jupiteri35
Harmless
Posts: 5
Registered: 24-8-2019
Member Is Offline
|
|
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](https://www.sciencemadness.org/whisper/files.php?pid=621181&aid=76784)
|
|
|
Tsjerk
International Hazard
Posts: 3032
Registered: 20-4-2005
Location: Netherlands
Member Is Offline
Mood: Mood
|
|
That is what you call tar. It might be possible to recover acid from it, but only when you're really desperate.
|
|
|
draculic acid69
International Hazard
Posts: 1371
Registered: 2-8-2018
Member Is Offline
|
|
Glycerin,hno3, h2so4.do you really want to distillation that mixture.doesnt sound safe
|
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
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]
|
|
|
monolithic
Hazard to Others
Posts: 436
Registered: 5-3-2018
Member Is Offline
Mood: No Mood
|
|
Yeah it's probably not to good an idea to do that reaction without stirring unless you want to risk a miserable death.
|
|
|
Herr Haber
International Hazard
Posts: 1236
Registered: 29-1-2016
Member Is Offline
Mood: No Mood
|
|
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
|
|
|
AJKOER
Radically Dubious
Posts: 3026
Registered: 7-5-2011
Member Is Offline
Mood: No Mood
|
|
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]
|
|
|
Herr Haber
International Hazard
Posts: 1236
Registered: 29-1-2016
Member Is Offline
Mood: No Mood
|
|
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
|
|
|
XeonTheMGPony
International Hazard
Posts: 1640
Registered: 5-1-2016
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
greenlight
National Hazard
Posts: 737
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
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
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.
Be good, otherwise be good at it 
|
|
|
jupiteri35
Harmless
Posts: 5
Registered: 24-8-2019
Member Is Offline
|
|
I disposed of it as you suggested. Thanks, everybody.
|
|
|
XeonTheMGPony
International Hazard
Posts: 1640
Registered: 5-1-2016
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
jupiteri35
Harmless
Posts: 5
Registered: 24-8-2019
Member Is Offline
|
|
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?
|
|
|
DavidJR
National Hazard
Posts: 908
Registered: 1-1-2018
Location: Scotland
Member Is Offline
Mood: Tired
|
|
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.
|
|
|
XeonTheMGPony
International Hazard
Posts: 1640
Registered: 5-1-2016
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by DavidJR |
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?
|
|
|
mackolol
Hazard to Others
Posts: 459
Registered: 26-10-2017
Member Is Offline
Mood: Funky
|
|
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.
|
|
|
DrIronic101
Harmless
Posts: 20
Registered: 16-9-2019
Location: Western United States
Member Is Offline
Mood: Insomniated
|
|
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.
|
|
|
zed
International Hazard
Posts: 2283
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline
Mood: Semi-repentant Sith Lord
|
|
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.
|
|
|
wg48temp9
National Hazard
Posts: 784
Registered: 30-12-2018
Location: not so United Kingdom
Member Is Offline
|
|
| 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.
I am wg48 but not on my usual pc hence the temp handle.
Thank goodness for Fleming and the fungi.
Old codger' lives matters, wear a mask and help save them.
Be aware of demagoguery, keep your frontal lobes fully engaged.
I don't know who invented mRNA vaccines but they should get a fancy medal and I hope they made a shed load of money from it.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
