Sciencemadness Discussion Board

ETN: almost killed myself... READ!

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aquaregia - 6-6-2011 at 03:00

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]

azo - 6-6-2011 at 03:39

i hope this is a warning to others , not to be as stupid as you

gnitseretni - 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:

azo - 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

Bot0nist - 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]

bbartlog - 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).

I had to post

aquaregia - 6-6-2011 at 05:21

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.

Jor - 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.

quicksilver - 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]

now to the core of the subject

aquaregia - 6-6-2011 at 06:06

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?

quicksilver - 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.

condennnsa - 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]

Welcome to La Club

The WiZard is In - 6-6-2011 at 06:49

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]

pjig - 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.

Bot0nist - 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.

quicksilver - 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]

aquaregia - 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?

gregxy - 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).

hissingnoise - 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 . . .

The WiZard is In - 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]

holmes1880 - 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.

Bot0nist - 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.

holmes1880 - 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.

Blasty - 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.

Polverone - 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.

holmes1880 - 6-6-2011 at 17:39

Ok, so here's what happened to him. The ETN was STUCK to the glass container-that's why he couldn't get it out. Well, being stuck to the glass creates what? Yes, Dear Watson, it created that small amount of self confinement ETN usually doesn't get when in a powdery form. Fast heating and that confinement led to KABOOM.


The end.



[Edited on 7-6-2011 by holmes1880]

ETN was recrystallized in Etoh

aquaregia - 6-6-2011 at 22:01

the ETN had been recrystallized in non technical grade of the shelf 95% Etoh twice. at first, the Etoh was gently heated to 40 degC, but the amount was not sufficient to disolve the entire ETN batch (which was neutral). This Etoh was set to cool off slowly and neddle like cristal formed. The rest of the ETN was disolved in room temp Etoh set in the fridge, then some water was added to it. platelike cristals formed. The PH was about 6 so I recrystalised the entire bunch the same way as the second part above, but, adding sodium bicarb solution to correct PH this time. the cristals were then left to dry on newspaper, before being introduced in a large test tube and melted in a hot water bath. IMOH the ETN was made sticking to the rulebook as far as ETN being experimental is concerned...
Now, Bot0nist, that guy with the spoon heating ETN over a candle flame, will have problems, guaranted! a spoon holds quite a bit, and seing what a few drops do, there is enough there for the spoon to chop his head off, and I am not even speaking of blast effect... You should send him a link to this post...

Microtek - 6-6-2011 at 22:42

A few years ago, I was doing a series of (very successful) experiments on small rockets with composite double base fuel (comprising AN, Al, nitroglycerine and microcrystalline nitrocellulose along with various modifiers).
Considering my great results, I felt it would expedite things if I synthesized a slightly larger amount of NG than usual instead of doing microbatches all the time. The synthesis went without a hitch, and so I found myself with about 20 ml of neutral, colourless NG in a beaker.
When I assembled one of the rockets, I dropped an end-plug (compact, made of steel and about the size of a 9 mm pistol bullet) from a height of about 50-60 cm into the beaker with NG.
The impact emitted an impressive DZINGGG, but fortunately nothing else happened.
I stood there for perhaps five minutes, contemplating how easily that could have maimed or killed me, then stopped experimenting for a while.

Since that day I have considered my luck spent, and have relied on sound work practices and rigid safety precautions instead. But I haven't stopped experimenting.

mabuse_ - 7-6-2011 at 00:28

Aquaregia, thank you for sharing your experience!
Fortunately it seems like you did not suffer any permanent damage.



I think that this here can not lead to any conclusion about the dangers in melting ETN.
By heating with a flame the glass and the etn layer directly in contact with it might easily got well beyond 200°, while the rest is not even molten.

It was clearly inconsidered handling that caused disaster. Just a little dropout most of us suffer from sometimes.


I got my slowly ethanol recrystalised, needle style (like Aquaregia described)ETN to 1,4g/cm³ by hand pressing, what I consider pretty good.
No need to melt.

aquaregia - 7-6-2011 at 01:24

hey? I was thinking. I do not know how that works, but the guys at science madness could at least change my status to "hazard to self" don't you think?:D

holmes1880 - 7-6-2011 at 01:59

A guy heating it with a TEA spoon has been warned few times by me and another few people, but he still did it. He actually showed what happens when ETN gets overheated over a candle flame in a spoon- it starts pumping out NO2 brown smoke until igniting. If it detonated in a spoon he'd have no shrapnel, but would probably be deaf for a few minutes.


Your incident was caused by CONTAINMENT that was created by the cast leftover ETN. It would most likely not have detonated had it not been stuck to the wall. Containment+ rapid heat. But most important-containment since it's a secondary.

You can't blame ETN stability for not being able to withstand those types of conditions.

Bowdlerize - 7-6-2011 at 02:23

Thank you Aquaregia,
Your brave post has made me stand back and re-access my situation. I have been moving quickly through new syntheses since I first distilled HNO3 a few months ago. Now I know I must stop until I have better safety equipment and a better understanding of chemistry in general.

I have deflagrated ETN on several occasions and once burn 1 gram at once. I shudder to think what would have happened had DDT occurred.

Your conviction to posting this hasn't gone un-heeded, you have changed the way I look at HE. No amount is "safe".

aquaregia - 7-6-2011 at 03:04

well bowdlerize,
that single post from you makes mine worth it. be safe

PHILOU Zrealone - 7-6-2011 at 03:38

I'm glad you survived and had not your big batch exploding.

Not everybody knows that explosives are tested many times in a way to asses properties...and that behind properties there are some statistics...
-Heat sensitivity by "slowly" increasing T° over time
-critical diameter of steel sleve test (direct flame heat)
-impact sensitivity
-friction sensitivity
-differential heat analysis

Usually a statistical method is used and thus the values are average values... this means something can happen before that value...but there is little less chance...this doesn't mean you are on the safe side! Thus it can be that the average is based on the 50% set off the explosive stuff (on 30-50 trials)...

