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Author: Subject: failiure at nitration, can I recover anything?
jupiteri35
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[*] posted on 24-8-2019 at 05:42
failiure at nitration, can I recover anything?


When slowly adding glycerin to the nitrating mixture I didn't stir the contents at all. When I picked up the flask the contents reacted quite vigorously and totally smoked my garage with NO2, I escaped in time. the aftermath looks like this. Is it safe to distill the sulfuric acid from this if the nitroglycerin can't be seen? Also, why is it black? It seems improbable to me that nitrogen dioxide dissolving into the solution would make it that colored.

IMG_20190824_153213[1].jpg - 2.1MB
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Tsjerk
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[*] posted on 24-8-2019 at 06:54


That is what you call tar. It might be possible to recover acid from it, but only when you're really desperate.
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draculic acid69
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[*] posted on 24-8-2019 at 07:23


Glycerin,hno3, h2so4.do you really want to distillation that mixture.doesnt sound safe
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hissingnoise
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[*] posted on 24-8-2019 at 12:51


Quote: Originally posted by jupiteri35  
When slowly adding glycerin to the nitrating mixture I didn't stir the contents at all.

Do you feel lucky you didn't win the "Darwin Award"?

Stirring is essential ─ preferably with a teflon rod or similar inert polymer.

I always used a thermometer and always had a fear of the bulb hitting glass with enough force to detonate the mixture...



[Edited on 24-8-2019 by hissingnoise]
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monolithic
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[*] posted on 24-8-2019 at 13:09


Yeah it's probably not to good an idea to do that reaction without stirring unless you want to risk a miserable death.
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Herr Haber
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[*] posted on 25-8-2019 at 00:13


I can think of a few fatal plants accidents that happened just like this in Nobel time.





The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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AJKOER
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[*] posted on 2-9-2019 at 13:53


Quote: Originally posted by Herr Haber  
I can think of a few fatal plants accidents that happened just like this in Nobel time.



If this implies an accident occurring in the manner associated with an NH4NO3 plant accident, several city blocks can be destroyed (case in point, the 1959 Roseburg, Oregon blast described at https://en.wikipedia.org/wiki/Ammonium_nitrate_disasters ).
---------------------------------------------------------------------

Anyone wanting to make a big bang, for educational demo purposes, it is safer to just employ two reagents that are, in themselves, not explosive!

For example, H2 plus O2 and a long fuse, or H2 plus dry Cl2 and a beam of red light,....

Note, escaping the blast noise may still be an issue, so do use ear plugs.

[Edited on 2-9-2019 by AJKOER]
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Herr Haber
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[*] posted on 3-9-2019 at 03:43


Quote: Originally posted by AJKOER  
Quote: Originally posted by Herr Haber  
I can think of a few fatal plants accidents that happened just like this in Nobel time.



If this implies an accident occurring in the manner associated with an NH4NO3 plant accident, several city blocks can be destroyed (case in point, the 1959 Roseburg, Oregon blast described at https://en.wikipedia.org/wiki/Ammonium_nitrate_disasters ).


I said Nobel because we were talking about nitroglycerine, not ammonium nitrate.
I did not imply storage accidents (never heard of a synth accident with NH4NO3)

Urbanski gives a few examples of how accidents can happen in a nitroglycerine plant. A biography about Nobel many more.

Most obvious way to cause an accident is for the stirrer to stop functioning during addition of glycerine.




The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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XeonTheMGPony
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[*] posted on 3-9-2019 at 04:04


Do not try to recover any of that it is a loss, add in acetone to have the volume of beaker and swirl, this will render safe any NG that did form and oxidize off the HNO3, go slow go steady, then dump in a fire pit and burn it.

Some times better to cut your losses.
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greenlight
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[*] posted on 3-9-2019 at 08:35


I agree, let it go, NG's not that precious.

I remember i did the same thing when I was about 16 years old. Too scared to stir it properly and the temperature shot up to 80°C. Wasn't too keen on that outcome so I dumped it into the emergency water bucket I luckily had been smart enough to have on hand.
Would love to go back to those days:D

Whenever I synthesize nitroglycerin now I add glycerin in small portions and swirl in a conical flask that sits in an ice bath and take the temperature carefully at intervals.





