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holmes1880
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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]
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aquaregia
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ETN was recrystallized in Etoh
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...
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Microtek
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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.
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mabuse_
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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.
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aquaregia
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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?
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holmes1880
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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.
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Bowdlerize
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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".
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aquaregia
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well bowdlerize,
that single post from you makes mine worth it. be safe
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PHILOU Zrealone
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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]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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quicksilver
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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]
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holmes1880
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Ok, we know the cause of all this. Let's move on.
[Edited on 7-6-2011 by holmes1880]
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gnitseretni
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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!
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The WiZard is In
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Print these out —
hang copies in your lab.
  
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
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unionised
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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.
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The WiZard is In
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Erythritol Tetranitrate deflagration point
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
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holmes1880
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^^^^^^
@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]
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The WiZard is In
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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]
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Cloner
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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]
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holmes1880
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| 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.
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holmes1880
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| 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. 
[Edited on 7-6-2011 by holmes1880]
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m1tanker78
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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
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The WiZard is In
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Somebody has to do the work...
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 706 times
djh
----
Allow me to rework an
old expression —
30-minutes in a
library can often save
30-days in hospital.
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The WiZard is In
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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.
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holmes1880
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Get a better source
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]
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holmes1880
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@ 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.
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