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TheAlchemistPirate
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[*] posted on 8-5-2014 at 14:19


Hey I have questions regarding ETN too, as you might see above I'm trying to make it.
I recently bought Crown denatured alchohol, and was wondering is if anyone has crystallized ETN with it. When checking the msds I saw that it contains methanol(works for recrystallization),ethanol(works too),isopropylene(solvent), and methyl isobutyl ketone(solvent). I figure that since all those chemicals are solvents that evaporate it wont affect anything, I would like your word on it. I have seen some threads on here regarding using OTC denatured alcohol and someone said that it wont work due to contaminates, but they didn't say mention a certain brand. I'm also not sure if it would be dumb to not recrystallize this batch at all, as I will use it the next day and will properly neutralize it with water and sodium bicarbonate. I haven't found any sure answers for these questions with google.




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[*] posted on 8-5-2014 at 16:37


Yes denatured alcohol will never be pure ethanol otherwise it couldn't be sold as "denatured" it will work. At least try it. I found the "natural" one for denatured alcohol is 95% ethanol. You'd probably be OK to not recryst. if you use it the next day but storing for any amount of time recrystalize it is best, it may be more sensitive without the recrystalization as that is a purification process. My question is whether acid can or can't be trapped in the crystals? I assume it can be when it is dumped into water forming tiny crystals, but probably not when a slow recryst. is done in ethanol forming larger crystals...
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[*] posted on 8-5-2014 at 18:53


I just tried making pure erythritol crystals with Truvia sugar substitute, but it isn't crystallizing.
I used this method. http://www.sciencemadness.org/talk/viewthread.php?tid=26679
The only differences between this procedure and mine were:
1.More water used (shouldn't have mattered)
2.When the Truvia was dissolved into the water,and all throughout the process, it remained clear.
I now have a clear solution sitting in my refrigerator, and its been 3 hours. I put a Teflon stir bar in it in hopes of starting the crystallization. I will probably leave it in there until I know what's wrong.

[Edited on 9-5-2014 by TheAlchemistPirate]




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[*] posted on 8-5-2014 at 21:05


i have used denatured alcohol many times to recrystallize ETN with no problems. there are many brands available with different additives, and one cheap one i tried even smelled like some sort of petroleum based chemical was added. this particular brand i did not attempt using for ETN though. there have not been any problems that i am aware of so far and i have recrystallized the ETN by crashing a solution into iced water, also both slow and fast cooling of a ETN/alcohol solution with ice and just allowing it to get to ambient temp then cooling. the crystals were well formed crisp snow white needles. it works well but i have not used plain ethanol so i dont have a reference to see if there really is any difference. Also i am not sure if truvia is pure erythritol or not. it probably contains stevia as well too going by the name of it.



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[*] posted on 9-5-2014 at 00:06


Quote: Originally posted by TheAlchemistPirate  
I just tried making pure erythritol crystals with Truvia sugar substitute, but it isn't crystallizing.
I used this method. http://www.sciencemadness.org/talk/viewthread.php?tid=26679
The only differences between this procedure and mine were:
1.More water used (shouldn't have mattered)
2.When the Truvia was dissolved into the water,and all throughout the process, it remained clear.
I now have a clear solution sitting in my refrigerator, and its been 3 hours. I put a Teflon stir bar in it in hopes of starting the crystallization. I will probably leave it in there until I know what's wrong.

[Edited on 9-5-2014 by TheAlchemistPirate]


I think the answer to your lacking cristallisation is obviously displayed in point nr 1. If you use more water, then the solution will not become saturated and will not precipitate the excess on cooling. Simply...just reheat the solution and dissolve an additional portion of truvia to match the ratios described in the process.




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[*] posted on 9-5-2014 at 19:43


You can buy pure erythritol on eBay. Its called ritolsugar and its around $10for a 1kg bag. I have used this with great results and you can nitrate it straight from the bag. Its pure erythritol without stevia or other additives like the trivia brand and it Just needs a little grinding. No need to recrystallize or purify and it lasts ages. Not really that sweet tasting though. Its worth paying for I think. Worth looking into if ETN is your interest.



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[*] posted on 10-5-2014 at 11:30


I got it to crystallize, as markx said I used way too much water. I am going to be making etn tonight, if my crystals would freaking dry out in time lol. I wonder if acetone would help... Anyways, I'm still not sure about how to set it off. I saw it regarded as a primary on one thread, a secondary on another, and as in-between somewhere else. I might put a propane torch to a tiny amount later, just to test it.



