alexzxz
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Well I F***** Up.
So I'm typing this at 4AM, because at 3AM I was woken up by the sound of an explosion in the next room. I had attempted to synthesize ETN using 220ml
(50%) Sulfuric acid, 15g of erythritol, and 45g of ammonium nitrate. This was all done in a plastic bottle (water type not soda) and the reaction
didn't seem vigorous at all, since I had heavily diluted the acid. Pretty much no heat was produced and the ice bath was almost unnecessary. Since the
reaction looked pretty stable, I just capped it, set it aside and went in for the night.
Maybe a buildup of gas pressure since I capped it tight, maybe temperature related, i don't know, but the whole bottle blew up, spraying very acidic
solution all over the room. I think I found bits of the bottle mouth and the wrapper and that's it.
So I got a mop and some baking soda and cleaned out the area a few times. Then took a spray bottle with a highly saturated solution of baking soda and
spray down every single spot I could see/hear till no more fizzing. Right now, I've got a dehumidifier running in the room. Probably not going to get
much sleep tonight...
Thank god:
-that it was a wet explosion, so much of energy was dissipated and there was no property damage (maybe the wood floors)
-the 3-4g of TATP in a nearby cabinet wasn't set off (I had decided to submerge it under rubbing alcohol previously for anti-shock storage safety)
-the sulfuric acid was low concentration so there weren't that many burn marks (there were some)
-I wasn't close when this happened.
I've always thought I played it pretty safe when it came to energetic materials, but apparently it's never enough. Never thought I'd have my own story
to tell.  At least it doesn't involve mutilation.
Anyone know what went wrong?
Also, the whole place smelled pretty strong, and I was cleaning up with only a dust mask, any health issues I could have, medication I could take?
[Edited on 11-6-2016 by alexzxz]
[Edited on 11-6-2016 by alexzxz]
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greenlight
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Is this a joke?!
I think everything you did was wrong but I list the main ones. Where do I start.
• Sulfuric acid concentration is too low (but I think thats the least of the problems).
• Reaction with corrosive acid done in a plastic water bottle instead of proper glassware.
• You sealed a container that would have been generating gas/fumes hence pressure buildup and rupture of container.
• There is no mention of addition rate of the erythritol to the nitration mix. Do you know what a runaway reaction is? It seems you just threw
everything in together and hoped for the best.
• No mention of any method of stirring of the nitration bath.
• You appear to have run this reaction which produces poisonous fumes in a room that you sleep in!?
• You left this reaction to run on its own without watching it.
Was there brown/red gas given off and in the room after the bottle ruptured? Did you breathe it in? If so my main concern would be going to a
hospital. This is nitrogen dioxide and can lead to DELAYED pulmonary oedema.
I think a lot of reaearch would be needed and some proper glass is required before attempting this again.
[Edited on 11-6-2016 by greenlight]
Be good, otherwise be good at it 
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alexzxz
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I thought a lower sulfuric acid concentrate would make it more stable, or does water content influence the reaction? Yep, did not do enough
research there.
Polyethylene is rated usable for the sulfuric/nitric acid as a temporary disposable vessel. I do have glassware, but didn't pack them for a
relocation.
Sealing the container was a horrible idea in retrospect.
Erythritol was slowly added over a 10 min period, and gently swirled.
It was in the next room, which is the open living room area.
Yep, will DEFINITELY watch it from now on. It appeared fine for 20-30 mins before I put it away. I guess the pressure built up over a 3 hour
period.
I don't know if there was a brown/red gas since it might have disperse from the explosion. It's in an open area, so it might have dispersed very
quickly. Either way, there were plenty of opportunities to breath in whatever there was while cleaning. I will now go seek medical attention.
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Lotilko
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Glad you didn't lose your fingers. Remember, nitrate esters are no toys. You should try RDX instead. A much safer alternative.
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PHILOU Zrealone
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Usually for esterification/nitration reactions it is a bad idea to allow for longer exposure time in acidic media (so a night after process even if
diluted is bad news)...once finished usually one wash with water (or mild Na2CO3 water) and recrystallize for storage.
Runaway is always unexpected everything seems right and cool ... and a few seconds later everything is out of the beaker in Brown NxOy fumes and
extremely hot.
A good idea of this runaway effect (to perform outside in a vented open large area) is the reaction of formaldehyde (formol) and HNO3 or the reaction
of aceton (or isopropanol) and HNO3...after a short delay (depending on concentration of the réactants, of the initial T° of those, of the external
T°, of the thermic dissipative power of the recipient, of the size of the batch and of the agitation)...if one or more of those single parameters
(but the agitation) goes up, the delay goes down (can be as short as a few seconds and as long as minutes).
