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Author: Subject: Unanticipated reaction!
James Ikanov
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[*] posted on 12-7-2015 at 17:54
Unanticipated reaction!


Hello there, I was hoping I could find some help here with this.

I love to experiment with metal flash powders, usually based on pyro grade aluminum, and thermites. But I find the high ignition point of thermites obnoxious.

So, I undertook an interesting (and highlyhighlyhighly unproffesional) experiment, to sensitize the thermite till it could be ignited by regular flame.

I mixed a slurry of:
Pyro grade aluminum, German dark
Paraffin wax
Potassium Chlorate
A flammable petroleum distillate
CuO
and Ammonium Nitrate

Into a Steel soup can.

I did not record any of my measurements, as this was more a proof of concept to see if it was possible. I mixed them in rough proportions, then added a small amount of a chemical based on what I experienced as results from a small sample of the batch.

After a few days, I noted a purplish salt forming across the top of my sample. It looked similar to previous attempts I'd undertaken to synthesize TACN. I was nervous that I was going to have a problem with unintended consequences of having that in the mixture, so I set it aside for a few days to see if the reaction continued, partially from curiosity, and partly to determine if this mixture would have storage problems. Indeed it does, because there is now a much brighter blue, almost neon-esque crystal forming across the surface of my container and my mixture.

I believe it's a mixture of TACN and CNO3, but I don't know exactly what it is or what precautions I should take with it.

It's a rather large container, but most of it appears uncontaminated and it's in a well ventilated area. What should I do with this stuff?
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[*] posted on 12-7-2015 at 19:41


Where is it? How much is there? Is it inside a house or apartment? Are you placing others in danger? What an interesting combination to just toss together. Do you know the number for 911? Sorry to sound parental, but I am. :D

How about the haz-mat team? A quick $5000 or so might fix this. The Fire Marshal will want in on this one too, and ATF. :(

In general it is better to call the authorities before you kill someone rather than after. That whole easier to get forgiveness than permission thing, eh?

No notes? I would not have done this, and if I had, I would have anticipated that there is a chance for this to ignite in an unhelpful fashion, say indoors from a gas water heater or stove, or spontaneously, or even deliberately and done this in a bare field, with an ignitor handy to "neutralize" the "mix".

Copper Oxide thermite with some Potassium Chlorate tossed into some undefined flammable hydrocarbon, and ammonium nitrate.

I bet it has a couple of interesting burn modes- the quiet hydrocarbony one with black smoke and a few sparkles, and the incandescent exploding pile of dispersing glops of thermite changing from wet to gaseous disaster mode. :P

Nomex, cotton, gloves, leather shoes, a face mask, goggles and a helmet. No polyester on you at all. The plastic will fuse to your skin and require skin grafts over months.

Will the ANFO go off? Should just burn, but maybe the CuO thermite will be vigorous? Well, who knows!! You are certainly finding out! Let me know. :)

A few crystals of Potassium Permanganate and a drop of glycerine, placed on top of your test thermite, is a safer and reliable ignitor relative to ANFO and random accelerants.

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James Ikanov
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[*] posted on 12-7-2015 at 19:59


The proportions are not balanced to form ANFO.

Yes, test burns are somewhat inline with what you've described, and very interesting in terms of results.

There's a mixture of simple slow burning, followed by crackling, popping, aggressive sparking, and then a burn similar to very slow thermite.

And despite this being my first post, this is NOT my first rodeo.

I've done CuO thermite several times before along with a wide variety of flash powders and metal powder incendiaries.

You seem to have misunderstood the purpose; I wanted fuse ignitable thermite that can be safely stored. The ammonium nitrate itself does this job quite well, and I had several very successful tests with it; the problem is that I've experienced an unanticipated reaction between I'm guess the copper and the ammonium nitrate, which are all thoroughly mixed together homogeneously and bonded with wax.

What I'm asking for is if anyone could simply tell me, or at least take a good guess, at what sort of crystals have precipitated out of this and the hazards that may be involved in handling them , with the understanding that this is time sensitive as it's continuing to react and form more when left alone, something that is really rather not what I'm looking for.

