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Author: Subject: etn explosive Combination with tnt
Bert
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[*] posted on 12-2-2014 at 14:46


There was a person in Alaska? I recall who made several large batches of ETN, then melted them under hot water to produce a LARGE single cast charge. He had pictures of the process, which he posted to roguesci.org along with video of detonating that big block...

He claimed to purify his ETN by melting it in hot water and agitating the mass while adding baking soda to the water in a fashion similar to the way nitroglycerin has been neutralized by some, rather than dissolving in solvent and re-crystallizing. For the quantities he made, the solvent required would have run to many gallons and he didn't think it was worth the cost.

I don't know what became of him. Alaska is big enough so no one may have noticed the crater yet.




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Turner
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[*] posted on 12-2-2014 at 15:38


Yes melting ETN under water was also a possibility that crossed my mind. You can purify/stabilize TNT by melting it under water w/ some sodium sulfite and agitating it which makes the water turn reddish/brown, this removes unwanted TNT isomers I think.

[Edited on 12-2-2014 by Turner]
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[*] posted on 12-2-2014 at 15:46


Quote: Originally posted by roXefeller  
The trouble with ETN is it starts acting like a primary when its molten. Not instant detonation, but more sensitive. Would you be willing to stir 20-100 grams of primary? When you get larger amounts you might get more casual/complacent with it (for whatever reason) or not be able to give it the respect you can with 2g, and the negative side of accidental detonation gets worse than lost digits.




ETN acts like a primary when it isn't molten, SA*DS is less impact sensitive (as far as I can tell) than ETN but it is classified as a primary. I have done hammer and friction tests w/ ETN in molten state and noticed nothing interesting as far as change in impact sensitivity, but I should do a few more tests. If you ever heat ETN w/ a soft flame you'll notice it quickly melts, and then some time goes by before it heats enough to burn.



[Edited on 12-2-2014 by Turner]
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Zyklon-A
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[*] posted on 12-2-2014 at 16:08



Quote:

What do you mean leave outside?

To test the decomposition, my mom wont let me store any explosive in the house (Except maybe TNT, or other very stable material). I have a few places outside where conditions wont cause accidental detonation.




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[*] posted on 12-2-2014 at 16:38


Will not decompose just because it is "left outside" do you mean left in a warm environment? Recrystalized and stabilized/nuetral ETN will not decompose in storage
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[*] posted on 12-2-2014 at 18:01


I just wanted to try it to see how long it will last. I heard that even good ETN will decompose slowly, maybe a warm environment, it's not warm night now.;)

I guess it may not be worth the waist, it was just going to be a test.




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[*] posted on 13-2-2014 at 02:16


Friends, etn What is your view about the press?(Higher density) ?
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[*] posted on 15-3-2014 at 08:28


it seems that people are not just lucky, but actually have been capable of doing even LARGE amounts decently well controlled
i think its sad to see that people keeps having these bias'es but then again... energetics accidents are often quite .. energetic

in fact a person on this forum melted a legit primary: TATP under water to then let it crystallize, im quite sure he used exactly this massive crystal to crush.. it was filmed when he crushed it, and even tho i was quite sure it was gonna blow up, it didnt act much differently than a big sugar crystal

i think Turner might have something to say with that the ETN will usually go bang when in contact with aluminium or glass, could this mean the detonation of this energetic is favored by presence of potential fuels??

i have an actual idea for testing this out...
sugar could be cast into a can of some sort, then have a pen or similar small stick like object inserted into it then let cool

the hole could then be filled up with ETN, which would then when inserted into a fire or similar get the ETN molten, and it would then be in full contact and fully sorrounded with sugar, perhaps they would melt together??
the idea of this is to see whether ETN can and or will undergo detonation if its molten and a potential fuel is present.

note: the hole should not go down to the bottom of the can

i think if this was done, it could give some pretty interesting results, perhaps smaller experiments done later on testing molten ETN with and without fuels present

i know for a fact that ETN powder mixed with P4 has a lower DDT unconfined as it slightly crackles, i did not see any video but i trust my source, not to mention i recall other members discussing ETN used as primary with aluminium powder mixed approx 95 5 ratio by weight to make the chances of it going HE to increase




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[*] posted on 15-3-2014 at 15:28


Bert: The chap in Alaska had an accident which nearly killed him (I can remember some of the details that I was told, can always elaborate if needed) and took down all his materials. The authorities got involved with the situation, I remember finding a couple of articles online about it. If anyone happened to mirror his videos I would love to get at them.