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[*] posted on 11-5-2014 at 12:23


Quote: Originally posted by TheAlchemistPirate  
I got it to crystallize, as markx said I used way too much water. I am going to be making etn tonight, if my crystals would freaking dry out in time lol. I wonder if acetone would help... Anyways, I'm still not sure about how to set it off. I saw it regarded as a primary on one thread, a secondary on another, and as in-between somewhere else. I might put a propane torch to a tiny amount later, just to test it.


You sound eager to rush things without having a proper understanding and a clear goal...bad combination. Never rush anything when engaged in a HE synthesis or any related process (drying for example). Make sure you have everything planned and all the tools and accessories ready before starting. Discovering mid synthesis that you don't have a vital tool or vessel ready can turn things ugly very fast.
As for setting off your product do not take a torch to it....very bad practice, plus in all probability you will have a deflagration if a small amount (<10mg) is used. Then you feel tempted to use more and that's when things will turn bad. Wrapping a small amount of ETN in foil and attaching to a pyrotechnical composition (black powder or KNO3+sugar type e.g) and lighting it via a fuse to heat shock the ETN is a 50/50 probability method to get it to DDT and see the power that unfolds. Use a quality fuse and a good length of it! It just makes my neck hair rise to high heavens when I see another vid of someone setting off a monstrous charge with a 10cm piece of fuse.

Find attached an article regarding nitric esters thermal stability :

Attachment: thermal stability-nitric esters.pdf (984kB)
This file has been downloaded 721 times





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[*] posted on 11-5-2014 at 13:20


What synthesis do you guys follow for ETN?
Yes, I have U.T.F.S.E and followed the thread titled 'ETN lab synth report' twice with failure.

The problem is I am using potassium nitrate, and the mixture clumps up when left to nitrate.
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[*] posted on 11-5-2014 at 13:24


Quick question, I recently stripped a miniscule amount of gold from a couple electronics, and for lack of a better use I dissolved it in some piranha solution. (Conc. sulfuric and 30% H2O2, 3:1)

I was left with a greenish solution which was evaporated to leave a orangey, red substance. It dissolves in water and when sodium metabisulfite is added (in solution) gold precipitated.

Any idea what this orange stuff is? I was thinking chloroauric acid, but that can't be - no chlorine atoms were ever present.




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[*] posted on 11-5-2014 at 23:15


Quote: Originally posted by Manifest  
What synthesis do you guys follow for ETN?
Yes, I have U.T.F.S.E and followed the thread titled 'ETN lab synth report' twice with failure.

The problem is I am using potassium nitrate, and the mixture clumps up when left to nitrate.


What constitutes as "failure"? No product at all or just a low yield? I assume you attempted the synthesis at a rather low temperature <10C?

To use the salt+sulfuric nitrating mixture one needs a sturdy mixing aid to keep things agitated during synthesis.
Also using excess sulfuric (10-20% depending on the gravity of the clumping problem) will alleviate the problem to some extent.
As will keeping the temperature of the nitrating mix around +20C. If you cool the mix in the fridge, it will clump up before even having the chance to add any erythritol to it.
As far as my experience, the erythritol nitrations seem not to be very prone to thermal runaways, but in some case there may be contaminants that provoke it, so do not count on it not happening. Use a small batch to test the higher temp! Proceed with caution and have a quenching bath ready.
One can also dissolve the erythritol in a separate batch of extra sulfuric acid and add that in small portions to the nitrating mix to aid in uniform distribution of the reagents. The erythritol dissolving process is slow and yields a viscous liquid...it will cling to the walls of the dissolving vessel, so expect some losses due to that.
In all probability the typical expected yield will be around 50% with this route.




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[*] posted on 12-5-2014 at 23:00
Burning dissolved explosives


Would a solution simply burn if you dissolved ETN, AP, etc in an organic solent such as ethanol or acetone. I'd like to dispose of some materials in a clandestine manner, and was looking for the safest/quietest method. There would be a high ratio of solvent to solute, I don't want some sort of blasting gelatin. Would this consistently burn calmly, or would it have a tendency to explode?
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[*] posted on 13-5-2014 at 01:08


Quote: Originally posted by Nitrator  
Would a solution simply burn if you dissolved ETN, AP, etc in an organic solent such as ethanol or acetone. I'd like to dispose of some materials in a clandestine manner, and was looking for the safest/quietest method. There would be a high ratio of solvent to solute, I don't want some sort of blasting gelatin. Would this consistently burn calmly, or would it have a tendency to explode?


