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Microtek
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I think the practise of breaking up a cast block of ETN (by hand) is a little iffy. If I was to do something similar, I would heat a beaker of water
to ca. 70-80 C with fast magnetic stirring, add the moist, purified ETN directly into the water, adjust the stirring speed until a suitable droplet
size had been attained and then cool the mix with continued stirring. This would likely result in ETN prills of the desired size, without any
grinding, and without melting the ETN dry.
Additionally, the dispersion of the molten ETN droplets probably reduces the sensitivity markedly. NG agitated in water in this manner reportedly
cannot be initiated with a number 8 detonator.
[Edited on 27-10-2015 by Microtek]
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zeroberts
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Return and report, deriving prills from cooling molten ETN stirred in water:
This method appears fairly effective. While the hot water/molten ETN were being stirred distinct round droplets of ETN could be observed swirling in
the beaker. High speeds whipped it into a frenzy of tiny droplets while slow speeds were unable to adequately agitate it so some tuning was needed.
I attempted cool the water while it was stirring by slowly adding room temperature water with a wash bottle, but I was too aggressive; resulting in
several globular masses.
Another process was attempted, cooling again with water added from a wash bottle but at a more gradual pace; results coming closer to the desired
prills, though still globular and varied in size.
Tonight I will allow the water to cool naturally to observe the results more patiently.
Aside from rate of cooling and its effect on resulting form; the crystal pieces are much harder than when ETN is simply melted and poured. Which means
they will be even cleaner to handle. Which is a large motivator in this process.
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Bert
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Perhaps an ultrasonic transducer on the water filled beaker combined with rapid stirring could get you REALLY fine prills?
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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zeroberts
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Im shooting for larger than that would give me for sure haha. That would be.. Thoroughly prilled.
Also for my own reference: is ETN typically odorless? Or should I be concerned by the slight.. I guess.. "mulchy" smell I'm detecting
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Aurium
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I'v had true recrystalized ETN and "fake" recrystalized ETN, as in dissolved in acetone, then letting the acetone evaporate.
The good white recrystlized ETN had no smell, however the faked one did smell quite a bit. I can't really describe the smell thou xD.
Since this thread turned out to be about making ETN, has anybody here ever used some other method of neutralizing the ETN other than with Sodium
Bicarb?
This because Sodium Bicarb. causes the ETN to inflate leaving me with a foam impossible to handle, making a huge huge mess.
I'd guess one can use ammonia but the only method I have of measuring pH is those pool indicators, a liquid test to mix with the water, or a solid
test strip that changes color.
Hey, if anyone has experience with this method please do comment.
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zeroberts
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I'm not saying it stinks up the place you really have to get down on it to smell it at all. Most mysterious given that it is properly recrystallized,
twice; this isn't some back yard shake and bake ETN here.
And maybe it's just me; but for me, the foamy mess you mention is manageable if you are using a filter of appropriate size for the quantity you are
producing. Thorough rinsing with a wash bottle tends to abate the issue.
Update on the prilling method:
I have this process dialed in to get consistent results of very desirable quality. Nuanced but generally simple. Now to filter my notes into a
procedure. This is exactly perfect and thank you to those contributing to a practical means to my end.
[Edited on 7-11-2015 by zeroberts]
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OneEyedPyro
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ETN should be completely odorless so I'm not really sure what you've got going on there but it's obviously not pure ETN.
Giving the ETN a few good rinses with water before hitting it with the bicarb solution will help keep the foaming down.
[Edited on 7-11-2015 by OneEyedPyro]
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zeroberts
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Whatever the smell was its gone now after processing the ETN into prills. Which I figured I'd toss up a picture in case there was any interest in the
outcome of that venture. I guess you could say I'm pretty satisfied with the results.
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OneEyedPyro
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That looks quite nice and uniform, good job. I would also be satisfied 
It should make for a powerful, quick to set up and very cap sensitive booster material.
I wonder what the density is. I may have to try this myself just for the easy/mess free handling.
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PHILOU Zrealone
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The following links are related:
entolite 1
entolite 2
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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nitro-genes
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Cool to see this actually works A very small amount of detergent may also help
to reduce droplet size, it will likely further add a hydrophilic layer around the droplets that prevents fusion into larger prills upon collision.
http://www.sciencemadness.org/talk/viewthread.php?tid=10575&...
Be sure to do this remote though as desribed above, molten ETN at 80 degrees C may be as much as 10 times (or even more) more sensitive than ETN at
normal temperatures, it may be similar to going crazy on NG with a stirrer bar.
[Edited on 17-11-2015 by nitro-genes]
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Microtek
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I don't think you have to be overly concerned about sensitivity as long as you add the ETN to already agitated water. As I mentioned in my other post,
NG is less sensitive to initiation than pressed TNT when it is suspended as droplets in agitated water (from Urbanski, IIRC). Dumping the energetic
into hot water and THEN beginning agitation could very well be dangerous.
I think the greatest benefit from doing this would be as a way of making mixtures such as ETN/TNT, ETN/PETN or ETN/RDX (or HMX) without running too
great a risk.
As nitrogenes suggests, you could play with surfactants and other additives (stabilizers perhaps) to the aqueous phase.
[Edited on 18-11-2015 by Microtek]
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Bert
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Close up photo of prills on graph paper or with other appropriate scale?
What is crush strength like on these...
From what I can see on a tiny screen, these grains are agglomerated "chunks" comprising a couple to a dozen or so of the small spherical prills?
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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nitro-genes
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Adding powdered ETN (with a little detergent) slowly to the hot water and waiting for the amount to melt before making a new addition may be safest
indeed. Thanks for posting that info on the sensitivity of NG/water mixtures. In my memories however, NG makes these fine dispersion mixtures with
water pretty easily with very small resulting droplet sizes. One would think that the size of the droplets may be an important factor determining
sensitivity. Like Bert suggests, it may be loosely bound aggregates, but if not, surfactants may still increase safety here, as well as improve
product.
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zeroberts
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In my case; as the water broke about 70 degrees it was removed from heat and the ETN was added.
Allow it to melt and sit on the bottom of the beaker. No stirring was applied while melting, only gentle tipping to allow the droplets to combine into
one mass.
As the temperature is approaching 61, begin stirring at a slow speed. The stir bar will kick up globs of the molten mass at slow speeds, so the
specific speed needed to be "dialed up to" gradually. I stopped adjusting once the desired size of droplets could be observed spinning around. By this
time the temperature is under 60.
I found that 57 degrees was a good time to pour cold tap water in as quickly as possible without disrupting the stirring.
Accelerated stirring immediately following addition of cold water prevents droplets from sticking together as they solidify. You can hear the
difference when the ETN becomes solid.
Filter, dry, enjoy on toast or with your favorite muffin etc...
I'm not at home with my notes or procedures so I apologize I couldn't be more informative about this process at the moment. When I do get home I'll
post a photo to provide more scale.
As for the prill composition: some are an aggregate of smaller particles but many are quite solid and rather hard. In fact, the hardness of each prill
is notably more than poured-then-cooled ETN I have worked with.
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Microtek
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| Quote: |
No stirring was applied while melting, only gentle tipping to allow the droplets to combine into one mass.
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I think that this may be quite dangerous. As nitrogenes said, the desensitizing effect of agitating in water most probably stems from the small
droplet size which makes both initiation and propagation difficult. Allowing the ETN to agglomerate on the bottom, removes these safety measures and
is probably no safer than melting it dry. It should melt while suspended so that the globule size is kept small. Whether heat is applied
before or after the ETN is added is probably not very important.
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