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Author: Subject: Nitrogen Triiodide Problem
Hawkguy
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[*] posted on 2-2-2015 at 20:45
Nitrogen Triiodide Problem


Alright so this sounds like a joke but it seriously isn't.. I made some Nitrogen Triiodide yesterday because it seemed interesting, and I had never done it before right? Right. So I was partially drying it (inside) so I could bring it outside and not have to wait for like 2 hours... I kinda forgot about it, and now theres like two teaspoons maybe? Of NI3 on my table in the garage. I kinda just wanna hear suggestions about what to do, because spraying water on it doesn't seem like a great way to destroy (desensitize?) it. Main problem, is nearby shit breaking, as I don't have experience in NI3 brisance. As well, I pretty much live in the first little piggy's house of straw, so window damage in nearby rooms is a concern. Help.

[Edited on 3-2-2015 by Hawkguy]
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[*] posted on 2-2-2015 at 20:52


Good question. You can destroy it simply by pouring copious amount of Sodium sulfite solution. It reacts with Sodium sulfite solution and produces a mixture of Sodium sulfate, Ammonium iodide and little hydrogen iodide. Hope this helps :)

NI3.NH3 + 3 Na2SO3 + 3 H2O ------> 3 Na2SO4 + 2 NH4I + HI

[Edited on 3-2-2015 by Shivachemist]
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[*] posted on 2-2-2015 at 21:34


FYI: it blows up wet too.

You've got a tiger by the tail- been there. Lost my glassware.

Quote: Originally posted by Bert  
I don't know if there is ANY "good first synthesis" if you're completely new to it and on your own. But nitrogen triiodide certainly is NOT a good first lab.

I swiped a few grams of Iodine from the high school chemistry lab at age 16. Did the obvious thing with it, of course.

Performed the reaction with my mom's "clear ammonia" between getting home from school and going off to my part time job at a local restaurant. The batch was left drying on the filter paper, sitting on my desk- In my bedroom. Indoors. About 5' from my bed. With all my prized lab glass sitting next to it.

Bad planning, that.

When I got home, my lab glass was in tiny pieces all over the room. A LOT of it was in my bed... My dad was waiting up for me, drinking a beer and when he talked to me he was rather surprisingly calm and non-judgemental... All he said was: Don't make anything explosive in the house. Don't bring anything explosive you MAKE into the house. Good night.

The next day, my younger brother who had the bedroom next to mine told me that he had been horsing around with a friend, and banged into the wall separating our rooms. There was a large explosion on my side of the wall... He opened the door of his room just in time to see my father finish his sprint to my bedroom door. Dad opened the door and looked inside at the cloud of purple iodine vapor hanging over the ruins of my desk and said to himself out loud: "Oh. He knows how to make that now?"

Dad then closed my door and went back to the kitchen table, cracked a beer and continued sketching electronics circuits for his next day's work. Don't know how many more he downed before I got home that night-

It took me hours to clean up all that broken glass. If it had not gone off until I had come home and entered the room, I'd have probably suffered injuries from flying glass, possibly hearing damage and maybe lost an eye or eyes. I was as lucky as such a fool can be.

At Dad's funeral, his older brother told me the story about Dad getting arrested at age 13 for a fireworks experiment that broke a neighbor's window back before WWII. Guess it runs in the family.

[Edited on 8-4-2014 by Bert]




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[*] posted on 2-2-2015 at 22:44


No, this is to destroy NI3 before it dries. Also, I agree with you. This is not for newbies. This must be performed under expert supervision.
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[*] posted on 3-2-2015 at 07:52


Oh good it all worked out. No glass was broken, the detonation occurred during the night... Judging from plastic and whatever from the table it was on though, the explosion must have been crazy tremendous..
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[*] posted on 3-2-2015 at 08:01


By my estimates, it sounds like you have close to 42 grams of NI3 on your table? It has a density of 4.278g/cm^3, and 2 teaspoons is approximately equivalent to 9.86 cm^3.

Does that sound right to you?
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[*] posted on 3-2-2015 at 08:20


I hope so badly my son doesn't do this (or not in this way anyway) when he grows up and figures out how to get certain chemicals.



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[*] posted on 3-2-2015 at 13:02


Quote: Originally posted by phlogiston  
I hope so badly my son doesn't do this (or not in this way anyway) when he grows up and figures out how to get certain chemicals.