The only use for an atomic bomb is to keep somebody else from using one.
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jupiteri35
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[*] posted on 5-9-2019 at 11:25


I disposed of it as you suggested. Thanks, everybody.
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XeonTheMGPony
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[*] posted on 5-9-2019 at 16:19


Next time, keep good cooling, add drop wise, and stir, there will be a fair delay from when you add the drop to the temp spike, patience and good stirring are vital.

and if you get any on your hands wash them and then make a very strong pot of coffee in case of a nitro head ache (It helps mitigate it) and it won't be an experience you'll forget in your life time. Nitro head aches suck.
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jupiteri35
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[*] posted on 6-9-2019 at 11:56


Quote: Originally posted by XeonTheMGPony  
Next time, keep good cooling, add drop wise, and stir, there will be a fair delay from when you add the drop to the temp spike, patience and good stirring are vital.

and if you get any on your hands wash them and then make a very strong pot of coffee in case of a nitro head ache (It helps mitigate it) and it won't be an experience you'll forget in your life time. Nitro head aches suck.


Can it really pass the skin?
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DavidJR
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[*] posted on 6-9-2019 at 13:48


Quote: Originally posted by jupiteri35  

Can it really pass the skin?


Yes it can - all the evidence you need is that nitroglycerin ointment is used as a treatment for anal fissures. And patients often complain of headaches while using it, too.
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[*] posted on 6-9-2019 at 15:13


Quote: Originally posted by DavidJR  
Quote: Originally posted by jupiteri35  

Can it really pass the skin?


Yes it can - all the evidence you need is that nitroglycerin ointment is used as a treatment for anal fissures. And patients often complain of headaches while using it, too.


Thankfully pure nitroglycerin is promptly cleaned off usually won't but it is those small drops that you miss can make for an annoying night.

Worse yet when you sip your coffee and get that pleasant sweet taste from the rim, oh crap here we go. "Who started the dubstep in my brain with a jet engine backer?
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mackolol
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[*] posted on 7-9-2019 at 12:09


There is nothing to recover man, Don't even start making nitroglycerin if you dont have proper equipment. I would say don't even make it at all, it's very dangerous and unpredictable.
Make rather some nitroglycol, it's more stable and more powerful.

I never tried to make nitroglycerin as it makes no sense if you can nitrate ethylene glycol.
And after all H2SO4 distills at 337 degrees C.
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DrIronic101
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[*] posted on 16-9-2019 at 20:51


You're lucky that it didn't just explode in your face. Stirring and cooling are essential to keep the reaction going in a somewhat stable manner.

I don't see the need to make nitroglycerin, anyways. It seems far too unstable and dangerous.




"Technically, chemistry is the study of matter, but I prefer to see it as the study of change. Electrons—they change their energy levels. Molecules change their bonds. Elements—they combine and change into compounds. Well, that’s all of life, right? It’s the constant. It’s the cycle. It’s solution, dissolution, just over and over and over. It is growth, then decay, then transformation." -Walter White on what chemistry is.
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[*] posted on 2-10-2019 at 13:58


So.....You dicked things up, and now you have a flask full of potentially lethal crud. Smoldering red Nitro is not something to mess around with.

Dilute it with at least 5 gallons of water, and dispose of it. Keeping in mind that concentrated Nitro-glycerine, poured on the ground, retains its explosive qualities.

Had a buddy one time, disposed of some decomposing Nitro, by pouring it on the ground. Thereby creating a greasy Nitro spot, that might might potentially act like a disembodied land mine. This situation caused a lot of sleepless nights, and a big water bill, as he wrestled with the problem.

Apparently, time, and a lot of water, diluted the problem. My buddy still has his legs.
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[*] posted on 3-10-2019 at 10:13


Quote: Originally posted by jupiteri35  
When slowly adding glycerin to the nitrating mixture I didn't stir the contents at all. When I picked up the flask the contents reacted quite vigorously and totally smoked my garage with NO2, I escaped in time. the aftermath looks like this. Is it safe to distill the sulfuric acid from this if the nitroglycerin can't be seen? Also, why is it black? It seems improbable to me that nitrogen dioxide dissolving into the solution would make it that colored.


If I remember correctly the nitroglycerin dissolves in the nitrating mixture and can be separated from it by diluting the mixture with ice cold water.

However as others have said I suggest you do not try this again at least until you have researched the procedure much more and take precautions.

There is probably a youtube video demonstrating what even sub gram quantities can do if its accidentally detonated.




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