But only 1% (or less) is sufficient to be dramatic.You may have experienced without troubles 100 trials, and the last one is fatal. So no YOU ARE NOT SMARTER THAN EXPLOSIVES, YOU ARE NOT ITS MASTER...always keep this in mind

Rules:
-treat it with due respect as if it was the first time
-always think before acting what would be the consequences of an unsuited explosion
-avoid glass and metals and favourize soft plastics
-keep quantities low

I would personnaly never cast/heat a nitric ester, nor recristallize it from ethanol...maybe the word transesterification is unknown to you but:
O2NO-CH2-R-ONO2 + CH3-CH2-OH <==> HO-CH2-R-ONO2 + CH3-CH2-ONO2
So from polynitrate esters you end up with hydroxypolynitricesters and volatile ethyl nitrate...


[Edited on 7-6-2011 by PHILOU Zrealone]

quicksilver - 7-6-2011 at 05:57

I'm not a stranger to hobby rocketry & have attended my share of LDRS events. MANY years ago an event was held in a park (since banned through by-laws) and the crowd was not too far back. The general amount of CATO's in any gathering is up to 1/3 or more of the launches and many if not most of the [rocket] bodies are aluminum (and some steel). (NOTE) A Hell of a lot of by-laws have changed over time: I'm making a point about learning from mistakes in judgement....
Whether the propellant was BP or a percholate or whatever; when they go; they go fairly nasty. In those instances material was easily thrown 200 yrs @ serious velocity.

When considering safety from ANY energetic one of the first things that a well planed situation demands is an assessment of "what if the worst happens?" This way of thinking has become an ingrained standard in applications from firearms reloading to rocketry.
It's very common to forget that "low explosives" such as black powder can easily develop enough energy to drive a projectile 400-500 meters with enough energy left to drop a large game animal. Per / chlorate rate of combustion being faster may yield more powerful explosions.
There are several definitions of "high explosive" but in general the velocity of detonation is often an order of magnitude that of a low explosive. So it's within possibility that in our scenario with an exploding test tube here some of that glass may have been traveling SO fast as to be frankly a serious level of lethality.

So why didn't some of that glass sever an artery? It's possible that it was pure luck. the individual pieces were not of a weight & ballistic shape to allow enough energy to be driven behind them to driven those pieces deeper than they went initially.
Glass is tough to find on an x-ray. In WWII the Nazis used what was referred to as a "Glass Mine". It's lethality was marginal due to some of the device powdering upon detonation; yet some of the mine DID retain weight. injuries were monstrous as the x-ray units of the period were limited and other forms of photographic physical investigation, not yet invented.

My point here is that elemental safety demands that an individual project into any scenario what COULD or WOULD happen if the worst were to take place. The next proper agenda would be to NOT act upon any experiment at all - until it has been thought through and the ramifications carefully weighed.
A classic example would be to then examine the experiment & outline the appropriate modality for it's design. Then notice within the last several days has ANY static electricity been present in any form? Is there any other format for ignition, etc?

I'm sorry to say that accidents very rarely happen. An accident is in the middle of an experiment - lightning hits your work place. Unfortunately what [generally] happens in terms of resultant injury is negligence.

These are rules I personally abide by; consistently. - IF you are not willing to go that "extra mile" or not informed of all issues concerning the experiment: put it off until you are.
This also includes aspects of poisoning.... The child-like desire to "touch or handle" certain materials can lead to problems without due consideration.

EDIT:
We live in a WORLD of these agendas, yet we have come to understand where they are in everyday life. but by opening up any format of laboratory, we find more of the same. A wilderness is a classic example of a laboratory that often leads to serious repercussions if not prepared. In such an example, "accidents" are more common. Yet even there it's negligence that claims more injuries than true accidents.





[Edited on 7-6-2011 by quicksilver]

holmes1880 - 7-6-2011 at 06:50

Ok, we know the cause of all this. Let's move on.

[Edited on 7-6-2011 by holmes1880]

gnitseretni - 7-6-2011 at 07:43

Making HE's can be very time consuming. If one lacks patience it may lead to taking shortcuts! I don't know if Aqauregia is an impatient man, but he took a shortcut nonetheless! He wouldn't have had this accident had he boiled some more water. So "don't take shortcuts" is another important lesson to be learned here, in my opinion!

Print these out —

The WiZard is In - 7-6-2011 at 10:37

hang copies in your lab.

Lab-blast-800.jpg - 208kB C&H-Idiotic-in-retrospect.jpg - 76kB Blasted-800.jpg - 184kB



Thus, pyrotechnics [energetic materials] cannot be regarded as a harmless
amusement and hobby for the amateur. Only if the processor always acts under
the assumption that his mixture can spontaneously "go off" without discernible
cause will he avoid grievous injuries and damage. Unfortunately, the beginner
will often pass through an initial period of caution and anxiety followed by an
optimistic feeling of relaxation and subsequent carelessness, culminating in an
accident.

Herbert Ellern
Pyrotechnics
Kirk-Othmer's Encyclopedia of Chemical Technology 16:840
Second Edition 1968

The late Herbert Ellern was well know for his two books :-

Modern Pyrotechnics : Fundamentals of Applied Physical Pyrochemistry
Chemical Publishing 1961

Military and Civilian Pyrotechnics
Chemical Publishing 1968



unionised - 7-6-2011 at 10:58

It's good to learn from your mistakes, but sometimes it's a lot better (and less painful) to learn from other people's so thanks for posting about your incident.

By way of light relief and a celebration of the fact that you are still around to laugh

http://xkcd.com/242/

But sometimes, "normal" is good.

Erythritol Tetranitrate deflagration point

The WiZard is In - 7-6-2011 at 11:41

I found this the hard way. I looked it up in Urbanski who
ref'd Meyer 1977. I own hard copies of the 3rd & 4th eds
and PDF of the 5th & 6th. This from the 6th.