I recall some melt methods being discussed over at roguesci.org as a possible purification scheme (most memorable was the over-complicated bit of glassware a member designed for it, until recently I had that image on a USB key until I lost it), some of which seemed similar to purification of silicon via melting. The melting in hot water seemed somewhat practical also.

A method I have heard of involves dissolving the ETN in hot basified (i.e. bicarb or similar added to) methanol, and actually using a food processor or similar to mix it. This was done by someone over on roguesci with MHN with a decent degree of success, they were of the belief that the mechanical mixing helped a lot with neutralizing the ester, followed by crashing into cold water to crystallize and another recrystallization to get the desired crystal form you wanted.

It has been a long time since I as much as touched an energetic material, but IIRC methanol produced easier handled crystals than acetone when recrystallizing MHN. Acetone would produce a powdery mess that was almost impossible to load easily, wheras methanol produced a more free flowing crystals with a "feel" similar to granulated sugar.

Probably entirely off topic, I apologise...
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[*] posted on 24-10-2015 at 09:26
ETN, proposal of procedure


Before proposing this process:
I apologize if I am posting flagrantly by some etiquettes, I have searched and found nothing specifically relating to this proposal and it's hard for me to tell (being new to contributing) how to tastefully amend my thoughts to existing topics. So. Here we are.

Much of my short work with ETN has mostly been in-lab versus a "synthesize, blow something up, repeat" approach. By dating my only other topic you know my tenure here and the relative brevity of my handling experience, but it has assuredly been quite involved. Based on my experiments with re crystallization I come seeking input on a process.

The objective of this process is to derive a highly purified product which is reliably very stable; existing in a clean form that is easy to handle and store, as well as convenient to work with.

The other night I had a dream... Only joking. I won't do that dream crap haha. Based on actual activities In the lab, the proposed process is as follows:

Rinse the filtered off crude ETN-- alternating between a solution of sodium bicarbonate in distilled water, then distilled water only. This is done thoroughly,and repeatedly until all foaming has apparently stopped; then once more with a long final rinse with distilled water.

The filter paper is laid out on paper towels and a second filter paper placed over the product. Another layer of paper towels is placed on top and the product is gently pressed to drive out excess moisture.

A hot water bath is prepared. The cake of crude ETN is gently broken up by hand and stirred into alcohol, deliberately over saturating the solution so as to have undissolved ETN swirling around as stirred. A vessel is prepared, containing very cold water (no ice), the volume of which is to be any excess of 10x the total volume of the ETN/alcohol mixture.

The beaker containing this mixture is then clamped and placed in the hot water bath and very gently stirred. The milky appearance of the mixture will give way to clarity as the temperature increases, at which point (proportionally dependent quantity of) sodium bicarbonate is added and stirred in. When the temperature has reached 61c the mixture is removed from the hot water bath and gently poured into the previously prepared cold water. The vessel is then refrigerated.

Due to the alcohol, the temperature is able to fall below 0 without freezing which (by my understanding anyway) will make any unprecipitated ETN less readily soluble. But even above 0 a white disk forms at the bottom of the vessel. This disk is comprised of small hard beads and the disk itself is rigid enough to be retrieved whole from the liquid.

A hot water bath is prepared again and the disk is dried gently by hand (it is mild in composition and will break or crumble if handled too aggressively) then broken up gently by hand. The pieces are placed in a beaker then melted via hot water bath.

The molten ETN is poured out on a sheet and allowed to cool. Residual moisture from the disk will separate readily from the molten ETN and therefore remain beaded up on the cooled sheet of ETN, and can be gently dabbed away with a paper towel.

The solidified sheet of ETN has an ivory color in my experience, and is patterned with overlapping starburst shapes comprised of long needles (apparently the natural crystal structure of ETN). The sheet is then gently broken up by hand into small "rocks"' which seems an appropriate term as at this point it certainly resembles crack. the rocks are laid out on paper until the slight alcohol smell is gone.

