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Author: Subject: ETN drying(or not in this case) and recrystallization ?
Thanatops1s
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[*] posted on 24-6-2013 at 14:26
ETN drying(or not in this case) and recrystallization ?


Hi, I've been experimenting with ETN and no problems with the synth and yield seems decent, but it just will not try. I had a fan on it for house and it got mostly dry. After sitting for 24 hours, it seems like it hasn't changed. Tried a small hammer test that did nothing but I'm guess because it was still wet. Putting a small bit on foil and heating it melts then deflagrates.

Also, I was wondering if anyone has ever tried recrystallizing with isopropyl? It's far easier for me to get that than EtOH or MeOH. I've found some denatured alcohol but it doesn't say what it actually is and I've read it can sometimes be isopropyl.

Any help would be much appreciated.
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golfpro
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[*] posted on 24-6-2013 at 16:26


What did you want to do with the ETN?? To dry it, scatter it out on a glass surface, you don't need it to be dry for recrystalizing, but you don't really want a big muddy soaking wet heap. After you recrystalize, back onto a flat glass surface to completely dry, or any surface.


Why did you make that?
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Thanatops1s
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[*] posted on 24-6-2013 at 17:26


I made it for the same reason as most people here. I've always had a love of chemistry and enjoy experimenting with energetic substances as a I have for about 15 years(I certainly have zero intention of hurting anyone or causing any harm). I happen to have an old abandoned quarry a short walk through the woods from my house to detonate them as well.

I haven't actually recrystallized yet, because I'm not sure what to use. The best ethanol I can acquire is 70% and I figured wasn't good enough. If it is, then problem solved.
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gnitseretni
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[*] posted on 24-6-2013 at 19:17


Sounds like you have residual acid in your ETN. Wash it thoroughly to get rid of the acid before you recrystallize it.
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golfpro
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[*] posted on 24-6-2013 at 20:24


I rinsed very well with water a few times and then a lot of weak sodium bicarb solution. The rinse again with water, then let this dry somewhat so it's not mud. I used 92% Ethanol, brought it too 55* C in a hot salt water bath, then dissolved it, set this in a freezer until it was -10 and all was precipitated out, then filtered and rinsed with water, then completely dry it out.

If you have a Home Depot near you, you can get higher % Ethanol. Some liqour is so high conc. alcohol it can be used for recrystalizing.


How were you going to detonate this? And how much?
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Ral123
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[*] posted on 25-6-2013 at 02:15


That product you have is dangerous with all these acids. Putting it on glass and hitting it with something hard is very likely to cause a very bad accident. Drying is done in dark place on let's say plastic surface with a small fan. Sun is very bad for almost all energetics, except may be ANFO and UN.
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Thanatops1s
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[*] posted on 25-6-2013 at 07:44


Quote: Originally posted by Ral123  
That product you have is dangerous with all these acids. Putting it on glass and hitting it with something hard is very likely to cause a very bad accident. Drying is done in dark place on let's say plastic surface with a small fan. Sun is very bad for almost all energetics, except may be ANFO and UN.

I'm not sure where you're getting this from, I didn't say anything about sun, or hitting anything on glass(I'm not an idiot). The tiny hammer test I did was wrapped in a little foil and done outdoors on a brick.

I'll have to check out Home Depot for better EtOH. I'm pretty much positive it's acid free. I washed it numerous times with a sodium bicarbonate solution. When it ceased bubbling I gave it another couple washes to be sure. Then rinsed it many more times with just plain distilled water. So I wouldn't think acid is the issue.

I must say though that this morning I noticed an improvement. Its still moist though. The high humidity definitely doesn't help either so maybe it just needs more time.

Would putting it in a contained with a desiccant of some sort maybe help?

As far as detonation, right now I planned to use 200mg of HMTD to initiate 2g of ETN. I would like to synth some silver acetylide also, the only reason I haven't yet is lack of precursors.