Erythritol Tetranitrate
Tetranitroerythrit; t ´ etranitrate d’ ´ erythrite
colorless crystals
empirical formula: C4H6N4O12
molecular weight: 302.1
oxygen balance: +5.3%
nitrogen content: 18.55%
volume of explosion gases: 704 l/kg
heat of explosion
(H2O liq.): 1519 kcal/kg = 6356 kJ/kg
(H2O gas): 1421 kcal/kg = 5943 kJ/kg
specific energy: 111 mt/kg = 1091 kJ/kg
density: 1.6 g/cm3
melting point: 61.5 °C = 143°F
deflagration point: 154–160 °C = 309–320°F violent explosion
impact sensitivity: 0.2 kp m = 2 N m


djh
----
An explosion may be defined as a loud noise
accompanied by the sudden going away of
things from the places where they were before.

Joseph Needham

holmes1880 - 7-6-2011 at 11:53

^^^^^^
@Wizard

Well, Sherlock. Then why isn't everyone using ETN as a primary then? God....


There is a context to this condition- ETN has to be very well confined to undergo DDT. When weakly confined, it can only do that with a very rapid rise in heat. In addition, ETN will not undergo DDT when in loose powder form- it will first melt, then deflegrate. NOT even when confined- well, it might do that 1/10 times, but it will be a rare occurence.





[Edited on 7-6-2011 by holmes1880]

The WiZard is In - 7-6-2011 at 12:08

Quote: Originally posted by holmes1880  
^^^^^^
@Wizard

Well, Sherlock. Then why isn't everyone using ETN as a primary then? God....


It fails test #1 for an explosive.... it is not safe at any speed.
US usage of explosive and blasting agents is ca. four-thousand
million pounds a year. Money counts in the real world. (Granted
only a fraction of the 4 to la 9th pounds are primaries.)

There are hundred's and hundred's of primary explosives yet
of these perhaps a half-dozen are most commonly used — the
ones that are as safe as can be be reliable put to work. A
hang fire is a nasty animal!

And ... most importantly it has to work. Why certain explosive
make good primaries is not science — it is black magic. (Unless
you can come up with good refs. I am a member of the black magic school.)



djh
----
The loneliest person in
the world is — the one who
lights the fuse.



[Edited on 7-6-2011 by The WiZard is In]

[Edited on 7-6-2011 by The WiZard is In]

[Edited on 7-6-2011 by The WiZard is In]

Cloner - 7-6-2011 at 12:08

Quote: Originally posted by PHILOU Zrealone  


I would personnaly never cast/heat a nitric ester, nor recristallize it from ethanol...maybe the word transesterification is unknown to you but:
O2NO-CH2-R-ONO2 + CH3-CH2-OH <==> HO-CH2-R-ONO2 + CH3-CH2-ONO2
So from polynitrate esters you end up with hydroxypolynitricesters and volatile ethyl nitrate...


[Edited on 7-6-2011 by PHILOU Zrealone]


Does this really happen, and how much so? As far as I remember, Etoh is frequently mentioned and I once made some ETN of good purity verified by NMR after recrystallization from Etoh. Hydroxyl would have shown up in the spectra. While ethylnitrite would evaporate, the other impurity would stay after drying and show itself.

I can confirm that I once melted a few hundred milligrams of ETN on a teaspoon with a cigarette lighter without disaster. I guess I was really lucky.

[Edited on 7-6-2011 by Cloner]

[Edited on 7-6-2011 by Cloner]

holmes1880 - 7-6-2011 at 12:38

Quote: Originally posted by The WiZard is In  


It fails test #1 for an explosive.... it is not safe at any speed.
US usage of explosive and blasting agents is ca. four-thousand
million pounds a year. Money counts in the real world. (Granted
only a fraction of the 4 to la 9th pounds are primaries.

[Edited on 7-6-2011 by The WiZard is In]


What? What "safe at any speed"? And I don't mean commercially....I mean in amateur use. I don't see people lighting ETN up like a primary. It doesn't detonate from fuse with any kind of reliability. I once had magnesium filings on top of ETN in a PVC pipe, but not well confined........and ETN didn't detonate.

The end.

holmes1880 - 7-6-2011 at 12:40

Quote: Originally posted by Cloner  


I can confirm that I once melted a few hundred milligrams of ETN on a teaspoon with a cigarette lighter without disaster. I guess I was really lucky.

[Edited on 7-6-2011 by Cloner]


You weren't lucky. ETN wasn't confined and the mass wasn't significant. It has to be heated rapidly and have confinement.

Confinement, confinement, confinement. Actually, with enough heat and confinement any secondary will go even cyclonites and HMXs....believe that. :cool:

[Edited on 7-6-2011 by holmes1880]

m1tanker78 - 7-6-2011 at 13:06

AquaRegia: Now you have some battle scars to show the young'ins. The smaller shards of glass that were missed will slowly surface. At some point, you'll be able to pick some of them out yourself. I'm sure you already know how fortunate you are! Thanks for garnering up the huevos to post your accident.

Regarding your comment about selling off your glass...

Why don't you just pack it away for a few weeks or months and then start from scratch, so to speak? Selling it off seems rather rash (but I certainly understand your motivation). I hope you get back up on [a more tame] horse someday.

Tank

Somebody has to do the work...

The WiZard is In - 7-6-2011 at 13:22

check the obvious refs.

This sucked out of my PDF copy of PATR-2700 (I also own
a hard copy.)

But first - how 'bout a little professionalism... and this is
not the first time I have mentioned it here. Could we stop
making up abbreviations?! ETN Notice? Yes!
PATR-2700 uses ErTeN.

NB - It sez — mp 61o detonates violently

Moving on ... there was a copy of ref (16) Detonation in
Condensed Explosives for sale....!