Best to show them under controlled conditions- Kids don't believe mere verbal and written warnings. I didn't. The OP didn't.

The parent's (universally effective!) curse: "I hope you grow up to have children who behave JUST LIKE YOU DID!!!"




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4. Only then are you permitted to say so much as a word of rebuttal or criticism.

Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).

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[*] posted on 4-2-2015 at 02:41


I have a son of 7 years old and sometimes I do some experiments with him and then I also show him the risks. I hope that in this way, he slowly will learn that doing experiment can be a very rewarding thing, but that it also is important to do things wisely and not to take unnecessary risks.

Having two spoons full of NI3 lying around does not sound like a wise thing to me. If I would make NI3, I would not make more than a pea-sized amount. Even such a small amount already can give a hefty bang.

@Hawkguy: Did you solve the problem with disposal of the NI3, or is it still lying in your garage. I really see no safe way of disposing of this. Maybe pack yourself in thick protective clothes and cover your ears with sound-damping ear-caps and construct a device on a LONG stick with which the solid can be taken from the bench very carefully. But doing this would scare the shit out of me. Another alternative might be to ask a professional company for cleaning up, but in that case you have a lot to explain and probably you also will have to pay a lot!




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[*] posted on 4-2-2015 at 07:21


It actually went off during the night, while I was sleeping. The reason I did so much was because I was like screw it Imma do this...
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[*] posted on 4-2-2015 at 07:23


Well, next time the "screw it, I'm gonna do this" might better be left unsaid. :)

I have only seen pea-sized amount of this detonated. What did ~42g of this stuff sound like going off?
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[*] posted on 4-2-2015 at 08:12


After grad school, my dad worked in a lab developing antidotes to nerve gasses, and there were many carts filled with cages of test rabbits around. Apparently, it was a common prank to leave a small puddle of NI3 drying underneath the cart, right in the path of the wheels.... poor bunnies...



Incidentally, several months after he left, it turned out that he'd never actually had the security clearance to work there. o_O





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Loptr
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[*] posted on 4-2-2015 at 09:33


Quote: Originally posted by mayko  
After grad school, my dad worked in a lab developing antidotes to nerve gasses, and there were many carts filled with cages of test rabbits around. Apparently, it was a common prank to leave a small puddle of NI3 drying underneath the cart, right in the path of the wheels.... poor bunnies...



Incidentally, several months after he left, it turned out that he'd never actually had the security clearance to work there. o_O



I bet the FSO for that facility got the boot!

[Edited on 4-2-2015 by Loptr]
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[*] posted on 4-2-2015 at 12:18


Nitrogen triiodide problems will take care of themselves.
Of course they will also take care of anything in the immediate
vicinity when they do. Best to make sure you aren't in that
radius.

Fortunately for most people, they don't have enough iodine on
hand to cause a really large explosion (ie. where did the house go).

In this case I am really surprised that more damage wasn't done
given the reported large quantity.
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[*] posted on 4-2-2015 at 12:42


I am not sure if these are accurate values, as I have had a hard time validating them anywhere, but I recall reading that nitrogen triiodide has a VOD of ~3000 m/s, and a lead block test of 350 ccm / 10 grams; however, I have a feeling these may have been values for NCl3.

I know very little about energetics, so this is just my recall.

[Edited on 4-2-2015 by Loptr]
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[*] posted on 4-2-2015 at 12:46


Quote: Originally posted by mayko  
After grad school, my dad worked in a lab developing antidotes to nerve gasses, and there were many carts filled with cages of test rabbits around. Apparently, it was a common prank to leave a small puddle of NI3 drying underneath the cart, right in the path of the wheels.... poor bunnies...



Incidentally, several months after he left, it turned out that he'd never actually had the security clearance to work there. o_O



I have also heard about this happening after someone leaves a black program, where they are essentially disavowed and all proof of their possible involvement destroyed. That way if they try and make any claims, they can be dismissed as another crazy.
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[*] posted on 5-2-2015 at 06:00


There are a multitude of lessons you can (should) learn from this close shave.