Any alternate suggestions for initiation are welcome.
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Motherload
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[*] posted on 25-6-2013 at 10:17


The crude product is a fine powder and holds more water
My recrystalized product always drys much faster.
As long as its acid free .... It will dry. Mine takes about 3 days to be free flowing crude product.




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Ral123
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[*] posted on 25-6-2013 at 10:28


Quote: Originally posted by Thanatops1s  
Quote: Originally posted by Ral123  
That product you have is dangerous with all these acids. Putting it on glass and hitting it with something hard is very likely to cause a very bad accident. Drying is done in dark place on let's say plastic surface with a small fan. Sun is very bad for almost all energetics, except may be ANFO and UN.

I'm not sure where you're getting this from, I didn't say anything about sun, or hitting anything on glass(I'm not an idiot). The tiny hammer test I did was wrapped in a little foil and done outdoors on a brick.

I'll have to check out Home Depot for better EtOH. I'm pretty much positive it's acid free. I washed it numerous times with a sodium bicarbonate solution. When it ceased bubbling I gave it another couple washes to be sure. Then rinsed it many more times with just plain distilled water. So I wouldn't think acid is the issue.

I must say though that this morning I noticed an improvement. Its still moist though. The high humidity definitely doesn't help either so maybe it just needs more time.

Would putting it in a contained with a desiccant of some sort maybe help?

As far as detonation, right now I planned to use 200mg of HMTD to initiate 2g of ETN. I would like to synth some silver acetylide also, the only reason I haven't yet is lack of precursors.

Any alternate suggestions for initiation are welcome.

Well, I've read some books and ETN has the sensitivity similar to NG, established around 1900'th year. Impure NG can explode that easily: http://www.youtube.com/watch?v=7SvW_P0safI
So while you dry your impure ETN in a dish for example, if it's hit by another for example ceramic object, quite a thing may happen.
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Thanatops1s
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[*] posted on 25-6-2013 at 10:34


In regards to my other question, if I am unable to find more than 70% EtOH, will ispropyl work?
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Motherload
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[*] posted on 25-6-2013 at 12:47


Methanol aka methyl hydrate at Home Depot works for sure.
Iso-Propanol will probably work as well although you may have yo use more of it.




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[*] posted on 25-6-2013 at 13:24


Quote: Originally posted by Thanatops1s  
In regards to my other question, if I am unable to find more than 70% EtOH, will isopropyl work?


≥95% EtOH works the best, MeOH works as long as it is lab grade not fuel grade and I have never tried iPrOH.

Is there a reason you cannot distill your own EtOH? There is no need for expensive glassware, you can use pretty much any macgyvered distillery device, or buy 3A molecular sieves as they are reusable as well.




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[*] posted on 25-6-2013 at 14:43


well yes ofcourse you can get it.. you can get ''Methylated spirits'' pretty much anywhere, its usually approx 90% EtOH and containing methanol, sometimes also isopropyl and some other liquids, the reason this tastes so horrific is because they fill in denatonium benzoate which is a solid, so if you care you can distill it away, as in the ethanol can be distilled off
still theres methanol in more than most likely so dont drink it

this works well for recrystallization also..

anyways since you cooled the whole thing to -10*C.. do you know what the solubility of ETN is?? im curious to see if this could have a major effect on the yields..

also for exotic initiation.. yes yes yes.. there most definately is..

if you manage to shockheat it (MP 61*C IIRC) meaning as heating it with great power much past its melting point then you will achieve a full detonation
this can be done with sparklers if you care to try it
thin layers of ETN can be packed in al foil (0.5g to a whole A4 sized piece of al foil, added in thin layers, then folded down and again added to al foil)
this can then be wrapped around the sparklers (3 sparklers?)
and more than likely you will get some interesting results..
rocket candy pieces can be used aswell, say pack them in straws of a decent size, approx. 0.5 cm wide and make a hole in it so you can insert a fuse plus something from fuse to rocket candy to make sure it works

one thing you might do wrong is that the fuse runs along the rocket candy, and the fuse will actually make the ETN pop around tearing the whole thing apart making some quite uninteresting stuff happen...