Naoúm ref. (6) has been reprinted I own a copy, you can
me thinks DL yours from Google.com/books. The ref is only
a single paragraph.

Danile ref (5) Poudres et explosifs: dictionnaire des matières
explosives By Jacques Daniel. [It can be DL'd from
Google.com/books which dobe where I got my copy.]

I don't speak/read French, however, cet éther détone avec
violence; il est très sensible, également, à l'action du choc.
caught my eye.... so I ran it through BableFish

this ether explodes with violence; it is very sensitive, also, with l' action of the shock

Ref (19) The Condensed Chemical Dictionary, 1961 (you will
never guess who owns a copy.) has a one sentence description
that add's nothing new.


Attachment: Explosive ErTeN PATR2700.docx (401kB)
This file has been downloaded 708 times



djh
----
Allow me to rework an
old expression —

30-minutes in a
library can often save
30-days in hospital.

The WiZard is In - 7-6-2011 at 13:36

Quote: Originally posted by holmes1880  


What? What "safe at any speed"? And I don't mean commercially....I mean in amateur use.



You forget the difference between amateurs and professionals....

If a pro blows himself up... he can collect workman's comp -
possible sue. The amateur .... is using whatever money he
had/can borrow to hire a lawyer to keep what's left of them out
of the gaol.

I operate under the - at my age 15-years is a life sentence
epistemology of political safety.


djh
-----
The difference between
high explosives and low
explosives is — small
pieces vs. big pieces.



Wayward Bodies
[Words attributed to unknown British Soldiers
1854/1856.] One of several versions.

Did you ever think when a hearse goes by,
That you may be next to die?

They take you out to the family plot,
And there you wither, decay and rot.

They wrap you up in a bloody sheet,
And then they bury you six-feet deep,.

And all goes well for a week or two,
And then things start to happen to you.

The worms crawl in the worms crawl out,
The ants play pinochle on your snout!

One of the worms that's not so shy,
Crawls in one ear and out one eye.

They call their friends and their friends' friends too,
They'll make a horrid mess of you!

And then your blood turns yellow-green,
And oozes out like whipping cream.
[Spoken] Darn, me with a spoon!

Your eyes fall in your teeth fall out,
Your liver turns to sauerkraut.

So never laugh when a hearse goes by,
For you may be the next to die.

Get a better source

holmes1880 - 7-6-2011 at 13:46

And.....this 100 year old reference is supposed to be some sort of source? They say ETN is friction sensitive............what kind of sh*t were they making? I've never ever ever had ETN go off from friction via rubbing of sandpaper on sandpaper with a hammer and applying all my weight to make it go off. I've done this numerous times. This paper has as much credibility as I do......probably less since I've done more actual testing.



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.


[Edited on 7-6-2011 by holmes1880]

holmes1880 - 7-6-2011 at 14:00

@ Wizard

You still didn't answer what you mean by "safe at any speed". I thereby hold you in contempt for trolling!


Difference between professional and amateur is the frequency of use-let's not forget that. Monotonous work produces lapses in judgement, therefore being more dangerous. It's also a matter of probability- the more you do, the more you get.



The WiZard is In - 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.


gregxy - 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?

holmes1880 - 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]

holmes1880 - 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]

to sherlock holmes

aquaregia - 7-6-2011 at 22:50

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!

This is a question for the experts

aquaregia - 7-6-2011 at 22:57

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.

a_bab - 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.

mabuse_ - 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?

holmes1880 - 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]

holmes1880 - 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.

a_bab - 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.

holmes1880 - 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.

Blasty - 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.

The WiZard is In - 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.

gnitseretni - 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.

Polverone - 8-6-2011 at 13:39

Please keep discussion in this thread civil.

The WiZard is In - 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]

Blasty - 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]

holmes1880 - 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]

holmes1880 - 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]

Rosco Bodine - 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.

holmes1880 - 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]

Rosco Bodine - 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]

holmes1880 - 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.

melted ETN or not.

aquaregia - 8-6-2011 at 22:27

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.

Rosco Bodine - 8-6-2011 at 22:34

@holmes1880 Precisely, the so called safety detonators use a fast hot pyrotechnic to generate a thermal shock induced detonation of the base charge. It isn't as positively reliable as an overdriven initiation by a primary, but it will cause sensitive secondary explosives that are actually borderline to being primary explosives to detonate. As was said by Davis in COPAE "MHN is almost but not quite a primary explosive", the same is true for NG, ETN, and some other sensitive secondary explosives. In larger quantities, PETN will undergo DDT and so will nitrocellulose.

@aquaregia A waterbath and a polypropylene test tube
would have been a better way to go. A kinder gentler approach to materials like ETN is required.

[Edited on 9-6-2011 by Rosco Bodine]

The WiZard is In - 9-6-2011 at 06:16

Quote: Originally posted by holmes1880  
A guy heating it with a TEA spoon has been warned few times by me and another few people, but he still did it. He actually showed what happens when ETN gets overheated over a candle flame in a spoon- it starts pumping out NO2 brown smoke until igniting. If it detonated in a spoon he'd have no shrapnel, but would probably be deaf for a few minutes.


Never-ever underestimate la spoon full.

Extracted from

RED PHOSPHORUS -- BRIDE OF FRANKENSTEIN
By Donald J Haarmann
American Fireworks News May, 1991

Perhaps the most famous victim (excluding your
fingers-still-intact author) of this infernal
l combination is Donald Sisco, better known as
"Kurt Saxon" of "Poor Man's James Bond" fame.
The following is quoted from his book:

"The photograph shows a spatula which
had been used to stir a mixture of about
1/2 half ounce of potassium chlorate and a
bit of red phosphorus. The mixer was
ignorant of the fact that these chemicals
together, stirred dry, will detonate
spontaneously.