What do you mean? Those solvents you mentioned are already very flammable themselves.

Me and my friend tried to dissolve a concentrated solution of ADN in ethylene glycol, and the impact sensitivity was high, it could deflagrate similar to nitromethane and ethylene glycol dinitrate
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[*] posted on 13-5-2014 at 05:15


Quote: Originally posted by Nitrator  
Would a solution simply burn if you dissolved ETN, AP, etc in an organic solent such as ethanol or acetone. I'd like to dispose of some materials in a clandestine manner, and was looking for the safest/quietest method. There would be a high ratio of solvent to solute, I don't want some sort of blasting gelatin. Would this consistently burn calmly, or would it have a tendency to explode?


The more dilluted, the safest.
I once disposed of a 100g CTAP (cyclo-triacetonperoxyde) in 100 ml nitromethane...CTAP fully dissolves into it.
I stikked a very long fuse, hoping for a big explosion.
The container was Polypropylene.
After the fuse was off, nothing happened...I came closer with caution...all was gone, the container was empty and intact...no flame, no noise, no explosion.
I was astounished because CTAP usually burns yellow (rich at carbon and negative OB).

So dillution with a solvent fuel is indeed a good way to burn HE with less danger. But each case must be studied because solvent properties and explosive properties interacts sometimes dangerously.




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[*] posted on 13-5-2014 at 07:05


Quote: Originally posted by Nitrator  
Would a solution simply burn if you dissolved ETN, AP, etc in an organic solent such as ethanol or acetone. I'd like to dispose of some materials in a clandestine manner, and was looking for the safest/quietest method. There would be a high ratio of solvent to solute, I don't want some sort of blasting gelatin. Would this consistently burn calmly, or would it have a tendency to explode?


Dissolve explosive in an excess of a flammable solvent, spread evenly over/absorb into a large sheet of dry cardboard, before solvent can evaporate, light a DRY, DOWNWIND corner of the cardboard and get away.

This has been done to dispose of nitroglycerin and Erythritol tetranitrate samples safely, have not tried it with primary explosives though.




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[*] posted on 13-5-2014 at 09:07


Quote: Originally posted by markx  
Quote: Originally posted by Manifest  
What synthesis do you guys follow for ETN?
Yes, I have U.T.F.S.E and followed the thread titled 'ETN lab synth report' twice with failure.

The problem is I am using potassium nitrate, and the mixture clumps up when left to nitrate.


What constitutes as "failure"? No product at all or just a low yield? I assume you attempted the synthesis at a rather low temperature <10C?

To use the salt+sulfuric nitrating mixture one needs a sturdy mixing aid to keep things agitated during synthesis.
Also using excess sulfuric (10-20% depending on the gravity of the clumping problem) will alleviate the problem to some extent.
As will keeping the temperature of the nitrating mix around +20C. If you cool the mix in the fridge, it will clump up before even having the chance to add any erythritol to it.
As far as my experience, the erythritol nitrations seem not to be very prone to thermal runaways, but in some case there may be contaminants that provoke it, so do not count on it not happening. Use a small batch to test the higher temp! Proceed with caution and have a quenching bath ready.
One can also dissolve the erythritol in a separate batch of extra sulfuric acid and add that in small portions to the nitrating mix to aid in uniform distribution of the reagents. The erythritol dissolving process is slow and yields a viscous liquid...it will cling to the walls of the dissolving vessel, so expect some losses due to that.
In all probability the typical expected yield will be around 50% with this route.



I leave it to nitrate and am left with dried up shit, I try dissolving it in water and filtering what remains but when I burn it it is potassium nitrate and potassium sulfate.
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[*] posted on 13-5-2014 at 23:29


Most information for PETN re-crystallizing suggest that acetone is the best choice of solvent for this particular HE. i cant find anyone who has chosen to use Methyl ethyl ketone as a substitute for the acetone, so my question is can MEK be used in place of acetone without any issues? i would think that it would be OK. if anybody knows reasons why MEK can't be used then i would like to know. i did try ethyl acetate recently but the results were tiny low density needles. I was just going to try MEK as an alternative and see what sort of crystals form. i would be starting very small scale if no other information is available about it.



