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Author: Subject: ETN: almost killed myself... READ!
aquaregia
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[*] posted on 6-6-2011 at 03:00
ETN: almost killed myself... READ!


gentlemen.
I am just out of hospital where they spent a great many hours taking glass shards out on my body under general anesthesia..
I read, every forum, every patent on ETN nitration, and successfully nitrated 50g of erythrol disolved in H2SO4, by adding fuming NO3H to it as per Bergheim in a ice bath. This worked well, I recrystallized the ETN twice and got it quite pure. I did a hammer test on the low density cristals, and that was not conclusive... So, I melted the material in a test tube, by dipping the test tube in hot water, and then poured it in a mold to makehandy inch long cylinders. hammer test of the cast ETN was successful (strong report). I had finished casting all my ETN, and all was left was a sliver of material solidified inside the test tube; a few milligrams, at best. I do not know why, but, instead of boiling water again, I applied the flame from the bunsen to the test tube to remelt what was left of the ETN. I knew I was fucking up, but thought:"the quantity is so small". Here is the result:
<img src="http://www.sergepetiot.com/wp-content/gallery/various/me2" width="600" />
<img src="http://www.sergepetiot.com/wp-content/gallery/various/me1" width="600" />
The little ETN there was went high order, and I saw a flash of yellow flame, then the blood on the floor (on my arteries had a hole in it). I ended up with hundreds on pyrex shards in my upper body. I am lucky it was not my face. You are all experts. You know what you are doing. I thought you needed to see this. I was very lucky.

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: reduced image size(s)]

[Edited on 30.10.13 by bfesser]
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azo
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[*] posted on 6-6-2011 at 03:39


i hope this is a warning to others , not to be as stupid as you
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[*] posted on 6-6-2011 at 03:41


Very brave of you to post. I don't think I would have.

Oh, and Azo, shut your pie hole :mad:
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azo
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[*] posted on 6-6-2011 at 03:52


I didn't mean stupid for doing it ,i ment not for providing protection for yourself.
I suppose it is like adding sodium cyanide to hydrochloric acid with no fume hood ,you wouldn't do it ? WOULD YOU
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[*] posted on 6-6-2011 at 04:24


Thanks for posting aqua. I'm glad it wasn't worse. Glad you have your eyes and digits.

Get well soon and try not to dread over it to much. I know from experience that the psychological aftermath of a mistake like this can last much longer than the physical damage. You are brave to have posted. Most people never come back here after an accident like that I bet.

[Edited on 6-6-2011 by Bot0nist]




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[*] posted on 6-6-2011 at 04:26


I think it is actually the *non*-experts that need to see this :-). Anyway, thanks for posting. This is why I don't mess with energetics: I can readily see myself having just the same sort of brain fart you did (I'm not by nature a careful and methodical person)...

@azo: physical protection would obviously have helped here, but it is not a substitute for sound judgment, and might actually lead some people to make even worse decisions. I think it makes sense to focus on the obviously avoidable error (heating with open flame).
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aquaregia
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[*] posted on 6-6-2011 at 05:21
I had to post


This is actually more for the "non experts" (like me) I had to post this. It is all very well to talk about energetic materials, but people need a reminder of what a few milligrams do... Nobody, nobody, is safe from making a stupid mistake, even experts. All too often, the price to pay is your life. I am lucky, so for me, chemistry is over, I'll concentrate on my wife and kid instead. If someone wants my glass, they can have it cheap. I'm in France. just send private message.
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[*] posted on 6-6-2011 at 05:37


It's a shame to hear about your accident, I hope you recover soon!

This why one should avoid HEs (like I do, I never make any, not even mg amounts). One small mistake can have so much more serious consequences than other chemistry.
This also proves that heating even very small amounts of energetics in test tubes is not safe. If I would ever do this chemistry, I would use plastic (HDPE) beakers, not glass.