Thus concluding the proposed process

This rock form is most suitable for my needs. They store easily and are very convenient to work with. I've done a lot of hammer testing of the rocks vs crude product and the difference in sensitivity and potency (though admittedly difficult to quantify through just hitting things with hammers) is surprisingly stark. The rock form requires a much more rigid back surface and notably more force to set off by striking it, and can be nearly deafening in even minuscule quantities.

Thank you to anybody who has made it this far and please any notes or chemical insights are most welcome in refining technique.

Note: the liquid from which the disk was retrieved still contains ETN, which can be processed out. Waste not.

[Edited on 24-10-2015 by zeroberts]
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[*] posted on 24-10-2015 at 11:41


Allowing an excess of undissolved ETN in the solvent probably isn't the best idea, simply adding the ETN after heating would be safer.

Also, one recrystallization won't remove all impurities so two if not three recrystallizations is best.
I like to do the first one with 91% isopropanol as the solvent then crash into a cold solution of tap water and bicarb followed by a recrystalliztion with methanol then crash in a cold solution of distilled water and 2% urea.
This gives a product with very good storage stability that melts to a clear color.
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[*] posted on 24-10-2015 at 11:41


Quote:
Thank you to anybody who has made it this far and please any notes or chemical insights are most welcome in refining technique.

Stop this Darwin Award-chasing practice of melting ETN for a start ─ if you continue, the explosive will detonate in your face at some point!

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[*] posted on 24-10-2015 at 14:16


Quote: Originally posted by OneEyedPyro  
Allowing an excess of undissolved ETN in the solvent probably isn't the best idea, simply adding the ETN after heating would be safer.

Also, one recrystallization won't remove all impurities so two if not three recrystallizations is best.



Suggested amendment to process:
"Heat alcohol first then add ETN to the preheated alcohol"?

Also, my own fastidiousness prompts recrystallizing a second time but for the sake of my written procedure I will no longer regard this as a "me" thing but SOP.

Lastly, to hissingnoise:
Please do not interpret the following as cockiness or argument. I am here to learn; and discussion of data and fact cultivates understanding. Additionally, melting ETN is a controversial subject with many schools of thought, but little if any recorded data to provide hardline tolerances. So it is respectfully that I posit these points for review:
•Careful observation of temperature is intended to prevent the exceeding of ETN's melting point. A primary safety measure relying on physical property.
•Strict use of a hot water bath (and only hot water, ever) for heating is intended to be a safer and more gradual means of applying heat while also acting as a safeguard against dangerous temperature ranges, as the entire apparatus operates at temperatures well below the known deflagration temperature of ETN.

While I concede that precaution on principle has merit, there seems to be no definitive data behind an aversion to melting ETN.
Again, not arguing with you. And working with molten ETN feels like the grim reaper is watching me work over my shoulder. But then again my mentor in building fireworks taught me to feel that way when handling anything that burns faster than a wet rag.
Data data data. I kindly appreciate any data leading to a conclusion on the safety of melting ETN
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[*] posted on 24-10-2015 at 14:56


I like Bert.

Pretty sure most of the other members do too.

zeroberts would be Bad choice of username IMHO, seeing as it targets a specific member, also a moderator.

Let me guess ... zephrahim roberts ... zenaide roberts, you Wild Dove !




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[*] posted on 24-10-2015 at 16:48


Woww At first I was worried I had done something to offend and tried to smooth things over somehow. Then I realized what you meant haha.

My name isn't targeting Bert, it's comparing myself to Bert. I am worth zero berts :D

And no it's just Zach nothing so... Dovey..?
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[*] posted on 24-10-2015 at 18:04





Quote:

I am worth zero berts


"berts" are not an SI unit. Not yet, anyhow.

This is probably going to get merged with one of the (many) pre existng ETN threads. OP may want to suggest which one...




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[*] posted on 24-10-2015 at 18:06


Add the ETN to water, melt it by heating up the water, and cool it. This forms little rocks of ETN. This might be a more effective route, although usually some water is trapped in the rocks and they have to be broken up.
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[*] posted on 24-10-2015 at 19:01


This thread has become. Amazing. I'll give the water process a go.

