC I put my hands Inside to press most of the acid out. Pretty much what you would do with a sponge. Sure, I felt the heat of the acid dissolving but it wasnt a concern.
The stupid move was to take the ball of wet with water and acids NC out of the water to squeeze it.
WHOOOOSH !
Some cotton burned on my labcoat, the gloves suffered a bit from the heat but fortunately I was still wearing my gas mask so no burnt eyerbrows or hair.
Of course, by that time, my friend who is not faint hearted was a bit concerned and I proceeded to cleanup.

So in one day I managed to:
- Provoke the most two common industrial accidents Urbanski mentioned.
- Etch into my brain that "accidents happen on the roads that you know best".

Lesson learned !


Sounds like an incident I had when I was still messing with HE's. Had made a few small batches of nitrocellulose via H2SO4/NH4NO3, and this was the process refinement batch, IIRC something like ~30g. Smooth nitration, washed until neutral with NaHCO3, rinsed and laid out to dry.

This was before I learned to wash my nitroesters with urea to neutralize any residual NOx, and when I still dried solids with a 100w lamp/fan combination. I was also somewhere around 14 and had that teenage invincibility complex thing going strong.

You can probably see where this is going. It's sunday night, I'm watching TV with my dad, and suddenly there is a large bang - I fly off the couch, run up to my room, and find the door shut - I always left it half open for the cats - open it, and see nothing amiss, odd. . go to where the NC was drying, and find a couple grams worth of smoldering scraps and a ~6" diameter mangled "hole" that used to be carpeted - Over the next several months I found the rest of the pieces of the tray the NC was on. So, I go back downstairs and pretend that nothing happened, fully expecting the worst - Not a word, and to this day we don't bring it up.

Lesson learned? More than I can begin to consider - But at the time, all I could think of was stabilization of nitroesters, since now I had to do it again to replace what was lost. Holy fucking misplaced priorities. . .




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[*] posted on 3-4-2016 at 14:46


Quote: Originally posted by The Volatile Chemist  
Yesterday I was trying to ignite a balloon filled with some hydrogen, but I couldn't get it to go off. Turns out a tiny flame from burning the string soaked in acetone won't pop a 1/4 filled balloon...

Put the string Around the balloon, not up through the hole where you put the gas in ...
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100PercentChemistry
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[*] posted on 3-4-2016 at 16:51


I was heating up a beaker and it broke. Luckily it was just sodium acetate. It did leak into my hotplate but nothing broke. I never have broken a beaker by heat before and it wasn't rapidly cooled.
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[*] posted on 3-4-2016 at 17:45


Quote: Originally posted by 100PercentChemistry  
I was heating up a beaker and it broke. Luckily it was just sodium acetate. It did leak into my hotplate but nothing broke. I never have broken a beaker by heat before and it wasn't rapidly cooled.


Could the beaker have been cracked? I'm thinking that maybe there was a small "star" crack.
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[*] posted on 7-4-2016 at 17:02


Today I was making some calcium carbonate. I dissolved 800 grams of sodium bicarbonate in 8L of water in a 20L bucket and then dissolved 700 grams of calcium chloride monohydrate in 1.5L water in an 8L bucket. Then I started pouring the calcium chloride into the bicarbonate, completely forgetting about the carbon dioxide gas that would be given off. This resulted in chalk on the floor, which I cleaned up with vinegar.
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[*] posted on 7-4-2016 at 17:48


I was doing the standard procedure to smell esters if you don't have the necessary apparatus to reflux and purify. I poured the reaction mixture in a plastic cup, and learned the hard way that esters dissolve polystrene. The oily ester layer on top ate a ring through the cup, made the bottom fall off.



my youtube channel, organic chemistry videos: https://www.youtube.com/channel/UC0qzaRyHxLUOExwagKStYHw
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[*] posted on 7-4-2016 at 18:05


Quote: Originally posted by Cou  
I was doing the standard procedure to smell esters if you don't have the necessary apparatus to reflux and purify. I poured the reaction mixture in a plastic cup, and learned the hard way that esters dissolve polystrene. The oily ester layer on top ate a ring through the cup, made the bottom fall off.

Well, I laughed! :D




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[*] posted on 7-4-2016 at 19:26
MHN


I heated up a 200 mg sample of Mannitol Hexanitrate in a steel measuring cup to see it melt and decompose and the instant I saw NO2 come off it detonated about 6 inches from my face and made my ears ring for a few hours. Didn't were a face shield or earplugs like a moron. I wasn't injured. Just absolute stupidity that should have been avoided.



