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Author: Subject: ETN: almost killed myself... READ!
The WiZard is In
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[*] posted on 7-6-2011 at 15:51


Quote: Originally posted by holmes1880  

I've made over 50 ETN nitrations and tested their properties through all kinds of contraptions known to man kind. And yet, I've never cast it- because I knew that is asking for trouble. It's pretty damn obvious that when substance has a melting point of 60C it is damn susceptible to undergoing DDT quicker than other secondaries.


Got to admit math's are not my strong point, however, I suffer
from the belief that there is no statistical test called luck.

The most common cause of auto accidents is - following to closely.
Reason being .... tens of thousands tell themselves ... I have
always done it and have never had an accident.


Experience alone is not always a safe index to sound practice. In on accident
investigated by this Bureau, one man was killed and two women in an adjacent
building were injured by the detonation of a sulfur-potassium chlorate
composition in the process of being mixed, although it was stated that the mixing
operation involved had been in use in that plant for 20 years without mishap.
There is, of course, the possibility that the raw material used at the time of the
accident may have been different from that upon which past experience was
based. Thus, if the particular lot of sulfur employed were acid, abnormal
sensitivity of the chlorate-containing mixture might result. In any event, safe
experience, even for 20 years, would not justify a practice that exposed the mix
operator and others. Instead, the hazards should be recognized and isolation and
remote control provided.

Irving Kabik
Hazards from Chlorates and Perchlorates in Mixtures with Reducing Agents
U.S. Bureau of Mines
Information Circular 7340
December 1945.


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[*] posted on 7-6-2011 at 16:02


The reason that it does not explode in a spoon is that the thermal mass and conductivity of the spoon are much greater than that of a test tube. In the spoon the ETN is heated slowly. You see it melt and then remove it from the flame, it probably just gets a few C above its melting point.

Aquaregia used a test tube and bunsen burner. The bunsen is hotter than a candle and the thin glass walls have little thermal mass. The ETN probably went from melting to 200C and on to detonation in seconds.

Explosives that melt before decomposing are safer since the heat of melting absorbs considerable thermal energy.

I don't think containment is an issue. How does a test tube provide more containment than the spoon?
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[*] posted on 7-6-2011 at 16:51


Quote: Originally posted by gregxy  

I don't think containment is an issue. How does a test tube provide more containment than the spoon?


It wasn't a test tube. It was the ETN itself being solidified to the surface- so hard that he couldn't scrape it off. When he started heating it rapidly the part that was adjacent to the glass wall- and thus trapped from air, melted rapidly and then DDT'd settiing of the rest of the whatever cast ETN there was.

It's that simple. I actually think you can get this to happen in a tea spoon if you melt it and let it solidify. Than rapidly heat it up in a fire. Although, glass is much better because it doesn't conduct heat as well, so the heating will be far more rapid.

[Edited on 8-6-2011 by holmes1880]
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[*] posted on 7-6-2011 at 16:56


Quote: Originally posted by The WiZard is In  



What is it that you want everyone to extract from the standard PETN description? You have no point, sir. Keep it together, please.


HMX has a melting point of 276C. See, I can troll too. :P

[Edited on 8-6-2011 by holmes1880]
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[*] posted on 7-6-2011 at 22:50
to sherlock holmes


I am sorry sherlock, but your posts are starting to ennoy me a bit:P. here is why. before the test tube blew up in my face, I can guarantee that the ETN on the wall I was heating was MELTED, so much for your confinement theory... also, keep in mind that the tube was a large one, the more so compared to the quantity of ETN in it. reading through all the very valuable information provided above, I think I can safely say that I did heat up the ETN to the point that it detonated, full stop. Now, people who still carry on heating ETN in spoons or whatever after seeing that there is a risk that it will detonate, are in my mind, extremely careless and will, at some point or another, have an accident. I can't remember who said that if the ETN in the proverbial spoon detonated, then the guy would have been quite safe... from my experience, this is downright CRIMINAL to post this. You have NO IDEA how powerfull ETN is! I really wonder what is required for people to understand THAT YOU JUST SHOULD NOT TAKE A FLAME TO ETN, candle flame or whatever... And please do not start babbling about candle flame temp:mad:! Jesus guys (some of you anyway) GET REAL!
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[*] posted on 7-6-2011 at 22:57
This is a question for the experts