I'm not looking for someone to try and talk down to me about how interested the Fire Marshal or Federal Authorities will be in my experimentation. I understand the risks of what I'm working with and being lectured on safety is not what is going to be helpful in this situation, although I certainly appreciate the... concern, you appear to have.
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[*] posted on 12-7-2015 at 20:06


I'd be carful with this mixture, chlorates and ammonium compounds aren't very finger friendly if you know what I mean - especially in combination with reducing agents. Dispose of it safely, by burning it, away from people and idiots.
Ammonium chlorate (which can form in minute amounts from combinations of other chlorate salts and ammonium salts) is very unstable, never store anything containing this.
If you want to make thermite easier to ignite, try adding a little potassium chlorate, no need for any of that other stuff. Better yet, put a small amount of flash powder on top of the thermite.




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James Ikanov
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[*] posted on 12-7-2015 at 20:15


I've done stuff with flash powder ignition before, it certainly does work.

I'll note the chlorate, thanks for the help.

Ammonium Chlorate was my primary concern, thank you for confirming my suspicions.

I think I'll go dig a pit and set it off remotely with some other thermite or flash.

For now it's behind a temporary blast shield.
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[*] posted on 12-7-2015 at 20:17


Yeah. Not that I am an expert in EM, but I would want to be disposing of that sooner rather than later. And I don't think I would want to be carrying it in a vehicle either.
I would put it in a safe place and ignite it with a small mound of KMnO4 and glycerine. That combination gives a reasonable ignition temperature and allows a good 30 seconds to stand clear. Who knows what you have crystallising. But the fact that you did not measure means that no one will ever know and there is not much point in hanging on to it to investigate.
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[*] posted on 13-7-2015 at 12:53


Blue. Copper? Permanganate?





Rapopart’s Rules for critical commentary:

1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
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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James Ikanov
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[*] posted on 13-7-2015 at 13:14


I'm not sure. It was, before I very hastily disposed of it, a shade of blue somewhere around this. It was very vibrant and almost purple, which made me fairly sure it was either TACN or a copper nitrate salt.

Looking at pictures of both types of crystals, I'm almost certain it was almost entirely copper nitrate with a small amount of TACN forming.

I was concerned enough that any formation of ammonium chlorate would cause all sorts of problems with spontaneous ignition, so I buried it about 3-4 feet underground, then flooded the left over divot with water. It is worth noting to me that the majority of the crystals formed on the side of the can and then the very surface of the material, which leads me to believe that the reaction was precipitated by environmental moisture. I think it might've been just copper nitrate.

[Edited on 13-7-2015 by James Ikanov]
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[*] posted on 13-7-2015 at 13:16


If you've got to handle it (and i guess you have) how about a photo before you destroy it ?

[Edited on 13-7-2015 by aga]




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James Ikanov
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[*] posted on 13-7-2015 at 13:17


Unfortunately, I've already buried it..... that said, I'm tempted to attempt to make a much smaller amount.... the color was absolutely beautiful.

Post garage search edit: I found a jar of an attempt to sythesize TACN, and it has a small pocket of similar color crystals. Here's a photo. Sorry for the poor quality.

The color of the previous Crystals was just slightly lighter.

[Edited on 13-7-2015 by James Ikanov]



[Edited on 13-7-2015 by James Ikanov]

[Edited on 13-7-2015 by James Ikanov]

Crystals.jpg - 445kB

[Edited on 13-7-2015 by James Ikanov]
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[*] posted on 13-7-2015 at 13:58


Keep better lab notes. Weigh or record volumes of reactants. If it had worked, you would have wanted to do it again...



Rapopart’s Rules for critical commentary:

1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
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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szuko03
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[*] posted on 15-7-2015 at 10:43


Seeing things like this make me cringe. I am not trying to be mean in any way but some people simply should not have access to things until they get some experience. Sure this wasnt bad this time but what would happen if it chose to spontaneously ignite in your room when you were not home? I would not want to live near you as creating things in a careless fashion like this can easily cause a fire and cause a threat to the apartment or neighborhood in a sense. Again I am not trying to be mean but the number of people who come here with no experience and ask dangerous questions can be concerning.

Whenever I have something that can do anything close to ignite I consider it active and either store it outside away from anything or dispose of it the second its made. It is simply not worth the risk in my mind to toss a bunch of stuff into a can and "see if it does anything" Get defensive if you will it just seems like a massive risk to no end,.




Chemistry is a natural drive, not an interest.
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[*] posted on 15-7-2015 at 13:23


The main thing is the OP is sharing information, and asking for help.

This means that they are learning, or ast least willing to learn.

I am sure that many things 'just get mixed up to see what happens' by people who don't ask here what the effects may be.

