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Author: Subject: Nitrogen Triiodide (simple set-up)
GreenD
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[*] posted on 30-4-2011 at 19:59
Nitrogen Triiodide (simple set-up)


So I have been wanting to make this stuff since I first saw it - love at first sight you may say. That was about 7 years ago (holy shit time flies!).

Anyways, a friend had came across some iodine crystals and I knew I had to make the stuff!

When I first saw it, my teacher had scared us and said it is impossible to make, it takes a long time, and it will explode on you. I took it to heart and assumed that the stuff needed very hard-to get reagents, and never really got around to looking at the procedure. Well, turns out there are two ingredients:

1. Iodine crystals
2. 30% Ammonium Hydroxide (lower concentrations work - but allow the reaction to proceed for longer)

Set up:

•Put a few milligrams of iodine (I eyeballed it for an amount the size of a fresh pea from the pod, so less than 100mg) in a small glass container (MAKE SURE THE CONTAINER IS EITHER A BOWL OR A BEAKER!)

If you use something like an erlenmeyer, the small opening may cause enough back-pressure to break the glass if an explosion were to occur.

•Pour and mix a decent amount (15-30-60 mL) of the aqueous ammonia into the container. The amount doesn't matter, really - you will be filtering off the solid anyway, but more is safer.

Contrary to belief, on scales this small it is relatively safe to pick up the beaker and start gyrating it, allowing the reaction to take place. Allow the crystals to sit in the aqueous solution for 5 minutes or more - just make sure that plenty of the liquid stays (no solid should ever be exposed to air during mixing).

•After the 5+ minutes get a funnel and filter paper and pour off the liquid.

Try to get off as much liquid as you can without actually pouring out the solid, i.e. try to keep the solid in the container, but pour off all the liquid.

•Once the liquid is removed [QUICKLY] remove the solid onto a paper towel, coffee filter, or filter paper.

It is OK IMMEDIATELY after the solution has been poured off to try to remove the solid by tapping the container upside down. However, this quickly becomes more danger as time passes. A safer route may be to use a scoopula and scrape out the solids - placing them on a paper towl or other absorbant media.

•Let the solids dry thoroughly for over 25 minutes. This gets longer with the more dilute your ammonia.

•eat. WAIT. NO DON'T EAT. Touch from a safe distance.

Discussion / conclusions;

After having done this I realized how slow the drying process is. When the product is in the aqueous media it is not very reactive at all, and in fact even when placed on the filter paper, a ball the size of half a pea was unreactive for some time (continual smashing did nothing for up to 25 minutes).

I became comfortable with the stuff and start to explode very small parts with my hands, it feels like someone hitting you with those popping throwing firecrackers, however the peices I was touching with my hand were about the size of a fruit fly.

Done on this scale, this is not a dangerous reaction at all, and in fact, I am not much more afraid of preperations of nitrous-containing compounds, as this procedure calls for no heat.

The reason I post this is because I found it hard to get a real good source on this website and it seems there is a bit of a fear of this reaction, and I wanted to demonstrate that it isn't in fact, as dangerous as some claim (ON THIS SCALE). The nitrogen triiodide is fairly stable in solution - in fact I've even seen people (and someone on here) have it stored in a bottle.

I would not condone anything even close to half a gram scale, or anything with a solid larger than the size of a pea.

[Edited on 1-5-2011 by GreenD]
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[*] posted on 30-4-2011 at 20:19


the way i did it was i put 100 mL of household ammonia solution with 1g iodine which i extracted from tincture of iodine, just be careful. let it dry where u plan to make it explode, i had a few mg of it explode in my lab when i tried to move it, thank god for goggles and gloves, i was scared shitless lol
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[*] posted on 1-5-2011 at 06:14


The reaction really doesn't seem to fear inducing. I think it is really just that novel shock value is the crystals only real efficacy. They are powerful and so stressed. It is really fun though. I saw it detonated by nudging the filter paper with a yardstick when I was in high school. The noise and instant purple cloud makes for a fun demo.

I have also heard that initiating a partially dried pile can scatter wet crystals about. To be found later.:o




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GreenD
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[*] posted on 1-5-2011 at 08:39


Yes - I was stepping on and popping crystals the entire demo, haha.

There is no real use for it other than novelty. One of my favorite noveltys though :)
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[*] posted on 1-5-2011 at 11:58


I believe that you can get it to dry quicker by washing with an alcohol.
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[*] posted on 22-6-2011 at 12:08


You never want to wash NI3 with water or any other solvent!! nitrogen triiodide forms an adduct with ammonia
NI3-NH3-NI3-NH3.... this is why the nitrogen triodide is stable when wet in ammonia, but when it is allowed to dry the ammonia leaves, leaving only NI3.. I tested this by (from a distance of course) washing wet NI3 with water to get rid of the ammonia. After about 200ml of water were washed through the filter paper some of the NI3 exploded, spreading NI3 everywhere making a fun residual crackling sound.
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[*] posted on 22-6-2011 at 16:30


Quote: Originally posted by GreenD  
So I have been wanting to make this stuff since I first saw it - love at first sight you may say. That was about 7 years ago (holy shit time flies!).


Here are being a slightly different method.