I don't see the purpose of making HE's. Yes it might give you a good feeling to make an explosion, but it's too dangerous . It's only a few compounds most members here make (exclusing Axt and a few others), so chemistry wise it's not that interesting, and it seems it's only for that BOOM!. That's asking for trouble.
Most chemistry hazards are not immediately life threatening, yes you might burn yourself or if you make a very stupid mistake (wich you can avoid by planning everything and using precautions) you can poison yourself. HE's are much less forgiving, one mistake and you can end your life or lose limbs.
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[*] posted on 6-6-2011 at 05:49


It's inappropriate to call someone names who has the courage of his convictions in displaying his mistakes.

When someone admits he has made a mistake and put that "on front street" it's obvious that he is doing so to show how dangerous something can be. This is NOT typical! Typically the injured individual slinks away and never communicates again.

If you would like to see just how fucking angry I can get - just call this man names.
Anymore name-calling & there will be problems.....I hope that is DAMN CLEAR.

His actions were ill thought out and he knew it yet he made extreme errors in judgement. He also was honest enough to publicly display his mistakes to benefit those who may mis-judge experiments with energetics. His honestly is commendable; his judgment was not....PERIOD!
Name calling in this instance makes me seriously angry. Gentlemen; to sit on the sidelines (and do so) is NOT science.

ONE mis-calculation with energetic materials can be enough to loose eyes, fingers/hands, genitals, etc. It HAPPENS - SO OFTEN that the majority here don't realize it.
One of the major thrusts of this forum is learning science and NOT practical applications. Lab safety cannot be stressed too much BECAUSE we eventually become lax.
Sometime back I discussed the concept of NEVER working with materials if you feel the least bit "off" that day. If your mind is elsewhere, if you are pre-occupied, or tired - whatever. I would be willing to BET GOOD MONEY that everything I had outlined the OP knew.

This is very important thread. The issues were containment, particle size/weight, stimulus, and proximity. IF you gentlemen are going to discuss this in elements of science then do so. And do so with the knowledge that the OP put himself out there for potential ridicule to PREVENT this from happening to others. However I will NOT allow this man to be ridiculed & I hope that is damn clear!

The MOMENT you think this can't happen to you is the very moment that it can! That is one of the first things taught in a variety of professional settings, so let it also be known here as well.





[Edited on 6-6-2011 by quicksilver]




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[*] posted on 6-6-2011 at 06:06
now to the core of the subject


Thx quicksilver.
which now brings me to the core of the post, which is why did this happen?
Believe it or not I worked for 10 years perforating oilwells with RDX or HMX shaped charges, 80 grain det cord, set off by fluid desensatized dets or EBW, so I do know explosives. In my mind ETN IS NOT a secondary explosive, as a secondary would ignite and deflagrates upon heating, and definatly not go off high order. ETN, even though we know it is the most sensitive to shock of secondaries, behaves like a primary when hot. Or at least, it shares alot of a primary properties. would anybody agree?
what happens when heating other secondaries like TNT, RDX, HMX for example? Has PETN the same properties? if so, I am surprises penthryte is used by the military, as a battlefield, can be very hot!!! image your own shells going off left right and center?
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[*] posted on 6-6-2011 at 06:20


We have some complications in the premise as the material was heated, enclosed, etc. While ETN, MHN and similar are "boarder-line" as some would say in their extreme sensitivity. Our application of heat was via thin walled glass which spread the temp quickly - YET it also [this application of heat] did not allow for a flame front to exist. Melt castings in this simplistic manner are very dangerous with sensitive energetics as it brings into the agenda high levels of heat with no cooling factors such as water. Had the same level of heat been disbursed and water being a mitigating factor this may have an entirely different outcome.

High-sensitivity esters can appear to function as primaries & often a reasonable "cut-off" line is sought. There are occasions where such a line is blurred due to application circumstances.




