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Madog
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Erythritol Tetranitrate
For those who don't know, Erythritol is a new low cal sugar subsitute.
http://www.sciencemadness.org/scipics/erythritol.gif
i used the pcedure posted on E&W by AXT
33ml of H2SO4 were added to 20g KNO3, they were blended, set in a salt ice bath and allowed to cool to about 10C. 5 grams of Erythritol were added in
portions, the temp didn't rise above 15C. It was stirred alot and let sit in the ice bath for 30 minutes. the product was filtered and
recrystalized from acetone. Final yield was a very embarassing 0.8g!
argh! longer nitration time, i thought. So i did the same thing again but let it go overnight. next morning i filtered, purified, etc. yield was 8.5g
from 5g Erythritol. now thats wht im talkin' about! thats 1.7g ETN per g Erythritol.
.5g was pressed into a straw and taped to a block of wood, set to be initiated with .2g HMTD.
The block was placed on the ground, fuse lit, and a large rusty metal bucket placed on it to cover it, a chunk of cinder block was placed on the
bottom of the bucket.
the bucket was knocked over, the bottom was 40% ton off, and there was an indent in the shape f the cinder block on it.
the piece of wood, fairly hard stuff i say, dented in around 7mm or so
i plan to do more experimention, perhaps some power comparisons, fueling, etc. i'll be sure to let you guys know about anything worthy.
the pics:
http://www.sciencemadness.org/scipics/etn1.jpg
http://www.sciencemadness.org/scipics/etn2.jpg
http://www.sciencemadness.org/scipics/etn3.jpg
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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rolfiboy
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Etn syntesys
Hi Ive tryet the same metod as axt and found out that the temperature around 20 - max 25 celsius would give much larger yeilds.
Im sorry for my langue
Use Explosives as a tool and nothing else!!!
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AngelEyes
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All well and good, but has Erythritol been approved for use here in the UK? I have searched the net, and online health stores like GNC etc, but cannot
find it at all. Some have xylitol / sorbitol, but no one carries Erythritol. Are sorbitol or xylitol potential candidates for nitration?
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Nevermore
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erythritol is not available yet as sugar substitute in old europe, should be approved in this year, then will take some time till it will be
distributed, so all the other sources are non OTC at now.
Sorbitol and Xylitol are good nitration candidates, as well as mannitol, dulcitol, lactose..
each one of them has its problems and is good points but most of them are easy to nitrate!
Nevermore!
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flashpoint
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I hear from E&W, this is a powerful explosive, does it have to be detonated?....or is there another way of setting a charge off...I'm
guessing this is a secondary explosive...therefore I suppose it needs to be det to be set off...
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Nevermore
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you want to set it off?
you can hammer it, warm it very fast up to 200°C, grind it, or stuffs like that..
Nevermore!
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Madog
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its very powerful. see here.
http://www.sciencemadness.org/scipics/PETNvsETN1.jpg
http://www.sciencemadness.org/scipics/PETNvsETN2.jpg
sorry, i kept forgettingto post these. the target was a thin steel AOL CD tin that came in the mail. .5g of each explosive initiated by .2gHMTD, all
pressed in astaw in configurations as close to identical as i could do.
PETN's higher bristance is clear, the hole is cleaner, less deformation in the plate and the hole is close but apears a little bigger. there is
also 9 sections of metal protrudeing from the exit side. there are only 7 on the ETN one.
the other day i found a can of silly string in my house and i decidedto blow it up, i used an unmeasuredamount of ETN in a straw, musta been about .3g
or so. it blew a nice hole in the can, which was unused. and there was huge chunks of green silly crap all over.
Most people outgrow their pyro tendencies, we are the ones who\'s tendencies outgrew us.
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flashpoint
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damn! You should've blown the CD's up too  Anyhow...do you use
electrical ignition for the straw det's?
[Edited on 18-12-2003 by flashpoint]
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Polverone
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hey flashpoint
Your one-line response didn't add much. If you want to chat, contact members through U2U messages, instant messaging, or e-mail.
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flashpoint
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Sorry Polverone, I was just curious it he was using fuse or electrical det. I was trying to figure out what U2 was, guess that's the messenger
 Thanks.
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Bob
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So I made a batch of white powder that SHOULD be ETN. It had condensed drops of liquid in the flask of ETN after a day storage. When I dried it, it
melted earlier than the 60 degrees I expected. Is there water in it?
[Edited on 28-6-2004 by Bob]
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DiPentaErythrit
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So I made a batch of me !!!!!
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The_Davster
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Was that really worth bringing up a 4 month old thread? 
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Vikascoder
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Can anyone post the procedure of making ETN since I have no access to E&W forms please post .