Also has anybody come to offer any definitive quantifiable data regarding ETNs sensitivities and tolerances in a molten state? This is one I would really like to see put to bed. Some say melt to your hearts content. Some say never melt. I'm starting to see a lot of the Ford-Chevy paradigm.

A well pointed search and diligent reading through these boards turns up plenty of well sourced and cited data that lands on the pro-melt side. I'm not being belligerent here Im just saying raise your hand if you melt this stuff and keep your hand up if you would still melt it once somebody ponied up the data to show that the physical properties were not conducive to doing so *safely*
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[*] posted on 24-10-2015 at 19:25


It depends how pure your ETN is I guess, otherwise it might decompose on heating.
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[*] posted on 25-10-2015 at 15:37


Zeroberts, why exactly is the molten rock form more convenient? A nicely Recrystallized ETN batch can produce a dense compact free flowing crystal powder which in my opinion would be more user friendly as wel as being easier to fire. Another point is the nitration media, if mixed acid is used the results will be a more pure product than using a nitrate salt which leaves a sulfate salt as an impurity.
Individual crystals show decomposition more readily too.
is always the possibility it may fire when molten in contact with aluminium especially,but otherwise I have melted it in amounts no more than 15g and remotely just in case, except for the time I made a 22g melt casting in combination with PETN as outlined in a post by Mr anonymous found in the last 2 or 3 pages of this board. That was a nerve wracking procedure with very good results. These days though if I want a meltable explosive is make TNT and use it as pentolite or with RDX.
The risk is always present with ANY energetic material and if provoked they may bite back - hard.




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[*] posted on 25-10-2015 at 16:27


All the accidents involving ETN I've ever heard of are full of bad procedure or just plain stupidity, I alway see people bring up that guy who foolishly heated ETN in a test tube over an open flame which then detonated as if to imply it's proof that melting ETN is a bad idea...

As long as your ETN is acid free and you use a setup where the ETN can't get too hot I don't see the issue. Many here have a deep rooted superstitious fear of casting ETN but there comes a time when you need to seperate the overly catious bullshit and speculation from the reality of the matter.

My testing shows ETN at 65C to be noticably less impact sensitive than NG, I used to vigorously shake NG with water in a sep funnel to help purify it and I still have all my fingers :D

[Edited on 26-10-2015 by OneEyedPyro]
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[*] posted on 25-10-2015 at 17:46



Quote:

As long as your ETN is acid free and you use a setup where the ETN can't get too hot I don't see the issue. Many here have a deep rooted superstitious fear of casting ETN but there comes a time when you need to seperate the overly catious bullshit and speculation from the reality of the matter.



That's true. Many times I am overzealous with ETN, maybe with no reason, due to the stories of accidents when melting it.
The thing with ETN is the novelty lack of knowledge about its behavior.

Also something that gets on my nerves is, when I finish my synthesis and go to wash everything at the sink, some leftover ETN gets carried away by the water into the sink's water exit.
I have the fear of enough ETN accumulating in the pipes and exploding for no reason.
I don't know if there a better way to wash my glassware, or if I should even be concerned.
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[*] posted on 26-10-2015 at 05:49


500mg of ETN molten in a plastic vail using a water bath... OK, I could see that happening using a long stick and a big enough water bath so you don't blow it up (still you have the problem of boiling water flying everywhere).

But 50 grams? That sounds like asking for a surgeon looking for shrapnel in places you don't want shrapnel to be in the first place or just plain suicide.
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[*] posted on 26-10-2015 at 09:11


Tsjerk, what makes you so sure melting ETN carries any risk of detonation? It still takes a firm whack with a hammer to set off molten ETN.
Many on here won't touch a gram of molten ETN with a long pole but they have no issues with handling NG, it's ironic because NG is significantly more sensitive than molten ETN...
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[*] posted on 26-10-2015 at 17:19


Quote: Originally posted by NeonPulse  
Zeroberts, why exactly is the molten rock form more convenient?


Call it a long standing habit from building fireworks I guess. Grains > powder, in the fireworkers mindset.
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