Bert's is the best advice :-

weigh everything, make notes of what you are randomly mixing up, how yo did that, what the temperature was etc etc.

If you'd made a block of pure Gold, you'd be a teensy bit annoyed if you could not do it ever ever again.

[Edited on 15-7-2015 by aga]




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[*] posted on 15-7-2015 at 14:38


Quote: Originally posted by aga  
If you'd made a block of pure Gold, you'd be a teensy bit annoyed if you could not do it ever ever again.


Aaaah. The accidental alchemist argument.
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[*] posted on 15-7-2015 at 15:16


Paraffin evaporates when heated to its boiling point. This may eject more chunks of material than otherwise, and is likely - by evaporative cooling, same as sweat, to slow burning, and could postpone ignition in higher amounts. Chlorate is probably unstable enough to offset that.

[Edited on 15-7-2015 by halogen]

[Edited on 15-7-2015 by halogen]




F. de Lalande and M. Prud'homme showed that a mixture of boric oxide and sodium chloride is decomposed in a stream of dry air or oxygen at a red heat with the evolution of chlorine.
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[*] posted on 16-7-2015 at 04:25


Aluminium is not compatible with moist NH4NO3 (catches moisture from the air)
NH3 and HNO3 formed as traces by moist NH4NO3 chew through the protective oxyd layer leading to naked reactive Al metal.
2 Al + 3H2O --> 3H2(g) + Al2O3

Potassium Chlorate and NH4NO3 are uncompatible owing to formation of unstable NH4ClO3, precursor of the even more unfamous NCl3 (very unstable and reactive with hydrocarbons what are precisely parafin wax and petroleum distilate

CuO reacts with moist NH4NO3 to form Cu(NH3)4(NO3)2 (TACuN) which may react with KClO3 to form Cu(NH3)4(ClO3)2 (TACuC).

Naked Al is uncompatible with Cu(2+) present in TACuN and TACuC because forming a battery in shortcut.

Thus too many uncompatibilities what leads to unpredictable behaviour...stability is very much of concern.
--> Big risks of spontaneous inflamation, fire and/or explosion.




PH Z (PHILOU Zrealone)

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[*] posted on 18-7-2015 at 13:24


Quote Szuko03:

"Seeing things like this make me cringe. I am not trying to be mean in any way but some people simply should not have access to things until they get some experience. Sure this wasnt bad this time but what would happen if it chose to spontaneously ignite in your room when you were not home? I would not want to live near you as creating things in a careless fashion like this can easily cause a fire and cause a threat to the apartment or neighborhood in a sense. Again I am not trying to be mean but the number of people who come here with no experience and ask dangerous questions can be concerning.

Whenever I have something that can do anything close to ignite I consider it active and either store it outside away from anything or dispose of it the second its made. It is simply not worth the risk in my mind to toss a bunch of stuff into a can and "see if it does anything" Get defensive if you will it just seems like a massive risk to no end,.

Quote PH Z:

"Aluminium is not compatible with moist NH4NO3 (catches moisture from the air)
NH3 and HNO3 formed as traces by moist NH4NO3 chew through the protective oxyd layer leading to naked reactive Al metal.
2 Al + 3H2O --> 3H2(g) + Al2O3

Potassium Chlorate and NH4NO3 are uncompatible owing to formation of unstable NH4ClO3, precursor of the even more unfamous NCl3 (very unstable and reactive with hydrocarbons what are precisely parafin wax and petroleum distilate

CuO reacts with moist NH4NO3 to form Cu(NH3)4(NO3)2 (TACuN) which may react with KClO3 to form Cu(NH3)4(ClO3)2 (TACuC).

Naked Al is uncompatible with Cu(2+) present in TACuN and TACuC because forming a battery in shortcut.

Thus too many uncompatibilities what leads to unpredictable behaviour...stability is very much of concern.
--> Big risks of spontaneous inflamation, fire and/or explosion."



So my take and analysis are pretty much right on. I truly didn't mean to patronize you, just scare you. I am not dead, but that is not for lack of trying. I have some serious insights into unfortunate choices, my own very bad ones, and others' (20 years in critical care and emergency medicine). Ask me about pulverone in glass.

Do I have the right to lord it over you like soooper parent? Nope. Never. I am thinking purely of myself and of my fellow neighbors.