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[*] posted on 6-6-2011 at 06:42


It's a horrible accident you went through, aquaregia.
I'm glad you are reasonably unharmed.
Several years ago when I became interested in chemistry as a hobby, it was like for many others as a result of my interest in pyrotechnics. All I had in my mind were things that went boom.
One time I tried to light a really small pile of CuO/Al thermite, about 0.4 g. I lit it with a handheld torch, even though I had read online about the violent behaviour of this composition, I underestimated it.
It went of with such a fast and violent flash, that I had a stain in my vision for the next 10 minutes or so.
Then I got thinking that I might as well have ended up with a droplet of molten copper in my eyes.
i could not believe how reckless I was.
This so called accident changed my view on energetic chemistry. And I decided that i'll never synthesize high explosives. If I want a boom, balsa ballmilled blackpowder is more than suitable, I do somewhat regret that I never saw a first person detonation, but I'm not willing to take the chances.
Years later, I grew up and even though my interest in explosives is still there, it's only about reading on them.

oh, yeah, your honesty about sharing the accident is admirable
i hope you have a fast and full recovery

[Edited on 6-6-2011 by condennnsa]
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The WiZard is In
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[*] posted on 6-6-2011 at 06:49
Welcome to La Club


Nitroglycerin — Ascanio Sobrero

On one occasion a small quantify of an ethereal solution of nitroglycerin
as allowed to evaporate in a glass dish. The residue of nitroglycerin was
certainly not more than 2 or 3 centigrams. On heating the dish over a spirit
lamp a most violent explosion resulted, and the dish was broken to atoms.
On another occasion a drop contained in a test tube was being heated when
it detonated with great violence, and pieces of glass cut my face and hands
severely and also injured others standing some distance away in the room.

Ascanio Sobrero "Some New Fulminating Products Obtained by the Action of
Nitric Acid on some Vegetable Organic Substances." Torino. Mem. Acad.
(1847), 195-203. In: GW McDonald "Historical Papers on Modern
Explosives." Whittaker & Co. 1912

----------
EXPLOSIVE POWER OF NITRO-GLYCERINE.

An instance of the extraordinary explosive power of a small quantity of nitro-
glycerine is recorded by Dr Gorup Besamez. The incident was the explosion of
only ten drops of the substance in his laboratory, and the astonishing effects he
records as resulting from this explosion are well calculated to give a most
respectable and respectful notion of the properties of nitro-glycerine. One of the
doctor's pupils, in the course of an investigation, placed the above-mentioned
quantity (!) of the substance in question in a small cast-iron dish heater over a
small Bunsen gas burner in common use in laboratories. While so engaged the
nitro-glycerine exploded with great violence, breaking 46 panes of glass in the
windows of the laboratory, hurled the iron dish against the brick wall, the iron
stand upon which it was supported partly split and partly twisted out of shape,
and the tube of the Bunsen burner split and flattened. Those in the laboratory
fortunately escaped without injury

----
Cause? Most explosives have a Cook off temperature
the collective readers will no doubt be astonished and
amazed too know there is a standard test to determine
the temperature. Time permitting I'll see if I have details at hand.

----
Revenge of the molecules perhaps?!?

Within hours of each other on the same winter afternoon in 1941-42, three
hot sulphuric acid melting point baths blew up at U of T[oronto], McGill and
a university in the United States, all of them working on the RDX [explosive]
program. The Toronto event only left a surprised graduate student with his
glasses cracked and minor burn spots, but one of the others put a student
temporally in the hospital. The very next day newspapers reported explosion
of a milk test device using sulphuric acid. A science buff in the labs
announced that what was taking place was The First Revolt of the Molecules,
with sulphuric acid leading the way. Would chlorine, or maybe caustic soda
be next? Fortunately the molecules clamed down and the revolt did not spread.

Donald H Avery
The Science of War : Canadian Scientists and Allied Military Technology
During the Second World War
U of Toronto Press. 1998.


djh
----
It is essential that persons having explosive
substances under their charge should never
lose sight of the conviction that, preventive
measures should always be prescribed
on the hypothesis of an explosion.

Marcellin Berthelot - 1892
Explosives and their power - Page 47



[Edited on 6-6-2011 by The WiZard is In]
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[*] posted on 6-6-2011 at 07:05


Thank you aquaregia, for being brave enough to post pics... It is a real eye opener for sure. Many of us as quicksilver said, can underestimate the reaction of a energetic material, more so if we arn't 100% in our thinking or a bit off in our full focus.