This is aimed at the more knowledgeable people here:
What Philou wrote really caught my eye, and I am wondering. Depending how you recrystallize ETN, you'll get needle like cristals or plate like cristals. as far as I know, cristal type you get depends on Etoh Temp used for desolving ETN strangely enough... Are we sure the the 2 cristal types actually are the same compound? what if, using hot EToh, did indeed cause the EToh to react with ETN, and produce something else? It'd be great to find out.
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[*] posted on 8-6-2011 at 02:16


An infamous experiment with NG was to drip it onto a hot plate (200 degrees C IIRC); this will result in very loud booms. If the plate was hotter, only deflagration was observed. Smaller temp just evaporated the NG.


One thing is for sure: some of these esters are prone to detnation on heating. Don't forget MHN, which almost behaves like a primary. Even with the tame TNT it was a known fact that in melted state the risk of ddn was a considerable one should a shock occur.


As for holmes1880: you know you are an "expert" till it happens. I hope for your own sake you will always stay in your own eyes an "expert". The rest is just useless speech, confinements, spoons etc.
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[*] posted on 8-6-2011 at 07:42


When I recrystalized mine I used hot ethanol, about 58°, as hot as possible, as it is quite expensive here.

Funny thing is, I had little blobs in that solution that did not dissolve... -> Ethyl nitrate?
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[*] posted on 8-6-2011 at 08:12


Quote: Originally posted by aquaregia  

You're "pretty sure ETN melted. :) Ok, then why did you continue heating it up? Wouldn't it pour out if it melted? My "confinement theory" holds water even with molten ETN- the bottom layer that is next to the glass gets hotter than the upper surrounding layer, and if heated really rapidly, it may just detonate. Which also leads me to believe you may have had close to 200-300mg ETN in that tube- it won't look much being molten- as its volume shrinks down to 25% the original volume, but it's got wicked power.

I have perfectly good idea how powerful ETN is- 100mg quantities are very loud and have some good shredding power. I've tested from minute ETN quantities to 1g quantities- they are all very sharp and scary.

I never commended the guy for heating ETN with spoon- I told him it's a bad idea and he should abandon it altogether. In fact, I never encourage ETN casting and never did it myself- it has no real benefit over pressing and is far more dangerous. I also never recrystallize with warm alcohol for that exact matter- warm recrystallization of any energetic via alcohol produces long crystals- that's a known rule. That in turn, leads to increased impact sensitivity, though I'm not sure about sensitivity to flame.

While I appreciate people sharing details about accidents, it really irks me when the preaching begins about how dangerous the material is, even though they've handled it as poorly as it can be handled. You basically develop a phobia of everything that pertains to the incident-which may be a good thing, perhaps. Now, I am not aiming it anyone in here, only to emphasize the overall concept of the accidents in scientific and amateur field, my good pyro buddy a while back said: "Everything becomes dangerous when you throw a retard into the mix". Still get a chuckle out of it....:)



[Edited on 8-6-2011 by holmes1880]
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[*] posted on 8-6-2011 at 08:39


Quote: Originally posted by a_bab  
As for holmes1880: you know you are an "expert" till it happens. I hope for your own sake you will always stay in your own eyes an "expert". The rest is just useless speech, confinements, spoons etc.


What is this condescending nonsense? Treat secondaries like a primaries- rule 101 of working with HE. Especially when it comes to ETN.
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[*] posted on 8-6-2011 at 09:16


You know very well what I mean. You are babling here about confinements and such. If you look well enough, your discussion is more like trolling with the initiator of the thread.