My parents stimulated experimenting to some extent, but strongly discouraged experimenting with anything 'energetic' on any scale, like most parents (understandably) would. I stubbornly did that anyway, in secret at first, but with their hesitant support later on when they noticed I was extremely careful and seemed knowledgeable. I abandoned it when I began to realiser the magnitude of trouble it might get me into when I grew up to the responsable adult stage.
So, there is a lesson I can use for raising my own offspring.

We have kids in the same age range, woelen. 4 kids here, girl of 7 years old, son 5, then twin girls of 3 years old. They are all incredibly curious and I can confirm that experiments are extremely entertaining and fascinating for kids of that age (even the 3 year olds).

I try to prepare them to some extent, but accidents happen and curiosity and enthousiasm are certainly able to prompt kids to try unwise things. I fully expect them to try to find out where the limits are someday.

[Edited on 5-2-2015 by phlogiston]




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[*] posted on 5-2-2015 at 11:59


this may be unrelated but it could help somewhat.
I have never really been interested by energetics outside of pure curiosity and maybe when i was younger ...
I did however made SMALL quantities of NI3 . and I noticed something interesting.
Maybe some of you have as well.
When done NI3 is wet and on the filter in a funnel and the funnel in a small beaker.
I did it in my basement and took it outside upstairs in the backyard where it would dry up.
Somehow there was ALWAYS tiny amount of it in my basement. that would snap when step on and it would always be in the same spot! at the bottom of the stairs...
I know nothing visible splashed out of the filter or leaked from the beaker ! so i have no idea how it would end up
there at all! I could cover the filter with my gloved hand while carrying it out and no NI3 would be on the glove but still 4 or 5 tiny beads of it would be on the floor of my basement ... almost everytime!




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[*] posted on 5-2-2015 at 12:05


There's ALLWAYS some of it left in the vicinity, and little "land mines" persist wherever this is made and exploded.

Maybe a lot of the other things we make escape too? The amateur chemist is not so informed by most other products of his synthesis, perhaps it's just the fact we can't overlook all the little explosions?




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[*] posted on 5-2-2015 at 12:49


i would agree if the explosion happened in the immediate vicinity but the bottom of the stairs and 3 trurns and 2 doors?
and the sink is a good 10 feet from the stairs and not a straight shot either.




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[*] posted on 5-2-2015 at 13:02


I noticed the same. Similarly, at work, I have always found minuscule droplets on my bench when working with intensely coloured solutions no matter how meticulously careful I am.

For this reason, I assume it is pretty much inevitable that you will contaminate your working area, especially in an amateur setting with often improvised equipment and rough handling. Should make you think twice about handling lead nitrate solutions etc. Especially with things like boiling, electrolysis (spray from breaking bubbles).

As anyone that regularly works in a lab where people handle solutions of radioactive compounds can tell you, the routine wipe surveys will occasionally pick up small amounts of contamination on various surfaces, that are not always reproducible upon re-checking. I've always assumed that this has a similar cause. Just tiny specks here and there.



[Edited on 5-2-2015 by phlogiston]




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[*] posted on 5-2-2015 at 21:37


Maybe the weird remnants would be understandable if I could see how they got there. I was sweeping out the garage just yay recently and there were those little NI3 bits everywhere, even in spots I did not tread across while preparing it...
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[*] posted on 6-2-2015 at 07:45


What about sublimation followed by condensation in cooler spots within the surrounding area?

I have read that nitrogen triiodide can be purified by sublimation at -20C, or would room temperature be too high to sublimate without significant decomposition?

[Edited on 6-2-2015 by Loptr]
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[*] posted on 6-2-2015 at 11:22


if you value your glassware and equipment i would not recomand any atempt at sublimation of NI3! even at low temp. -20 seems way too warm by the way.



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[*] posted on 6-2-2015 at 12:01


Quote: Originally posted by neptunium  
if you value your glassware and equipment i would not recomand any atempt at sublimation of NI3! even at low temp. -20 seems way too warm by the way.


I have no interest in ever attempting to prepare, or purify NI3, but thank you for the warning!

I was wondering if it could explain the bits of NI3 left about after its preparation, as mentioned in the above posts.

[Edited on 6-2-2015 by Loptr]

Inorganic Chemistry, by Egon Wiberg, Nils Wiberg, pg 641

https://books.google.com/books?id=Mtth5g59dEIC&lpg=PA641...

[Edited on 6-2-2015 by Loptr]
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