COUNT YOUR BLESSING"S friend.... This are lessons learned the hard way, but learned non-the-less.. I think many, if not all of us who dabble with energetics will have a accident sooner or later that will shape our view of how we respect this field of interest .....

Once again thank you for sharing ...I hope it detours unexperienced amateurs from making mistakes as such.
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[*] posted on 6-6-2011 at 07:36


I'm not sure on France's laws, but in the U.S. one could be in some serious shit along with the pain and grief you are already are feeling. Do you think you may face legal ramifications? What did you inform the hospital staff as to what happened. I'm just curious.

Again, I'm really sorry this happened to you.:(
I wish you the best of luck in all your future endeavors.




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quicksilver
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[*] posted on 6-6-2011 at 07:43


NG can also be called a "boarder-line" material in this context discussion. Further, when realized just the sensitivity level NG displayed the 1st thing utilized was a buffer state. This is old news to some.
What some folks don't know is that many of the (nitrated) polyols display this high sensitivity in one stimulus & not another. Industrial-Melts are generally mfg w/ a buffer of some sort: water (heated, steam, plastics, lower melting materials & physical shielding). The "buffer" can be a mfg mechanism or part of the material. The reality is the higher a sensitivity level exists the closer to melting temp to initiation temp we find it. Thus we move that temp away from initiation level. Obviously in our example case there existed no buffer and a temperature spread existed with thin walled glass.

In order to understand the inherent dangers in the mfg process we are generally routed to MHN as ETN was not subjected to the same scrutiny due to it's expense (at the time) of the major precursor. MHN DID find a place in this unique line between primary & secondary.
{See the works of Clarence Hall & Spencer Howell} "Initial Priming Substances for High Explosives" `1917 (Dept of the Interior USBoM Technical Paper 162) had some very interesting things to say about materials such as MHN. And it might be the clearest form of information regarding it's sister, ETN.
However for all intents and purposes ETN IS truly experimental. We should NEVER forget that. There is little track record of it's performance, in and of itself.

"Hot-Wire" detonation of MHN was often attempted and it's use in initiation mechanism (detonators) had been proposed quite often due to it's obvious appropriate VoD, wave-front, etc. However it was not widely commercialize due to it's qualities (similar to NG) of [not] maintaining both stability, shelf life, & predictability in an enclosed capsule under a variety of conditions. It showed promise in sand test performance but less stability than mercury fulminate in shelf life & exposure testing. I am generalizing here (in a broader agenda) but in making such a comparison for an understanding of the appropriate "cut-off" point of products subject to heat, impact, and other forms of initiation & their application in cast or solid usage.

Casts and melts demand certain mfg efforts. The elimination of bubbles has long been a problem area for a variety of reasons. The utilization of trinitrated toluene has been often used to lower the melting temp of RDX-mixed compounds in such casts for the reasons above. Interestingly PETN has often been utilized as a crystalline state. Both RDX & PETN have performance similarities however it's the nitrated amine that is chosen for a cast.
RDX will react to impact testing & the "buffer" of the TNT has lowered it's sensitivity to both shock & temp. This has not been the case with PETN.* Contrasts demonstrate that in a mfg effort, the PETN had been subject to a "plastic"-buffer design for commercial use. MHN on the other hand was not chosen for melt casting to any great extent: it's sensitivity was observed to be too high to make such an industrial effort. ETN obviously is a real unknown. To attempt a cast with ETN is a serious risk and should be realized from the outset.

IF such an experiment were ever attempted on a professional basis, every effort should be brought into play to minimize the possibility of unintended detonation. Direct application of heat should not even be considered unless it is via a water bath or other mitigating mechanism. Further research should be applied toward the cast-melt dynamics in lab and plant-level operations.