OK, he did something stupid, and he *knew* it was plain wrong, moreover he admited it openly.
You are showing off and dork around. Yes, we all know how good you are; just go and bark some other tree. Your interventions here are tiring to say the least. You've made your point, now go away.
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[*] posted on 8-6-2011 at 11:00


If you're going to accuse me of trolling you need to at least give an honorable mention to Wizard. I am just weighing in on what actually happened. I don't like to give extended theoretical explanation to a problem that is pretty straight forward, albeit some details aren't perfectly clear. And what have you responded to the question TS asked? TS asked why did it happen and I gave him a clear-cut answer. If you want answers, I'll give you answers. If you want the truth, you can't handle the truth! See, now I am a little guilty of trolling.

/thread.
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[*] posted on 8-6-2011 at 12:13


Quote: Originally posted by aquaregia  
I am sorry sherlock, but your posts are starting to ennoy me a bit:P. here is why. before the test tube blew up in my face, I can guarantee that the ETN on the wall I was heating was MELTED, so much for your confinement theory... also, keep in mind that the tube was a large one, the more so compared to the quantity of ETN in it.


Perhaps I am misunderstanding you, but this seems to contradict what you said earlier:

Quote:
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:


In any event, as you yourself acknowledge, you "fucked up" doing that. You were too impatient and submitted an explosive material to a very sudden thermal shock and/or overheating. NEVER do that, no matter how "safe" any given explosive material is reputed to be.
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[*] posted on 8-6-2011 at 13:01


Quote: Originally posted by Blasty  

In any event, as you yourself acknowledge, you "fucked up" doing that. You were too impatient and submitted an explosive material to a very sudden thermal shock and/or overheating. NEVER do that, no matter how "safe" any given explosive material is reputed to be.



Have you and "Sherlock" ever considered changing your stage
names to Dr. Pangloss?! You both seem to live in a world separate
from the real one.
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[*] posted on 8-6-2011 at 13:04


I think you misread it, Blasty. I think he's saying that it was solid before he applied heat, then after he applied heat the ETN was melted before it went off.
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[*] posted on 8-6-2011 at 13:39


Please keep discussion in this thread civil.



PGP Key and corresponding e-mail address
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[*] posted on 8-6-2011 at 15:18


Quote: Originally posted by Polverone  
Please keep discussion in this thread civil.


Amen.

Aquaregia who I would nominate for the
ScienceMadness Medal of Honor for his uncommon courage
for bring to our attention the details of his accident is greeted here
by the Panglossian Front rising up in their arrogant-ignorance
to excoriate him. Rather than thanking him for his candor and
uncommon warning - he is accused of being everything but a
Christian starting with them claiming his mothers diet was low in
iodine.

The basis of safety is not -

It is safe because -

I think it is -
I wish it was -
I believe it is -
I say it is -

Like the kid in a NYC Housing project who stuck his
head though the opening in the elevator door (the
glass was missing) you have to know where Courage
ends and stupidity starts.


A lack of knowledge is not equivalent to stupidity. Many
are the scientist who were bit in the ass by their
discoveries, e.g,. Bunsen, DuLong, Davis &c., &c.

For your edification I present Howard 1880.

With this view he mixed such substances with alcohol and nitric acid, as he thought
might, by predisposing affinity, favour, as well as attract an acid combination of the
hydrogen of the one to the oxygen of the other. ..............
The precipitate was separated by filtration aid consisted
of small acicular crystals having a saline taste. ...... He, therefore,
for obvious reasons, poured sulphuric acid upon the dry crystalline mass. A violent
effervescence ensued, and, to his great astonishment, an explosion took place. The
singularity of this explosion induced him to repeat the process several times, and,
finding that he always obtained the same kind of powder, he prepared a considerable
quantity of it. He gives the following method as the most satisfactory for the preparation
of fulminate of mercury:— [The usually method of preperation].
.......... He once poured six drams of concentrated sulphuric acid on fifty grains of
fulminate. An explosion took place, almost at the instant of contact. He states that he
was wounded severely and most of his apparatus was destroyed, and then adds, "I
must confess I feel more disposed to prosecute other chemical subjects."


djh
----
It is not the critic who counts: not the
man who points out how the strong man
stumbles or where the doer of deeds
could have done better. The credit
belongs to the man who is actually in
the arena, whose face is marred by
dust and sweat and blood, who strives
valiantly, who errs and comes up short
again and again, because there is no
effort without error or shortcoming,
but who knows the great enthusiasms,
the great devotions, who spends himself
for a worthy cause; who, at the best,
knows, in the end, the triumph of high
achievement, and who, at the worst,
if he fails, at least he fails while daring
greatly, so that his place shall never
be with those cold and timid souls who
knew neither victory nor defeat."