"The resulting blast kneaded the spatula
out of shape. It atomized the first 3/4 inch of
the bone handle and split the rest. It
shattered the plastic mixing bottle.

"The fingers holding the bottle had
the flesh blown off the bones and the bare
bones had to be amputated. The palm of
the hand was turned to hamburger and its
inner bones were smashed.

"The hand holding the spatula was
undamaged except for particles of plastic
bottle which pierced the skin."

--------
Luck he? Yes. It was only a pyrotechnic mixture
and not an explosive.


djh
---
Daedalus

Tension in miniature

The smaller a component, the stronger it
tends to be - which explains the value of
fine-fibre reinforcements. A very fine fibre
can carry so much tension as to reach
an almost explosive strain-energy density.
Daedalus is now devising a fine
powder whose particles are tense with
locked-in stress.

Stress, he remarks, can accumulate
during crystallization. A needle crystal,
growing in solution and bent while it is
still very narrow, will develop intense
stress as it thickens. Successive sleeves
of new molecules are deposited under
compression on its inner radius and under
dilation on its outer one. If it cannot
straighten, the accumulating stress will
snap it. So, says Daedalus, grow a
needle-crystal compound on a micro-scale
circular seed, and it will thicken into a
tiny ring, tense with stress. A small shock
will crack it; it will snap straight,
releasing its energy ballistically as flying
fragments.

DREADCO chemists are now trying it.
Their circular seeds are plasmids, ring-
polymer molecules, and ring-shaped
structures made by coating a micro-fine
wire, stretching it to shatter the coating
into tiny rings, and dissolving it to release
them. The chemistry is still unfocused and
exploratory, but some promising
systems should emerge soon. The final
product will look like any ordinary white
powder: flour, salt or cement. But it will
be tense with strain energy.

DREADCO's Stressed Powder, crystallized
almost to spontaneous explosion, will
be highly dangerous. its fiercely
screwed-up particles will need a thin inert
coating to prevent the mutual abrasion
of handling or pouring from setting them
off. It will form a novel physical explosive.
Fired by a sudden shock, it will release
no chemical fumes, just a violent hot
blast of abrasive fragments. A weaker
grade of Stressed Powder, removed
from the crystallizing bath earlier, will
have wider uses. It will make a splendid
active abrasive, cutting through the hardest
Workpiece by forceful local energy release.
It will transform the technology of
surface abrasion, from etching to
paint-removal to dental hygiene.
Grit-blasted at a workpiece from an
air-nozzle or sunk into it from a
flexible pipe, Stressed Powder will
penetrate like a drill. It will solve
the age-old problem of making a
deep hole, maybe curved or of
non-circular cross section, in a
hard solid. Electricians facing the
once intractable task of putting
wiring into an old stone
building will bless the name of
DREADCO.

David Jones
Nature 406 [24] August 2000



holmes1880 - 9-6-2011 at 07:18

@Rosco

I believe it can be as reliable as with a primary initiated charge, otherwise they wouldn't make them commercially, I'd imagine. Here's a sample detonator using undisclosed pyrotechnic mixture. I don't think it's thermite since the system requires very low voltage to ignite it-and thermite, most kinds, are notoriously difficult to fire up.
http://www.dynonobel.com/NR/rdonlyres/TDS%20-%20Initiation%2...

I think ETN is the midpoint between PETN and NG/MHN/EGDN. The latter are at least 2X impact sensitive and MHN can actually go off from being squeezed between pliers, or I was told.

The WiZard is In - 9-6-2011 at 08:00

Quote: Originally posted by Rosco Bodine  
@holmes1880 Precisely, the so called safety detonators use a fast hot pyrotechnic to generate a thermal shock induced detonation of the base charge. It isn't as positively reliable as an overdriven initiation by a primary, but it will cause sensitive secondary explosives that are actually borderline to being primary explosives to detonate. As was said by Davis in COPAE "MHN is almost but not quite a primary explosive", the same is true for NG, ETN, and some other sensitive secondary explosives. In larger quantities, PETN will undergo DDT and so will nitrocellulose.

@aquaregia A waterbath and a polypropylene test tube
would have been a better way to go. A kinder gentler approach to materials like ETN is required.



Well as I posted a few back ... DuPont patent'd an explosive
based on ErTeN.

Primary? A Sand Test result for ErTeN would be useful. Any volunteers?



Attachment: 1751436.pdf (119kB)
This file has been downloaded 835 times

Rosco Bodine - 9-6-2011 at 08:06

@holmes1880, Apples and Oranges. That type detonator uses a different principle and system from the typical safety detonator. It uses a progressive density loading in a tuned aperture to shorten the runup distance for DDT, and these have been used with PETN alone. These type detonators require exacting control over the particle size and progressive loading density and the geometry of the confinement which is a reenforced detonator type, and if anything is out of precision spec they fail, so they are more difficult and complex and expensive to manufacture.

[Edited on 9-6-2011 by Rosco Bodine]

holmes1880 - 9-6-2011 at 08:37

Be as it may. I think thermite would work without hickups. It would be far more desirable to replace PETN with RDX. I'm sure RDX can be detonated via thermal shock, question is in the delay time.

@Wizard
I don't have sodium nitrate or woodmeal. I did see a video of people mixing ETN/AN in larger quantities, making a very OB positive mix. It works, but is a waste of ETN, IMO.

Rosco Bodine - 9-6-2011 at 08:51

Thermite itself is difficult to ignite so advantage would be lost there for needing
something to ignite the thermite, and it requires a specialized sort of thermite based on barium peroxide IIRC. Anyway this discussion seems to be wandering off course. There is a lot of technology which seems to be a solution in search of a problem to solve that really isn't a problem.

The WiZard is In - 9-6-2011 at 09:16

Quote: Originally posted by Rosco Bodine  
Anyway this discussion seems to be wandering off course.


Driving thread off the road where it crashes and burns....

If you run DDT Detonators through Google Patents
you will get 6-hits.