I do have an instinctive defense of something I love (pyrotechnics) though, and it seems under external attack lately, some of that attack ever more justified by VERY VISIBLE idiotic behaviour. Mixing random stuff is dangerous. It just is. Sorry. :)

It used to be easier to kill yourself without it being overly remarked or particularly surprising (bless their hearts) when I was a kid, but with youtube, OMG. You can't do anything without it being social media worthy, and recorded, with an eye to stardom. Really? Nobody around here is a special flower. http://waitbutwhy.com/2013/09/why-generation-y-yuppies-are-u... if you care.

And the idea of you driving around with potentially explosive mixtures is alarming. :o

And I suspect ATF has seen this thread already. But why I stay careful and legal is how horrifying it would be to hurt someone because I was an idiot who kept making bad decisions. :o

Please don't be him (or her).

cb4july--22.jpg - 2.4MB
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James Ikanov
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[*] posted on 28-7-2015 at 14:12


Despite whatever impression you may have be given by my opening post (unfortunate it was this really, I've got a lot of other projects and questions I'm interested in sharing, and it seems this particular smear might hang around for a while.) I'd really rather have just let this alone, but.....

I do actually have some idea of what I'm doing.
For better or for worse I know a fair amount specifically about energetic materials, the safety of various compounds, things you should never ever do, and don't have as much depth in chemistry as I'd like, because it's just something no one seem to thought was important to teach me, and that I've struggled to find a simple resource on. I naturally gravitated towards something that actually interested me, and that was energetic materials.
My goal is to actually find new stuff, things that haven't been done or tried before, and I completely expect that I will encounter various levels of screw ups along the way, but yes, I do in fact have some idea of what I'm doing.

You seem to have the wrong idea about me. I entirely understand the personal risks that I'm taking by doing what I'm doing and I take a lot of precautions to make sure nothing goes wrong. I tried to make something I could find no particular resources on just to see what would occur, and it was certainly a learning experience for me.

No one was maimed, nothing bad occurred, and based on the proportions of the components I added (By the way, you may note that I specifically admitted this entire thing was highly unprofessional, but I digress.) the worst risk was fire... inside of a steel can that was left on a non-flammable surface surrounded by water.


The fact that you seem to not understand that what I did was very intentional and not just comprised of "random" stuff, but a specific mixture that I did actually do at least a tad bit of thinking on with a specific goal in mind is really rather insulting. Your concern was at first a welcome but perhaps condescending voice asking about safety precautions.

What you've reached now is essentially taunting and really rather obnoxious. Your continued implications that I'm either an idiot, or am going to maim or kill myself or others is at best impolite.

Go bother those people making organic peroxides with hydrochloric and no ice baths, not me because I made a mistake trying out a new and as I now know, deeply flawed experiment. You can't make any progress without fucking up at least once, and I'm certainly not going to apologize for something as small as this.

You are not scaring me, you're being condescending, and I really don't appreciate that.

Regardless, I appreciate the point and reason of your message. I've read all about people doing wonderful things like making an AN/NM "rocket" and trying to "fly" with it. I'm not that guy. Don't worry.

[Edited on 28-7-2015 by James Ikanov]

[Edited on 28-7-2015 by James Ikanov]
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[*] posted on 28-7-2015 at 14:43


You're being too hard on the SM comments, and yourself.

Some people here are Experts.

Others (like me) are Amateurs.

You'll keep on doing what you're doing no matter what anyone on this forum says, and it is not like there is any Law here.

If an Expert said to me 'do not do it like that, do it like this' then i would listen(or at least try it)

Some comments may sound Patronising, but some of us are Parents : it just means that they Care, and do not want you to Die soon, or Kill anyone else by accident.

In Pyro, The Experts are those that do it a lot, stay alive, and stay out of jail.

Personally i regard all the flashy-bangy thing as a dangerous waste of time.




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[*] posted on 28-7-2015 at 17:04


Aluminum+chlorate+nitrate+water = decomposition, generation of heat, release of ammonia and a possible ignition if a large enough mass is involved. Adding Copper makes this worse.

Google "Bill and Sue Hoyt"




Rapopart’s Rules for critical commentary:

1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
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 28-7-2015 at 17:11


Quote: Originally posted by Bert  

Google "Bill and Sue Hoyt"


Not sure what that yields that's relevant here.

What's surprising and dangerous is that among the wannabe 'energetic materials' creators are also some of the worst chemists. Good luck with that (you'll need it!)




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