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[*] posted on 8-4-2016 at 11:03


First major fuck up i ever did was when i disposed of my first batch of chloroacetone by pouring in a load of sodium hydroxide, and i was using a thin necked 500 ml flask, so everything shot upwards in a second or two after addition of lye...
Thankfully i had my face mask on and didnt burn my face...
After that i stopped using thin necked flasks with exothermic reactions.
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[*] posted on 8-4-2016 at 11:09


Quote: Originally posted by Fegie  
First major fuck up i ever did was when i disposed of my first batch of chloroacetone by pouring in a load of sodium hydroxide, and i was using a thin necked 500 ml flask, so everything shot upwards in a second or two after addition of lye...
Thankfully i had my face mask on and didnt burn my face...
After that i stopped using thin necked flasks with exothermic reactions.


Yesterday was the first time I ever had a runaway in a 20L bucket... of course, the reactants were rather benign. I can't imagine what lye and chloroacetone shooting out of a flask must be like... horribly corrosive, toxic, and burning. Must have been a nasty cleanup....
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[*] posted on 9-4-2016 at 00:45


Quote: Originally posted by Keith Fletcher  
I heated up a 200 mg sample of Mannitol Hexanitrate in a steel measuring cup to see it melt and decompose and the instant I saw NO2 come off it detonated about 6 inches from my face and made my ears ring for a few hours. Didn't were a face shield or earplugs like a moron. I wasn't injured. Just absolute stupidity that should have been avoided.



MHN is a strange material bordering on the line of a primary. A lot of times it may just melt and puff like gun cotton but the rest of the time il will detonate. You probably would have been safe if was far less than 200mg./




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[*] posted on 9-4-2016 at 13:48


Quote: Originally posted by JJay  
Quote: Originally posted by Fegie  
First major fuck up i ever did was when i disposed of my first batch of chloroacetone by pouring in a load of sodium hydroxide, and i was using a thin necked 500 ml flask, so everything shot upwards in a second or two after addition of lye...
Thankfully i had my face mask on and didnt burn my face...
After that i stopped using thin necked flasks with exothermic reactions.


Yesterday was the first time I ever had a runaway in a 20L bucket... of course, the reactants were rather benign. I can't imagine what lye and chloroacetone shooting out of a flask must be like... horribly corrosive, toxic, and burning. Must have been a nasty cleanup....


I always do all my first experiments outside on pavement area that i treat with army grade chemical cleanup washing powder(no idea what it contains, i bought 10Kg of it for 5 euros from a surplus store, but it works wonders with acids and alkalines...) and wash afterwards if any spills occur.

Cleanup was pretty easy but the pavement area was left with a permanent faint etch, it has been there throughout the winter and summer...

Living in the middle of the woods is a good thing, nobody will complain about the terrible smell or noise...

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The Volatile Chemist
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[*] posted on 9-4-2016 at 17:25


Today I attempted to dry some sodium nitrate I had made, but there wasn't quite enough water in it to out my hot plate on 3 and expect it to dry out, so it splattered a bit. Got some on my lab computer's screen...

Yesterday I tried to grow a large crystal of copper(II) sulfate 5H2O with a seed and a supersaturated solution of copper(II) sulfate, only to find out the solution wasn't quite saturated...

But on a better note I did eventually make a larger crystal, and successfully dissolved some Tin solder.




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[*] posted on 15-4-2016 at 10:45


Today i performed the classic Dumfuk Reaction (Tos, Pot, Richard Head et al 2016) of trying to distill Nitric acid using boiling chips

It became a lively NO2 generator and boiling chip remover.

[Edited on 15-4-2016 by aga]




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[*] posted on 15-4-2016 at 15:27


Quote: Originally posted by aga  
Today i performed the classic Dumfuk Reaction (Tos, Pot, Richard Head et al 2016) of trying to distill Nitric acid using boiling chips

It became a lively NO2 generator and boiling chip remover.

[Edited on 15-4-2016 by aga]

Lol :) Turns out home-spun boiling chips aren't as great as cracked up to be (or any for that matter...).




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[*] posted on 15-4-2016 at 17:15


My latest frustration in the lab: I was trying to produce glyoxal from alcohol. Since mixing nitric acid with ethanol can turn into an "exciting" oxidative experience, it took me a while to feel comfortable scaling the reaction up to 20mL.

The oxidation seemed to have carried along OK. I neutralized the solution with CaCO3, and then evaporated the mixture down. The copper catalyst seemed to have colored the mixture of salts a bit. I figured, "Hey, the procedure recommends extracting the glyoxal with ethanol, but calcium nitrate is soluble in it. I'm going to try acetone instead".