Now back to the original topic... >


1700 Gram Sand Tests



Explosive grams % TNT
crushed

PETN 57.9 140
Mannitol Hexanitrate 56.4 137
Cyclonite (RDX) 53.2 129
EDNA 48.4 117
Teryl 47.7 116
Dinitroethyleneurea 45.0 109
TNB 43.2 105
Picric Acid 41.8 101
Trinitroanisole (TNAns) 41.7 101
TNT 41.2 100
Trimonite 39.9 97
Diazodinitrophenol 39.7 96
(DADNPh)
Trinitrotehylbenzene 36.3 88
(TNEB)
Trinitroxylene (TNX) 34.5 84
Ammonium Picrate (AP) 33.7 82
Amatol 40/60 33.4 81
Amatol 50/50 34.0 83
Dinitrobenzene (DNB) 23.6 57
Mercuric Fulminate (MF) 22.5 55
Lead Azide (LA) 18.6 45
Lead Styphnate (LSt) 10.9 26

From: PATR 2700 B298

The fact that this is on my HD had slipped off my mind

The WiZard is In - 10-6-2011 at 13:57

Journal of the Society of Chemical Industry
Vol. 18 1899 p. 83

ERYTHROL TETRANITRATE: A CAUTION.
Chem. and Druggist, Jan. 14, 1899, 59.

A correspondent of the British Medical Journal states that he
recently received by post a sample labeled erythrol tetranitrate, a
white powder in a small glass bottle. There were no directions or
dose printed on the bottle, so he put it in the waste-paper basket.
Result: an explosion occurred next morning, and the cook was
partially stunned and received about two dozen small wounds on
the hands, arms, and face, three or four containing glass. The
housemaid had emptied the waste-paper basket into the dustpan
containing hot ashes. " So explosive a compound as erythrol
tetranitrate should surely not," adds the correspondent " be sent
out without special precautions."

pg. 315

ERYTHROL TETRANITRATE.
Chem. and Druggist, March 18, 1899, 443

The Home Secretary states that erythrol tetranitrate is not an
explosive within the meaning of the Explosives Act, but the
question is under consideration whether an official warning should
be issued calling attention to its explosive character.

pg. 415

OFFICIAL NOTICE.
ERYTHROL TETRANITRATE.

SIR,

An accident, by which a chemist lost his life, happened at a tabloid
factory at Dartford on December 15,1897. He was engaged in
mixing tetranitrate of erythrol with finely-powdered lactose in a
mortar when an explosion occurred.

Again, at the end of 1898, an accident was caused by tetranitrate
of erythrol being inadvertently thrown into a fire, and one person
was injured.

Tetranitrate of erythrol is possessed of explosive properties, and is
highly sensitive more so, indeed, to percussion than dynamite or
guncotton. As it has lately come into some use in the place of
nitro-glycerin as a remedy for angina pectoris, I should be glad if
you would draw special attention in your paper to the dangers
attending the handling of this drug.

I have the honour to be, Sir,
Your obedient Servant,
A. FORD (Colonel),
H. M. Chief Inspector of Explosive.
Home Office, Whitehall, S.W., March 24.




The Dangers and Uses of Erythrol-tetranitrate.
The Medical bulletin: a monthly journal of medicine and surgery,
Volume 20 1898

We have received from Messrs. Burroughs, Wellcome & Co., a
detailed account of the circumstances attending the fatal explosion
of erythrol-tetranitrate, which occurred at their works at Dartford.
It appears that the deceased—a qualified chemist—was engaged
in stirring together in a mortar a mixture of erythrol-tetranitrate
and lactose, presumably for the purpose of making tabloids. The
quantity of the active drug served out to him was four ounces, and
there is reason to believe that the dangerous nature of the
combination was fully explained to him at the time by the chief of
the department. The explosion was violent, but its effects were,
fortunately, local. The jury returned a verdict of "accidental death,"
and passed a resolution expressing their appreciation of the
facilities placed at their disposal by the firm for investigating the
circumstances of the case. For much of our knowledge of the
physiological action of erythrol-tetranitrate and its congener,
mannitol-hexanitrate, we are indebted to Professor Bradbury, of
Cambridge, who gave some account of the pharmacology of these
substances, based chiefly on a series of experiments made by Mr.
Marshall, M.B., in Professor Schmiedeberg's laboratory at
Strassburg.

Erythrol-tetranitrate is solid and crystalline, and melts at a
temperature of 61° C. (142° F.). When pure it is colorless, and if
kept in a dark and moderately cool place is fairly stable. If exposed
to warmth, and especially sunlight, it rapidly undergoes
decomposition, turning yellow and giving off nitrous fumes. Its
solubility in water is slight, but it dissolves readily in alcohol and in
ether. It is a vasodilator and belongs to the group of which
glycerol-trinitrate, known familiarly as nitroglycerin, may be
regarded as the typical representative. Blood-pressure
experiments show that the nitrates of erythrol and mannitol have a
less marked, but more prolonged, action than those of glycerol
and glycol. On theoretical grounds, it might be supposed that the
new remedies would be useful in the treatment of cardiac pain,
Bright's disease, migraine, and Raynaud's disease, but, as far as
we have been able to learn, there has been very little demand for
them. Professor Bradbury, in a letter, states that he is able to
speak very highly of its therapeutic properties in warding off
attacks of angina pectoris. Dr.- Garraway mentions the case of a
who has derived immense relief from its use, and won long
periods of complete immunity. Dr. Bradbury, in the lecture to which
reference has been made, stated that the dose of the solid organic
nitrates was a grain, but that more might be given if thought
necessary. He suggested that they should be taken in the form of
pills or tablets or in alcoholic solution. There is now, unfortunately,
very little doubt that these new organic nitrates cannot be handled
with impunity in any form in which trituration is necessary. They,
in common with many other nitrates, were known to be explosive,
but that they would develop such activity by being merely gently
stirred with lactose could not have been foreseen, although
Professor Bradbury in his letter expresses the opinion that, mixture
with some readily oxidizable substance might increase the liability
to explosion.—British Medical Journal.