* see: Choices in Industrial Explosive Manufacturing (ISEE March 1992)








[Edited on 6-6-2011 by quicksilver]




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aquaregia
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[*] posted on 6-6-2011 at 08:43


Bot0nist.
you are right. Here, as anywhere else, ETN manufacture or possesion is illegal. However, for all intend and purposes, what ETN I had has been melted in acetone and burnt. I'll tell you what, seing what a drop can do, I was scared shitless of those cast I made. Now, to any law enforcement person, who might come across this post I'll say this:
I have been well punished allready and I have learned my lesson the hard way. I do not see any need to take this matter any further. Also, I posted these pictures in order to, maybe, (I hope) dissuade others from making high explosives. This is my punishment. As I said, and I mean it, chemistry for me is now over. I have a wife and kid which I love so fuck chemistry. I told the hospital that I got injured when the glass I was using reacting HCL and Zn to inflate a balloon for my kid with H2 to make it fly blew up. I do not think they believed me, but they know I am/was only a danger to myself and left it at that.
I do not believe in the divine and am a comfirmed atheist. But, when you consider that the glass only hit my torso and harms instead of my eyes (I was not wearing goggles even though I normally do), it is a miracle. As I said, if people reading this think that this is never going to happen to them, let me tell you: you are SO wrong. People who have lost their eyes to "energetic materials" aren't on this forum to tell you about it are they? I'll repeat my message: DO NOT MAKE THAT STUFF. Life is very beautiful for me right now, and I never appreciated life as much as I do now. Can I be any clearer?
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[*] posted on 6-6-2011 at 12:25


Aquareagia, I wish you the best. You are not alone. Years ago I made silver fulminate and was cut by flying glass when a small amount in a glass vial went off. It was under water so we thought it was safe... I was very lucky that none of the pieces hit my eyes. It was enough for me. I left the hobby alone for about 30 years. After finding this forum, I came back to it just long enough to do a couple small experiments but have now moved to something safer.

If you could do a survey I'll bet you would find that more 80% of people that experiment with energetics for more than a year have some form of accident or "unintentional initiation". Of those maybe one in 5 is serious enough to require a trip to the ER (or worse).
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[*] posted on 6-6-2011 at 13:22


I haven't read all of the posts, but what can one say?
Accidents sometimes happen for no apparent reason.
Though very painful, your wounds will heal, and then you should try to pinpoint why what went wrong, went wrong.
Thanks for letting us know about it, as these things are important.
It might be advisable to take a more passive role for a while . . .

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[*] posted on 6-6-2011 at 14:04


Quote: Originally posted by The WiZard is In  
----
Cause? Most explosives have a Cook off temperature
the collective readers will no doubt be astonished and
amazed too know there is a standard test to determine
the temperature. Time permitting I'll see if I have details at hand.



Found it, but first, Aquaregia is to be praised for posting a
classic "a picture is worth a thousand words snap.
When I mention safety here the wind blows up - shakes the
trees and all the nuts fallout. You know - the ones who
despite having no life experience or training on explosives, but who
because they own a computer and are able to access
la Net proclaim think/proclaim themselves experts [in their own minds] on safety.

---
AR - NG can also be called a "boarder-line" material in this
context discussion.


Sobero was the discovery of nitroglycerin,
in his hands it was a brand new chemical with unknown properties.

---
It is hard to separate quantity vs. brisance (wow finally
someone {AR} [French] who know how to pronounce the word!).
Presumable NG would have resulted in finer particles of glass.

---
I had my tests mixed up. I was thinking of the —

[Cribbed from R. Meyer, J. Köhler, A. Homburg
Explosives]

Deflagration Point
Verpuffungspunkt; température de d´ecomposition

The deflagration point is defined as the temperature at which a small
sample of the explosive, placed in a test tube and externally heated,
bursts into flame, decomposes rapidly or detonates violently.
A 0.5-g sample (a 0.01-g sample in the case of W Initiating Explosives)
is placed in a test tube and immersed in a liquid metal (preferably
Wood’s metal) bath at 100 °C (212°F), and the temperature is raised
at the rate of 20 °C per minute until deflagration or decomposition
takes place.

This method is identical with the official method laid down in RID.
Nitrocellulose and nitrocellulose powder are tested in a stirred paraffin
bath, heated at the rate of 5 °C per minute.

The EIDS Slow Cookoff Test (UN Test 7(f) is a 'hole
nother animal. See TB 700-2 for details.