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[*] posted on 14-5-2014 at 00:23


Quote: Originally posted by NeonPulse  
Most information for PETN re-crystallizing suggest that acetone is the best choice of solvent for this particular HE. i cant find anyone who has chosen to use Methyl ethyl ketone as a substitute for the acetone, so my question is can MEK be used in place of acetone without any issues? i would think that it would be OK. if anybody knows reasons why MEK can't be used then i would like to know. i did try ethyl acetate recently but the results were tiny low density needles. I was just going to try MEK as an alternative and see what sort of crystals form. i would be starting very small scale if no other information is available about it.


Refer to the according section of Urbanski for information on PETN solubility in different solvents vs temperature. MEK is not discussed there, but aside from the question of PETN's solubility in it I see no problem with using it as a recristallisation medium.


PETN solubility.jpg - 102kB




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[*] posted on 14-5-2014 at 01:41


Yeah, i did see that chart and through out the section on PETN there was a heap of other interesting data but there was nothing on using MEK that i could find, neither in any of the urbanski volumes that i have. i guess that is why i thought i would ask others in the know here. as i mentioned i will start with a small batch and see how it goes.



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[*] posted on 14-5-2014 at 11:50


I have seen many topics on this site and other ones about explosive "casting" , and after looking it up I became interested and want to know how to do it. I have picked up on several things about it, but there are a few things Im not sure of such as:
What equipment do I need?
How much experience do I need to do it?
Is it too dangerous?
What situations is it necessary in?
I do know that casting is practiced in order to get as much explosive as you can into a certain area, since there are no spaces for air when it is a solid form. I also know it is used since it increases the VoD because a casted explosive is a single form and not separated by spaces, therefore shockwaves are able to travel more freely throughout the form. I also know that it can be dangerous to do because it might be heated to much, and to never try to cast a primary. I doubt that I can just use a hot plate with a water bath to heat a beaker full of say TNT, and just pour that into any form I want. Unfortunately, there doesn't seem to be any tutorials on this on the internet, at all. So please if you can, give me a link or tell me if this is too dangerous.




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[*] posted on 14-5-2014 at 12:34


I also want to find out more on the casting of explosives.
If you are going to cast ETN use nothing but a hot water bath and a plastic container for the ETN. 15g or less can be casted this way safely I suppose if the ETN is neutral and recrystalized. I suspect that large amounts of molten ETN (50g or more) would be more prone to spontaneous detonation, I don't know why this is however


An example of a use for cast explosive is pentolite boosters used for ANFO in blasting industry.

I tried making a cast of TNT (15g) by melting it under water that was heated by hotplate. It turned out OK. I did not try making a cast by melting the material dry though .

Pic:





I would comfortably heat a beaker full of TNT heated by water bath until all material is molten and pour this into a mold



Process for preparing pentolite:

http://www.google.com/patents/US2395341

[Edited on 14-5-2014 by Turner]
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[*] posted on 14-5-2014 at 13:07


I have a question! It's actually reagent acquisition but it fits energetics too.

I've been trying to find erythritol here in Brazil, with no luck. Are there any south american members that can help me with this?
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[*] posted on 14-5-2014 at 13:17


Quote: Originally posted by NexusDNA  
I have a question! It's actually reagent acquisition but it fits energetics too.

I've been trying to find erythritol here in Brazil, with no luck. Are there any south american members that can help me with this?

Erythritol is in several artificial sweeteners, I used Truvia and purified it with recrystallization. Here's a link on how to do it
http://www.sciencemadness.org/talk/viewthread.php?tid=26679
There are also some listings selling erythritol on ebay as well.




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[*] posted on 14-5-2014 at 14:07


I've only found baking blend Truvia which contains too little erythritol to be a reliable source.

The major problem is shipping edible things from other countries... they have a nasty tendency of not making it to my place (I've tried to import tea twice). :P
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[*] posted on 14-5-2014 at 22:05


Quote: Originally posted by Turner  
I also want to find out more on the casting of explosives.
If you are going to cast ETN use nothing but a hot water bath and a plastic container for the ETN. 15g or less can be casted this way safely I suppose if the ETN is neutral and recrystalized. I suspect that large amounts of molten ETN (50g or more) would be more prone to spontaneous detonation, I don't know why this is


I believe it to be a matter of probability.
ETN compared to TNT is sensitive and unstable.
Smaller the quantity ..... Smaller are the chances of running into "that" molecule
that "falls apart" during casting.
Just my theory.




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