Rosco Bodine - 10-6-2011 at 17:05

Quote:
"Result: an explosion occurred next morning, and the cook was
partially stunned and received about two dozen small wounds on
the hands, arms, and face, three or four containing glass. The
housemaid had emptied the waste-paper basket into the dustpan
containing hot ashes."


Yogi Berra .....It's deja vu all over again

holmes1880 - 10-6-2011 at 20:35

How unusual. ETN was filed for patent in 1927, yet these accident are happening in the late 1800's.

I doubt they were using the erythrol product we're working with today. It was still the dawn of HE, and I'm sure the production process was far from optimal.

[Edited on 11-6-2011 by holmes1880]

The WiZard is In - 11-6-2011 at 07:16

Quote: Originally posted by holmes1880  
How unusual. ETN was filed for patent in 1927, yet these accident are happening in the late 1800's.

I doubt they were using the erythrol product we're working with today. It was still the dawn of HE, and I'm sure the production process was far from optimal.


Me thinks your transmitter works but you receiver has burned out.
As I had posted sometime ago ErTeN (to be professional) was
first made in 1847.

"filed for patent" is academically lame, without a issuing country
and patent number it is impossible to know what you are talking
about. I would posit your patent was for a specific method of production.

"production process far from optimal." If you are synthesizing it
by the pound for use as a drug any process is good enough —
by the ton for use as an explosive - only the most efficient
process is good enough.

And ... whatever method was used to produce it ... it went KAFUCKINGBOOM.

ErTeN's first use was for the treatment of Angina Prectoris,
currently nitroglycerin and PETN are used. I don't know when
its explosive properties were discovered.

From my ever useful copy of WB Campbell, Hand-Book of Modern
Medical Treatment and Medical Formulary, 1912.

P.368

Angina Pectoris.

Erythrol-tetanitratis gr j.
Alcohois, f13j.
Aquae dest. f3vij

Let me say another dirty word here — history.

Picric acid was first made by first noticed by Glauber 1742,
however, it was not until 88-years latter 1840, that Welter
suggested its use as an explosive.


djh
----
Trivia —

Campbell suggest injecting carbolic acid
to treat a felon.

You can make picric acid from public hair
and other common household products.







holmes1880 - 11-6-2011 at 08:22

Keep it together, old man. Ammonium nitrate also exploded once and so did nitromethane. Everything that's explosive can explode if required conditions are met.

I know you're not used to Google, but here you go:

http://www.scribd.com/doc/25882721/Erythritol-Tetranitrate-E...

a_bab - 11-6-2011 at 12:01

Ammonium nitrate exploded way more then once, and I'm not talkin' ANFO here but that nice fertilizer that once instantly vaporised in a huge fart leaves a horrible red plume of NO2.

holmes1880, you suggested you'll leave this thread once. Your evolution here went like:
- being critical with the initiator - launching the "confinementsky theorietzki" - trolling - promissing to leave the thread - trolling again - more trolling - ...

All you did here was trolling, mostly. Then you trolled even more. By trolling I mean useless, irrelevant interventions. Obviusly, ETN is the subject of your thesis, and you probably use it to salt up your food or something. So it looks at least. Or you want to.

Oh, BTW: you don't want to know the purity achieved by the early 19'th century chemists in their synths. You can't compare it with your home setup, using draino etc. no matter how much you'd dream about. Read a bit about Bunsen's life for instance, or any other chemist from that period. I'm sure you can't make your own ultra balance, nor can you blow your own glassware.

Really, just fuck off.

The WiZard is In - 11-6-2011 at 12:18

Quote: Originally posted by holmes1880  
Keep it together, old man. Ammonium nitrate also exploded once and so did nitromethane. Everything that's explosive can explode if required conditions are met.

I know you're not used to Google, but here you go:


The (my point) has missed the target.

The fact that ErTeN was an explosive was discovered by accident.

Howard - mercury fulminate, DuLong - nitrogen trichloride,
"Bunsen met with a severe accident in 1841 while analyzing the
cyanide of [k][c]acodyl. The combustion tube exploded and injured
one of his eyes, and the experimenter himself lay for weeks
between life and death, owing to the combined effects of the
explosion and the poisonous nature of the vapor." Ascanio Sobrero
- nitroglycerin. All found out the explosive nature of their
inventions when they bit them in the ass.

My 6th edition copy of Bretherick's Handbook of Reactive
Chemical Hazards is 1 926 pages of unexpected results.


----
Noted in passing ..

Bunsen called his compound Kacodyl after the Greek - meaning
smells worse than a used woman.

I would note (patting self on back) that I am cited in Bretherick's
6th page 1376. #4017, Potassium chlorate - Phosphorus (red).


djh
----
"Tramp" explosives or detonators are like
poisonous snakes — usually strike when least
expected. More often than not, they badly maim
or destroy the eyesight or other parts of the
body of their victims.

US Bureau of Mines
IC7038

quicksilver - 11-6-2011 at 12:22

Does this thread need to be closed or can we deal respectfully with each other?

holmes1880 - 11-6-2011 at 12:23

@a-babe

Is this that time of the month for you? You're way too angry and emotional. Every post in here has been a silly little attack of me. Get lost.


EDIT @ quicksilver:

a-bab is crossing some lines here. Not the first time either.

[Edited on 11-6-2011 by holmes1880]

Lord Emrone - 12-6-2011 at 06:02

It's a bad idea to melt ETN and people don't know this. I've done it twice above a candle, luckily nothing happened.

Maybe members of this forum should make a manual on how to synth and handle safily this kind of explosives.