There also dobe a Thermal Stability (Tube Method) used
for pyrotechnics. A SS tube is heated with a nichrome wire.

Evaluation of Test Methods for Pyrotechnic Hazard Classification.
Personal Author: Wilcox, Wayne R
Corporate Author: GENERAL ELECTRIC CO BAY SAINT LOUIS MS ENGINEERING AND SCIEN...
Source Code: 409145
Page Count: 160 page(s)
AD Number: ADB004208


[Edited on 6-6-2011 by The WiZard is In]

[Edited on 6-6-2011 by The WiZard is In]
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[*] posted on 6-6-2011 at 14:36


This is intriguing. To explain this incident:


*** Molten ETN has sensitivity of NG- being very sensitive.
*** ETN may decompose when brought over the 60C mark- when casting-acids may be trapped within


So, what I think happened was the partial decomposition during casting of ETN, creating a trapped acid, and when it was heated with a torch really fast through a glass tube, it underwent DDT.


Another IMPORTANT issue we don't know about is how you recrystallized your ETN- did you heat up your alcohol to help dissolve the ETN? What was the eventual appearance of ETN? That could also affect the sensitivity of ETN as it has been rumored that through hot methanol recrystallization you can make "primary-type ETN". That....coupled with some 60C+++ casting could be the cause of this accident.

Mystery not solved, but we're getting close.
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[*] posted on 6-6-2011 at 15:42


I don't mean to sound callous, but what's the mystery? The man heated a small quantity of the sensitive HE ETN over an open flame. It has been known to readily detonate when heated strongly in foil and even proposed as a replacement for primaries in that aspect. While I can't speak for aqua, I bet he knows where he went wrong. I believe he even said 'I knew I was fucking up."

The main issue seems an underestimation of the power of this material in a mg scale when confined. I know from experience with my M.E.K.P. experiments that big bangs can come in small packages.




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[*] posted on 6-6-2011 at 16:07


@Bot0nist

Yes, ETN will detonate CONFINED if STRONGLY heated, but I've not seen it DDT just from flame. I saw a video of pyro who cast ETN in spoon over a candle flame- he's done that probably over 2 dozen times for his detonators and he didn't have detonation.

This was was a bit out of the ordinary and I think the problem was the casting/rapid heating combination with a trapped acid inside.
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[*] posted on 6-6-2011 at 17:00


Sorry about your accident, but it is never wise to give explosive materials a sudden thermal shock, no matter how "safe" they are reputed to be.
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Polverone
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[*] posted on 6-6-2011 at 17:07


Quote: Originally posted by holmes1880  
@Bot0nist

Yes, ETN will detonate CONFINED if STRONGLY heated, but I've not seen it DDT just from flame. I saw a video of pyro who cast ETN in spoon over a candle flame- he's done that probably over 2 dozen times for his detonators and he didn't have detonation.


I am sure the DDT conditions could be rigorously tested by someone with appropriate materials and patience, but in this context speculating about whether you're going to experience a low-order accident or high-order accident indicates inattention to safety. Spoon-over-flame casting of ETN seems needlessly hazardous even if its practitioner has so far retained all appendages. You only get the one body, and if you void its warranty you will have a lifetime to regret it.

I know that I have scolded people about safety here before and I surely will again. I am glad that aquaregia escaped without serious injury and has learned from his accident. I have known one friend who has to live his whole life with only one hand because of carelessness when he was 16. I have seen members here and at other forums report serious accidents, sometimes ones that could have ended in fatalities. The ones who actually die we know sometimes from news reports or word of mouth.

This is not a new problem. Archives of the Journal of Chemical Education, old amateur rocketry manuals, and newspaper back files attest to many injuries and deaths inflicted by careless chemists on themselves. Most casualties are unsurprisingly male, young, and interested in fireworks, rockets, and/or explosives. This is not to say that I am categorically against experimentation in these more dangerous areas. We have the Energetic Materials forum for a reason. But it is inherently a hazardous subject, and avoiding injury requires planning, discipline, and attention to detail.




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