"Citizenship in a Republic,"
Speech at the Sorbonne, Paris, April 23, 1910




[Edited on 8-6-2011 by The WiZard is In]

[Edited on 8-6-2011 by The WiZard is In]
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[*] posted on 8-6-2011 at 15:20


Quote: Originally posted by The WiZard is In  
Have you and "Sherlock" ever considered changing your stage
names to Dr. Pangloss?! You both seem to live in a world separate
from the real one.


If you think that submitting explosive materials to the sudden and direct action of a gas flame is "just fine and dandy" instead of a prescription for an accident, the one living in a parallel universe is apparently none other than you.



[Edited on 8-6-2011 by Blasty]
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[*] posted on 8-6-2011 at 15:30


Quote: Originally posted by The WiZard is In  

Have you and "Sherlock" ever considered changing your stage
names to Dr. Pangloss?! You both seem to live in a world separate
from the real one.


Oh, the irony.... God bless you Wizard, but you may have been lost within the 100 year old publications yourself. I read the essential literature on "ErTeN" and I also went out many-many times to test out its properties. Reality require to actually test things out, you know....

And besides, who is claiming that ETN is safe to heat up after being cast? It's inadvisable to cast it at all, frankly. However, you keep saying that ETN will detonate basically beacause its deflegration point is 160 and it says "violent explosion" next to it. That is not true unless certain conditions are met.

An anecdote, last summer I was getting rid of 10g batch of 5month-old ETN and thought of burning it up at once or in 1g amounts. But after thinking about it, I just drained it down the toilet. Moral of the story- treat secondary like you treat primaries.

That's all.

[Edited on 8-6-2011 by holmes1880]
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[*] posted on 8-6-2011 at 16:03


Quote: Originally posted by The WiZard is In  


djh
----
It is not the critic who counts: not the
man who points out how the strong man
stumbles or where the doer of deeds
could have done better. The credit
belongs to the man who is actually in
the arena, whose face is marred by
dust and sweat and blood, who strives
valiantly, who errs and comes up short
again and again, because there is no
effort without error or shortcoming,
but who knows the great enthusiasms,
the great devotions, who spends himself
for a worthy cause; who, at the best,
knows, in the end, the triumph of high
achievement, and who, at the worst,
if he fails, at least he fails while daring
greatly, so that his place shall never
be with those cold and timid souls who
knew neither victory nor defeat."

"Citizenship in a Republic,"
Speech at the Sorbonne, Paris, April 23, 1910


What's "djh"....... "Degrassi Junior High"?

Nice of you to include the passage for those of us who are actually testing energetics despite the time, money, legal constraints and potential risks.

[Edited on 9-6-2011 by holmes1880]
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[*] posted on 8-6-2011 at 17:59


There is a huge difference between conjecture and knowledge.
In many of life's pursuits, experience can be a teacher of hard lessons
about the difference. I am continually astonished by how little distinction
is generally made between the two things by people who have little experience
or have no real aptitude for science, or both, while thinking they know a lot more than they do, never mindful of the old wisdom that a little knowledge is a dangerous thing. Anyone can make a stupid mistake, electricians get electrocuted, pilots fly airplanes into the ground, ect. When such things happen it isn't because the electricity or the airplane behaved in some anomalous way,
but because the operator was distracted and/or made an error. But usually when such a thing occurs there is a mindset of complacency which facilitated that error and
led to a faulty decision. Just like a food diet can cause flatulence, so can an undisciplined mental diet lead to a brain fart. Not discerning the difference between conjecture and knowledge provides exactly that deficient mental diet that will lead to a brain fart and an action derived from it which may be consequential. Experimenting with an energetic material is dealing with a weighty matter.
Such a pursuit which courts danger should be regarded seriously, and people should be sure of the difference between what they know and what they only think they know and then act accordingly. Otherwise it becomes a testing of fate where it is only a matter of time before somebody recklessly playing with fire gets burned.
Experimenters should try to be mindful of what they don't know for certain, and not be overconfident about what they do know, and then use common sense.