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https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 25-6-2013 at 19:38


If you were to use a .2g HMTD cap in a straw or something, how would you meet the critical diameter of .5cm? I was wondering this, because looking at 2 grams, that is hardly anything at all, I couldn't think you could have a straw in the middle of pressed 2 grams etn in a tube with .5cm of material in order to detonate???

I don't know about heatshock detonation, if you use too much etn in the cap like more than .1 gram, it won't heat fast enough, and it has to be a thin slice in contact with the hotness in order to go off.

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[*] posted on 25-6-2013 at 19:42


Pressed ETN has very little critical diameter. It detonates in a straw with no difficulty. The bigger problem is to make the HMTD to detonate in a straw. If it does, the whole thing will be well set off. I've never understood how can sub gram organic peroxide be used reliably.
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[*] posted on 25-6-2013 at 20:17


I thought any primary confined would detonate at any amount. I have used tiny little 1cm long tubes w/ fuse and pressed hmtd, no more than .05g, this detonates, it makes a little pop.



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[*] posted on 25-6-2013 at 20:30


I can barely call a straw a confinement. Also I prefer to leave the primary detonate 1-2cm, to gather velocity when it reaches the secondary. Also I warp foil around the straw(before stuffing with primary) to add inrtial confinement:
http://www.youtube.com/watch?v=J2qLkvcaWds
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Thanatops1s
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[*] posted on 26-6-2013 at 17:23


Quote: Originally posted by Ral123  
Pressed ETN has very little critical diameter. It detonates in a straw with no difficulty. The bigger problem is to make the HMTD to detonate in a straw. If it does, the whole thing will be well set off. I've never understood how can sub gram organic peroxide be used reliably.

I have made HMTD detonators that work quite well. I've used them many times on their own and only once did it deflagrate. I realize it's a very unorthodox design, but they are a cube made of cardboard from an empty cigarette pack and packing tape. My design for this is one of those embedded in the center of a larger cube with the ETN between the inner and outer cube. Based on the size, it looks like it's actually going to be about 3.5-4g of ETN when it gets filled.

Also, I've never detonated anything in a bucket of sand before and was wondering if that does much for reducing SPL? Just wondering if I could be closer to civilization doing it that way.

[Edited on 27-6-2013 by Thanatops1s]
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golfpro
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[*] posted on 26-6-2013 at 18:02


Would you dare detonate 3grams etn on the street?
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[*] posted on 27-6-2013 at 08:23


Testing detonators in a bucket of sand works pretty well, muffles the sounds down to a pop but 3.5-4g of ETN will most likely destroy the bucket and make a lot of noise. You should know that explosives should never be tested in public areas, you can't account for everything; kids, pets, peering neighbors...



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[*] posted on 27-6-2013 at 08:28


Three day's ago it was the nationnal day where I live, even if I don't like this day, it gave me a good oportunity to test to noise made by energetic. I used 0.3g HMTD (all what I had made) and 0.03g Silver acetylide (all what I had made). I live in a semi-rural area. The sound was extremly loud, even with hand on my ears and 50 feet away it was loud. The frensh workbook (1.25inch thick) was destroyed in many pieces. I do not even want to know what 3.5g on a street would do.

It was my energetic experiment for the year. Playing with these stuff is very near stupid.




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Ral123
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[*] posted on 27-6-2013 at 09:02


Fellows watching is often the most dangerous thing. They tend to have their own safety standards and not back off, even after you've lit the fuse.
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Thanatops1s
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[*] posted on 27-6-2013 at 17:37


Quote: Originally posted by golfpro  
Would you dare detonate 3grams etn on the street?

On the street, absolutely not. I just mean a little closer than I would otherwise. I detonated .8g HMTD a couple weeks ago and I was standing about 20 meters away and it was still very loud. I realize how loud this is going to be. I think what's most likely going to happen is I'm going to bury is 10-15mm underground while still being well away from people and buildings.
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