My two cents...

albqbrian - 12-6-2011 at 06:42

First, AR a big thanks for sharing. It's very difficult to go public when you did something that in hindsight you just can't believe you did. You're certainly not alone in doing something like that; but you are unusual in sharing it for all of our benefit.

A disclaimer. I had an inadvertent explosion in my hand a long time ago. It involved some flash powder that I'd made many times previously. But that day, for whatever reason, it went off. Luckily it was a small quantity and only wrapped in tissue paper. I got away with 2nd degree burns on my wrist. And quite an ass chewing from my family doctor. After that I've been much more cautious. Anyone working with energetic materials is always taking a chance. You must realize that, decide that you are thus going forward, and do all you can to protect yourself.

AR's accident has some additional instructional value. In another thread we discussed shielding and examining your set-up to see how it would propel itself as shrapnel if things went wrong. Look at AR's pic; you see a classic shrapnel pattern from an exploding cylinder. Things fly radially from the long axis. That's why when I test rocket motors I bury them upside down. If the thing goes boom the pieces all get flung into the dirt walls. I'd say AR was holding the tube in his right hand with the open end slightly above horizontal. His body art certainly suggests that. I'd also guess that, in this case; it was a good thing the tube wasn't too far away from his body. A greater offset would have "opened up" the pattern and the shrapnel would have hit his face.

If you're going to work on energetic materials think of what will protect you if the stuff blows up. Because you're dealing with probabilities, not certainties. Can you shield yourself? Can you use remote handling? Etc., Etc.

AR, I wouldn't bail on chemistry right now. Yes, this has refocused you on your family which is correct. However you're still in a vulnerable place emotionally. Take a few months off. There are many ways to dabble in our beloved field with the direct, very risky HE path. maybe rocketry will interest you and your little one, maybe volunteering at a school, who knows. Just give it some time.

On a less pleasant angle. I suggest you get a consultation with a criminal defense attorney. So if you are contacted by a cop you don't say or do anything that could cause you more problems; problems that should be avoidable if you have a good legal plan.

Best of wishes for your recovery!

The WiZard is In - 12-6-2011 at 09:30

Quote: Originally posted by albqbrian  

If you're going to work on energetic materials think of what will protect you if the stuff blows up. Because you're dealing with probabilities, not certainties. Can you shield yourself? Can you use remote handling? Etc., Etc.


I have always thought this a good idea.


Rocket-motor-shield.jpg - 101kB


Extracted from :—

Teleflite Corporation
Building Your Own Rocket Motors

Predecessor to :—

David G. Sleeter
Amateur Rocket Motor Construction:
A Complete Guide To The Construction
Of Homemade Solid Fuel Rocket Motors

holmes1880 - 12-6-2011 at 11:23

I use a wooden block 2X4 about 3'' long to press ETN caps in thin aluminum. If for some reason it goes bang, the wood should catch most of the aluminum and the 3 layers of tape prevent wood from going at very high velocities in a small splinters. My fingers would be 1'' away from the block and I expect to have no permanent injuries at that distance. Caps range between 0.5-1g.

protection 002.JPG - 62kB

The WiZard is In - 12-6-2011 at 11:39

Quote: Originally posted by holmes1880  
I use a wooden block 2X4 about 3'' long to press ETN caps in thin aluminum. If for some reason it goes bang, the wood should catch most of the aluminum and the 3 layers of tape prevent wood from going at very high velocities in a small splinters. My fingers would be 1'' away from the block and I expect to have no permanent injuries at that distance. Caps range between 0.5-1g.


My WAG would be even the best tape in La Word "Gorilla" brand
Duct tape would not stand a chance. And by the by .... wood is
not radiopaque. Glass is not much better. If you are going to use
glass used leaded glass, melt down the front screen from your old
CRT monitor - Grandma-ma's crystal-ware.

Put your device to a test or two and please report back.

djh
----
Extracted from :—
Tell The WiZ (donald j haarmann)
American Fireworks News # 38 November 1984


USES FOR PYROTECHNICS YOUR MOTHER NEVER TOLD YOU ABOUT.
THE WORLD'S MOST EXPENSIVE FOUNTAIN — THE HYDROGEN BURNOFF IGNITER.

[Watch for it on the next/last Space Shuttle Launch.]

The device was designed to burn off excess hydrogen gas near the
Space Shuttle main engine nozzle immediately before ignition.
Design'd to function for 8+2 seconds, producing a
three foot flame with a temperature greater than 1500 degrees F
at maximum output, while projecting hot particles 15 feet when
fired directly into or perpendicular to a 34.5 knot wind (40 mph).
[If indeed this gem can project hot particles 15 feet perpendicular
to a 40 mph wind, it must hum!]

A total of 46 units were fabricated, and of these 21 “were to go into
lot qualification and 20 units were for shipment". [How would you
like to test to destruction every other device you produce before
sale?!]

You can DL the complete copy of this report from the DTIC.

[Edited on 12-6-2011 by The WiZard is In]

holmes1880 - 12-6-2011 at 12:16

I use electrical tape, gorilla tape, and again electrical tape. It would be shocking if the wood would splinter through those layers. I'm wearing thick goggles, just in case, so I'd be all right. Hearing would suffer, I'm sure, but in the short term.

P.S. Yes, I need to put it to the test in a thick cardboard box to see how the splinters behave and whether the wood is catching the aluminum shrapnel.


[Edited on 12-6-2011 by holmes1880]

Lord Emrone - 12-6-2011 at 15:15

holmes, your ETN-press-thing doesn't look safe. You should surround the cap with an absorbing material like styrofoam. Wood doesn't absorb. If your fingers are in the same position as on the picture during a det, you could very well lose your thumb. And instead of aluminium you should use paper.

Rosco Bodine - 12-6-2011 at 15:44

Maybe it was ignorant shipbuilders who constructed the decks of battleships from laminated wood timbers. Yeah it was probably conjecture and not engineering
which caused wood to be selected as the material of choice.
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