I did the extraction, and then evaporated the acetone away on the hot plate. I finished off the last bits of solvent in the vacuum chamber. What I ended up with was something that looked like a few mL of green snot. I poked it dubiously with a spatula, and it stretched away reluctantly as I pulled the spatula out. "OK, so glyoxal has been described as a thick, syrupy liquid..."

I did a Tollen's test with some of the goop, and the result came back negative.

Aaaarrrrgggggh!!!!!! I added a bit of dextrose to check my sanity...and got an instant silver mirror. Yaaarrrrgggh!!!!!!

I decided to bring out "My Precious", an unopened, small, 30mL glass bottle of glyoxal that I bought on eBay a year ago, just for lab emergencies like this. I cautiously pipetted some of the yellow looking liquid out, and performed another Tollen's test. Negative!!!!!??????? Aaaaarrrgh!!!!! *@&#^!!!!!

The little bits of "glyoxal" that I added to the beaker floated on top like a sample of motor oil. Hmmm... the CAS# said that it was 40% glyoxal. The label said "GLYOXAL" in big, bold, letters. Sigh...maybe it was the trimer. But how the heck was it lighter than water??? I boiled a sample of it in water, and it would not dissolve at all. The little oily globule floated there, mocking me. I blasted it in the ultrasonic tank, and made a milky suspension. When I took it out, the solution cleared back up into its neat little oily drop.

I added acetone to it, and then it was like, "Oh, you mean you wanted me to dissolve? OK!!! Sure!!!!" I have no idea what exactly is in that bottle, but it looks like light machining oil or something. I'm quite annoyed about that.

I went back and did the procedure again, but with too much alcohol, and not good enough reflux. I think I did actually end up with some glyoxal that time, but not very much. It gave a strong positive for the Tollen's test. I went back and took some of the precipitated salts (mostly glyoxylate and glycolate), and they also gave a positive result. Then I remembered that glyoxylic acid also has an aldehyde group. At this point, the results are inconclusive. Glyoxal is hard to purify, because it can't be separated by distillation. It forms a polymer that is very non-volatile.

So there was my latest batch of lab frustrations.




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[*] posted on 19-4-2016 at 05:29


Quote: Originally posted by WGTR  
My latest frustration in the lab: I was trying to produce glyoxal from alcohol. Since mixing nitric acid with ethanol can turn into an "exciting" oxidative experience, it took me a while to feel comfortable scaling the reaction up to 20mL.

I did a Tollen's test with some of the goop, and the result came back negative.

I decided to bring out "My Precious", an unopened, small, 30mL glass bottle of glyoxal that I bought on eBay a year ago, just for lab emergencies like this. I cautiously pipetted some of the yellow looking liquid out, and performed another Tollen's test. Negative!!!!!??????? Aaaaarrrgh!!!!! *@&#^!!!!!

The little bits of "glyoxal" that I added to the beaker floated on top like a sample of motor oil. Hmmm... the CAS# said that it was 40% glyoxal. The label said "GLYOXAL" in big, bold, letters. Sigh...maybe it was the trimer. But how the heck was it lighter than water??? I boiled a sample of it in water, and it would not dissolve at all. The little oily globule floated there, mocking me. I blasted it in the ultrasonic tank, and made a milky suspension. When I took it out, the solution cleared back up into its neat little oily drop.

I added acetone to it, and then it was like, "Oh, you mean you wanted me to dissolve? OK!!! Sure!!!!" I have no idea what exactly is in that bottle, but it looks like light machining oil or something. I'm quite annoyed about that.

I went back and did the procedure again, but with too much alcohol, and not good enough reflux. I think I did actually end up with some glyoxal that time, but not very much. It gave a strong positive for the Tollen's test. I went back and took some of the precipitated salts (mostly glyoxylate and glycolate), and they also gave a positive result. Then I remembered that glyoxylic acid also has an aldehyde group. At this point, the results are inconclusive. Glyoxal is hard to purify, because it can't be separated by distillation. It forms a polymer that is very non-volatile.

So there was my latest batch of lab frustrations.


Damn that just sounds like one shit day in the lab. Oh well, it happens. How long have you had this bottle though? Has it been exposed to a lot of light? I wouldn't think it would have any effect but maybe an oligomer formed if it sat there in the light forever. Maybe it's just a shitty Chinese product. Maybe you could try to find a better route to glyoxal. Try starting with a high purity acetoaldehyde and oxidize that perhaps. Good luck though, this compound seems awfully tricky for being just the most basic dialdehyde.




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