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Turner
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[*] posted on 26-1-2014 at 13:39
Warning to All


Be careful what residues of explosives you leave behind in your work area. Today I was making silver nitrate from a few silver coins I had. I distilled nitric acid and then diluted it to about 65%. I put the coins in the acid and began to use heat to start the reaction. It got going pretty well and once it was warm enough it was violently releasing NOx gases so I took the beaker off and set it down on the wood surface, about 30secs later I set the beaker on the metal heating surface and BANG, next thing I know nitric acid has splashed everywhere and is boiling vigorously on the plate and my garage is completely filled with nitric acid fumes.

here is the result:







I think what happened was when I set the beaker on the wooden bench it picked up some sort of tiny amount of ETN from a long time ago, even though I have wiped and cleaned the surface of this wooden bench many times since. As the warm beaker touched the VERY hot metal surface, the ETN stuck to the bottom of the beaker (1mg?) detonated with enough force to break the beaker allowing the nitric acid to spill out, but thankfully not enough to send tiny glass fragments.
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macckone
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[*] posted on 26-1-2014 at 13:47


Wood + nitric acid + heat -> potential nitrocellulose
If you have been doing nitrations and there has been spillage,
your workbench itself may be explosive.
Other spillages could also be a problem.
That is why most lab workbenches are phenolic resin.
It is very unreactive.
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Dany
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[*] posted on 26-1-2014 at 14:02


The only one who should be careful is Turner.

if a small quantity (few milligrams) of ETN can do such damage, imagine what ten's of grams of cast ETN will do if it detonate...

Dany.

[Edited on 27-1-2014 by Dany]
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NeonPulse
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[*] posted on 26-1-2014 at 14:42


Its reasons like this that I work on a thick sheet of perspex and after the work is done it comes off the bench and is hosed off completely. No residues are left. And any work with powder or crystals is done on a sheet of black card.Glad it wasn't any worse for you Turner, although spilling nitric acid sux to clean up.



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NeonPulse
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[*] posted on 26-1-2014 at 15:29


Its reasons like this that I work on a thick sheet of perspex and after the work is done it comes off the bench and is hosed off completely. No residues are left. And any work with powder or crystals is done on a sheet of black card.Glad it wasn't any worse for you Turner, although spilling nitric acid sux to clean up.



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caterpillar
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[*] posted on 26-1-2014 at 16:15


Residues of explosives on your own table? That's cool! Have you ever seen "Vertical limit"? Pools of liquid NG on the floor of storage. You should learn by their example.



Women are more perilous sometimes, than any hi explosive.
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BromicAcid
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[*] posted on 26-1-2014 at 16:26


Used to be much more common, perchloric acid has a long history of causing such mishaps. Spilled and dried on wood it might sit for weeks, months, or years before someone scuffs it just right and it suddenly goes up.



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Turner
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[*] posted on 26-1-2014 at 19:35


I strongly believe what exploded was not NC.

I made the mistake of discounting Mg amounts of ETN as not capable of causing any problems to speak of. I used to do burn tests w/ ETN on the wood there and sometimes not all of it would burn, but just melt and then harden in that spot. I think I set the warm beaker on the wood in a spot that may have had some piece of ETN that may have melted onto the beaker, as soon as the glass beaker touches the hot plate, BANG and then all 50ml of that nitric acid instantly boiled off into heavy chocking fumes and splattering around.

At the very worst I am out a pyrex 250ml beaker that's all.



[Edited on 27-1-2014 by Turner]
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Zephyr
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[*] posted on 26-1-2014 at 20:33


Quote: Originally posted by Turner  

At the very worst I am out a pyrex 250ml beaker that's all.


And you got hot nitric acid everywhere!
I, and as it seems everyone else, work on phenolic resin covered wood. Maybe next time you should do explosive tests outside or at least on a metal sheet? Good luck salvaging the precious silver nitrate.




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[*] posted on 27-1-2014 at 00:12


Can happen to anyone. That's why I say safety glasses every time. A lot of fresh water must be around.
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[*] posted on 27-1-2014 at 00:18


Always keep your workstation clean and organised....jeesh, especially with energetics involved. I always cover the bench with paper or plastic wrap that I can discard afterwards. Keeps most of the spills from seeping into the table. If possible the tabletop should be permanently made of (covered) with a nonabsorbent nonreactive material: PP sheet, PE sheet or tiled over with glazed ceramics.
I also learned the hard way in the beginnings....forgot a small glass jar with residues of KClO3 and carbon black on the tabletop. Which I also used for welding, by the way (the stupidity). You can imagine what happened when a stray spark hit the jar dead center. From that day on I never leave any residues, spills or leftovers from any experiments sitting somewhere to be forgotten and then rediscovered in a most undesirable fashion.




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Zyklon-A
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[*] posted on 27-1-2014 at 05:59


Whenever I make energetics, I keep all my materials on a disposable plastic sheet, anti static spray if necessary.
Then once a week, I go to a safe place, and burn all of that weeks worth of plastic sheets, sometimes I'll hear a pop or a bang as it's burning.
I haven't had any accidents that I can remember...

Quote:

The only one who should be careful is Turner.


No... The only one who should be careful, is everyone. He is the only one who had the accident AFAIK, but he is trying to warn everybody to be careful. I think it's better to learn from other peoples mistakes, that way maybe someone else may not end up with a broken beaker and hot nitric acid splattered all over his/her lab.

[Edited on 27-1-2014 by Zyklonb]




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Fantasma4500
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[*] posted on 2-2-2014 at 06:55


hoard some newspapers and when you handle ETN then have newspapers as surface below beakers or whatever you handle it in

we can all the armchair warriors telling you exactly what you did wrong, but shit happens, and if it doesnt, then its probably just building up for one big shitstorm waiting to be unleashed on your most unlucky day.. (:

i think if you ever have a spill in the future you could take advantage of that ETN is hard to get out of acetone when first dissolved in it..
1:1 mix acetone:water should be effective for removing any ETN residue..

infact, i recall having heard somewhere that ETN from acetone that has just been let evaporate off cannot be heatshocked even with a butane flame, packed in aluminium foil??




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