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Tsjerk
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I guess the reaction never started because of the low concentration sulfuric, hence you didn't see any temperature changes during the addition.
Sometime at night it decided it would be a good idea to go, filling your bottle with gas. Maybe good you closed the bottle, now at least the bang woke
you up instead of letting the NO2 slowly giving you an oedema.
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greenlight
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* No, the less water in the reaction the better thats why 98% Sulphuric is used. A stable product would be synthesized through temperature control
and thorough washing of the finished explosive and recrystalization.
* Proper glassware would probably still be best.
* Did you use a thermometer to keep the temperature under a specific Degrees C?
* You might be fine if it took 3 hours to burst. The way you explained it was like it happened a short time after you added the reagents and capped
the bottle so i thought it was a runaway reaction. The nitrogen dioxide gas would have been noticeable as it is heavier than air and seems to flow
down and along bench tops instead of rising up.
Better to be safe though.
Don't leave reaction like this unattended as well, I once did it with nitroglycerin when I was young and it had a runaway and I have never done it
since.
Be good, otherwise be good at it
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alexzxz
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The more I read about it, the more I'm convinced it was a delayed runaway reaction just like you guys said. I'm guessing the more water there is the
longer the delay is, causing the solution to appear stable for hours.
Me thinking that diluting the acid would make the reaction smoother is like shooting myself in the foot.  Yeah, I need to brush up on certain aspects of chemistry. Been years since I took the courses.
As for health, I went to the hospital to get checked and they said I was fine, breathing seems ok, oxygen levels checked out with a few tests. One
doctor explained that what I was smelling/irritating throat was probably the acid burning the wood floor, or perhaps there wasn't enough exposure, so
my trachea was affected, with very little going down to my lungs. Definitely will not attempt this again before getting a respirator and some better
equipment.
I was a little overzealous with the baking soda spray and now there are white splotches everywhere...
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greenlight
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Yes, I think the water would have had something to do with the delayed reaction.
I would crash it into water and filter and wash the ETN after the addition and period of stirring instead of leaving it overnight as well like PHILOU
said.
Good to hear that you lungs are fine. The white fumes given off from the nitration aren't lethal but still not good to breathe.
Just watch out for the red/brown fumes in the future which will usually evolve from the mixture during a runaway or on the synthesis of some
explosives where periods of heating are involved (I noticed them when synthesizing trinitrophenol during the heating stage but I was outside with a
respirator).
[Edited on 11-6-2016 by greenlight]
Be good, otherwise be good at it
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Daffodile
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Quote: Originally posted by Lotilko  | | Glad you didn't lose your fingers. Remember, nitrate esters are no toys. You should try RDX instead. A much safer alternative. |
The reaction to make RDX from Hexamine is really prone to runaway. Also he would need to make a primary anyhow to test its brisance.
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NeonPulse
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Holy shit. I never thought that people out there would still be so reckless with this stuff. Mistakes can kill you or worse blind or like the very
unfortunate accident with Yamato in his thread. You are very fortunate! Nitration mixtures can cause fires too in the wrong things are hit by them.- I
guess you obviously know you botched it but you really need to take care!
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ecos
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don't leave any EM in acidic solution more than necessary.
did you use ice bath ?
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CharlieA
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If the OP has to ask if water can influence/affect a reaction, I submit (in all seriousness and without any sarcasm) that it is time to get a new
hobby. Leaving any chemical reaction untended (let alone one that is knowingly supposed to produce an explosive product) shows a complete lack of
understanding anything about chemistry.
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Bert
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Thread Moved
11-6-2016 at 18:52 |
hissingnoise
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| Quote: | | As for health, I went to the hospital to get checked and they said I was fine, breathing seems ok, oxygen levels checked out with a few tests. One
doctor explained that what I was smelling/irritating throat was probably the acid burning the wood floor, or perhaps there wasn't enough exposure, so
my trachea was affected, with very little going down to my lungs. |
What cover-story did you give them?
Just curious...
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alexzxz
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I told them I spilled a half a bottle of drain cleaner everywhere and had some exposure to the fumes when cleaning up. Half-accurate. Whether they
believed it...who knows? Quite a lot of hospital staff have a filter for BS.
Haven't messed with energetics since. Currently waiting for safety equipment to be shipped before attempting any further experiments.
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crazyboy
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Making 15g of ETN in a plastic bottle and leaving it sealed unattended? You should refrain from the synthesis of explosives in the future. I'm sure
you feel quite stupid as is, but this is the kind of judgement that in another situation could well have maimed you or removed you from the gene pool.
You should give some serious thought to the prospect that you lose a hand or worse, for the thrill of making some energetic material.
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