Anyway there is not some big mystery to solve here that manually holding an NG class energetic material in a fire is not at any stretch a safe or recommended manipulation.
What occurred as a consequence is logical and predictable even though unfortunate. If someone douses themselves with gasoline and then strikes a match, an energetic chemical reaction will also soon follow very predictably,
and if someone opens a gas tap in a room with a lighted candle there will be an explosion also. These events are not the fault of chemistry, but are more like simple arithmetic.

conjecture:
1. Inference or judgment based on inconclusive or incomplete evidence; guesswork.
2. A statement, opinion, or conclusion based on guesswork

knowledge:
1. The state or fact of knowing.
2. Familiarity, awareness, or understanding gained through experience or study.
3. The sum or range of what has been perceived, discovered, or learned.
4. Learning; erudition: teachers of great knowledge.
5. Specific information about something.
6. Carnal knowledge.
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[*] posted on 8-6-2011 at 19:32


Rosco, have you done any controlled testing with ErTeN or NG to see how it responds to heating? It sounds like you've tested it out already.



[Edited on 9-6-2011 by holmes1880]
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[*] posted on 8-6-2011 at 20:24


No I have not tested the materials for the reliability of their response to initiation by thermal shock. However I do have confidence in the many reports in the literature including patents that NG, ETN, MHN, and hexanitroinositol are 4 materials in particular that are similar in their propensity for detonation from thermal shock as well as from more gradual overheating. I would expect that with the slower rate of heating it may be a coin toss whether there is a deflagration or detonation for a very small sample. For larger samples it becomes a moot point because the deflagration generates thermal shock for the remaining material. With a flame heated surface like a test tube there is an uneven heating and it would seem likely that a small droplet of molten material dripped or flowed rapidly onto a portion of the surface which was superheated to the contact detonation temperature where thermal shock then provided the initiation which communicated detonation to the remaining material. Tens of milligrams would be my estimation of the quantity more likely involved.

Axt reported a heat gradient testing for contact of sprinkled crystals of ETN and said that at lower temperatures there was deflagration, and then at higher temperatures there was contact detonation.

[Edited on 9-6-2011 by Rosco Bodine]
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[*] posted on 8-6-2011 at 21:59


I will confirm that. I heated up a stove plate to light red- not glowing red, and placed tiny 1mg pieces of ETN on it- one at a time. 3 deflegrated and the last 4th piece gave a loud and unpleasant to the ear snap. That 4th piece was placed about 1 minute after the 3rd one, when the hot plate warmed up significantly more. I did not proceed further for hearing's sake.

In that case, the heating with Bunsen burner could have created a very hot spot on the glass, where already molten piece came in contact with, setting off the other remaining residue. There is certainly a high critical temperature where ETN cannot gradually evaporate and ignite, but instead just detonates. That's how thermite/PETN detonators work, actually.
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[*] posted on 8-6-2011 at 22:27
melted ETN or not.


to answer queries above, the ETN was solidified as a very thin sliver to one side of a large test tube. I kept the tube fairly far away from the flame for the purpose of heating it just enough to melt it. just before it detonated, the entire bottom half of the sliver had melted. The flame from the bunsen was around the bottom of the tube and the ETN started bubbling/boiling. then it detonated with a bright yellow flash mixed with black soot (this is what my eyes registered... I think). To be noted, I was holding the test tube in my right hand by pinching the very top. The top of the sliver did not detonate as I found some glass fragments with ETM still stuck to it on site and I sill possess all digits;).
The timescale of the above is about one second.
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