Leonard A Ford
Fun With Chemistry
Fawcett Publications
1959

A few years back on of my acolytes sent me a copy of the
Dover Publications second edition, revised by E Winston
Grundmeier. 1993.

"I have also updated some of the information. I have found it
necessary as well to make some substitutions of chemicals
to meet modern safety requirements."


Scanned from 1st ed.

Ford-Nitrogen-iodide-B&W-800.jpg - 282kB


Here is something to do with you nitrogen iodide in your spare
time.


Alpha Particles as Detonators.
Nature, Volume 109
June 10, 1922 p. 749

WHEN an alpha-particle passes through matter it may be considered
that the matter in the proximity of the path of the swiftly
moving particle is momentarily raised to a high temperature.
Looked at in this light the action of an a-particle may be likened
to that of a detonator and it may be possible to detonate a
sufficiently unstable substance by the action of these particles.
This has been found to be the case with the familiar explosive
compound, nitrogen iodide.

The experiment forms a rather striking lecture demonstration.
Nitrogen iodide is prepared in the usual way by the mixture of
finely ground iodine and strong ammonia and allowed to dry
overnight in the open air. On bringing a fairly strong radioactive
source (say the active deposit of radium) within 3 or 4 cms. of
the compound the iodide explodes. It may readily be shown by
the use of screens of suitable thickness placed over the source
that the result is due to o and not to ft or other rays.

Detonation is not caused by the first a-particle which happens
to strike the substance, but seems to be a probability effect.
With a button of nitrogen iodide of about o.1 cm.2 area a
source of radium-C equivalent in 7-ray activity to about 3 mg. of
radium placed i cm. away causes the button to explode in about
20 seconds, i.e. when between 107 and 108 a-particles have
struck it. Increasing the size of the button or the strength of the
source decreases the time necessary. Quantitative
measurements are not very accurate, as it is difficult to ensure
identical conditions of experiment. Doubtless other unstable
compounds might be found which would also be exploded in
this manner.

G. H. HENDERSON.
Cavendish Laboratory, Cambridge, May 23.
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[*] posted on 22-6-2011 at 16:58


Funny to see that page again after so many years. I must have been about 12 when I memorized that Fun With Chemistry page from my junior high school library. I've always wondered why so many other instructionals omit the KI.
Later in high school I convinced the vice principle and my chemistry teacher to let me buy the chemicals from the stockroom to make it. I kind of played down the explosive part of it to the vice principle, said it made more of popping, snapping like caps going off or something. I was a lab assistant and also allowed to borrow glassware, hot plates, etc. I remember getting a call at home from my chemistry teacher saying to be careful with it. I had made some after class earlier that day too with the teacher and a few of my fellow students, and drew a crowd outside the classroom from the loud explosions. That probably wouldn't fly in today's world. ha
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[*] posted on 22-6-2011 at 22:44


Try to get off as much liquid as you can without actually pouring out the solid, i.e. try to keep the solid in the container, but pour off all the liquid. = "decant".Silghtly more economical use of language




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[*] posted on 1-10-2011 at 14:58


I wouldn't be afraid of the explosive itself, rather, I'd be afraid of the cloud of iodine vapour it produces after detonating. Acid nibbling on the inside of you nose is never good ;)
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[*] posted on 2-10-2011 at 02:23


has anyone tried detonating this with an alpha source?

I remember attempting it a few years ago with one of those americium buttons from a smoke-detector but never could get it to work
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[*] posted on 2-10-2011 at 08:04


It is unfortunate for Americans and those in the eastern european countries, since pure iodine has become such a restricted chemical, due of course not to "terrorists" making NI3, but rather the proliferation of illegal drug making.

[Edited on 2-10-2011 by AndersHoveland]




I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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[*] posted on 2-10-2011 at 14:23


Can alpha detonate wet NI3?
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[*] posted on 2-10-2011 at 16:36


I'm not sure, as with all things, it depends on intensity. You can't levitate a drop of water over a fridge magnet. But if you put a drop of water inside the field of a 18T superconducting electromagnet, surely enough, it will levitate.
If you bombard a sample of NI3 with alpha particles from an americium smoke detector unit, it won't detonate. Put it into a beam of a particle accelerator and it will detonate:)
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[*] posted on 3-10-2011 at 11:29


:D dry NI3 explodes because you look at it, to my mind iniating it with alpha not important.
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[*] posted on 11-10-2011 at 10:26


One of the properties of NI3 that I always found amusing was that when wet, it will soak into porous materials without detonating. My chemistry teacher in high school particularly liked dipping sticks of chalk into wet NI3, letting it soak for a time, then taking them out and letting them dry in a fumehood overnight. Trapped in the chalk, the NI3 was a little bit more stable, enough so that he felt comfortable picking up the chalk sticks (with leather gloves) and walking outside to toss exploding chalk sticks at the sidewalk.

A side note along these lines: No seriously, be careful with how you dispose of that filter once you're done.
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[*] posted on 12-10-2011 at 12:06


Zander:

I heard this one guy used to paint telephone poles in NI3 so that the squirrels would get one hell of a scare:)
There are so many things this explosive could be used for. But unfortunately the cloud of iodine that results from the explosion is more hazardous than the explosive itself, too bad.




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