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virgilius1979
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I successfully produced ETN using drain cleaner sulfuric acid (92%) - in excess and NaNO3 (NH4NO3 dissolves even better) and keeping the temperature
at about 20-22C when adding the erythritol, with careful stirring. It is than precipitated with cold water, neutralised with NaHCO3, washed again, and
recrystallized with ethanol-acetone mix (I choosed 4:1 ratio).
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Swede
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http://www.sciencemadness.org/talk/viewthread.php?tid=20638
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ManyInterests
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I've decided to necro this thread since as of writing this I have my first ETN nitration in process. I used a mixture of 22ml 68% nitric acid, 33 ml
of 96 or 98% sulfuric acid that was cooled to sub-zero temperatures and in a salt-water ice bath (it was VERY cold) and I added roughly 5.4 grams of
erythritol. I stirred it with my glass thermometer until I saw nothing but a white slurry with little to no granulation left in the solution. The
temperature never rose above 0 degrees Celsius. I believe it was still sub-zero the whole time.
I used Darian Ballard's video as a reference. He said to keep it nitrating for just 30 minutes at 10 degrees celsius, but I don't think I can get to
that level, so I will play it safe and let it continue to nitrate overnight (or a few hours at least).
But I have one question: I've seen many nitrations call for 68% or 70% nitric acid while others show that the same thing can be accomplished by adding
a nitrate salt directly to sulfuric acid works all the same, as OP did. Why is this so? I am asking because it took me quite of experimenting to
finally make a workable bit of HNO3, and probably a bit more to make good WFNA. If the nitrations that call for 68% nitric acid can be accomplished
just by adding a nitrate salt to sulfuric acid it will make things a whole lot easier.
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fredsci93
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Quote: Originally posted by ManyInterests  |
But I have one question: I've seen many nitrations call for 68% or 70% nitric acid while others show that the same thing can be accomplished by adding
a nitrate salt directly to sulfuric acid works all the same, as OP did. Why is this so? I am asking because it took me quite of experimenting to
finally make a workable bit of HNO3, and probably a bit more to make good WFNA. If the nitrations that call for 68% nitric acid can be accomplished
just by adding a nitrate salt to sulfuric acid it will make things a whole lot easier. |
Not all reactions requiring nitric acid can be substituted with a nitrate salt, ETN's synth is very viable in many conditions as it's a simple
formation of a nitrate ester, these types of reaction in general are very forgiving and either a nitrate salt or nitric acid can be used.
(nitrocellulose, Methyl nitrate, EGDN etc) However, for more complex reactions nitric acid is a must for the reaction to proceeded, I would imagine
this is either due to the sulfate salt generated reacting or hindering good mixing or in the case of AN reactive intermediates being generated (a more
complex reaction would be RDX, HMX etc). There are of course exceptions though, this is just a rough explanation/guide. There's no great way of
predicting whether a reaction will work with a nitrate salt, just experimentation.
Also, this reaction in particular gives near quantitative yields with the use of ammonium nitrate and not (azeotropic) nitric acid at room temp (the
reaction starts at -18C however it warms to 10C-15C and is kept there for 90minutes, don't leave it overnight, it fucks the yield and is totally
unnecessary), just as an aside.
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ManyInterests
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| Quote: | | Not all reactions requiring nitric acid can be substituted with a nitrate salt, ETN's synth is very viable in many conditions as it's a simple
formation of a nitrate ester, these types of reaction in general are very forgiving and either a nitrate salt or nitric acid can be used.
(nitrocellulose, Methyl nitrate, EGDN etc) However, for more complex reactions nitric acid is a must for the reaction to proceeded, I would imagine
this is either due to the sulfate salt generated reacting or hindering good mixing or in the case of AN reactive intermediates being generated (a more
complex reaction would be RDX, HMX etc). There are of course exceptions though, this is just a rough explanation/guide. There's no great way of
predicting whether a reaction will work with a nitrate salt, just experimentation. |
Duly noted. I didn't stop to think about the sulfate formation, which is something I had to learn to deal with when making nitric acid. At any rate,
the only nitrate salt I have access to is KNO3, which I got from turning calcium ammonium nitrate cold packs into potassium nitrate using potassium
chloride.
| Quote: | | Also, this reaction in particular gives near quantitative yields with the use of ammonium nitrate and not (azeotropic) nitric acid at room temp (the
reaction starts at -18C however it warms to 10C-15C and is kept there for 90minutes, don't leave it overnight, it fucks the yield and is totally
unnecessary), just as an aside. |
Well it's a bit too late since I did keep it out overnight. I was a bit too tired last night to clean it up. It does not appear to have reduced my
yield that much. But then again, I am still filtering the stuff and neutralizing the acids (you can NEVER have enough sodium carbonate/bicarbonate in
this hobby!) and washing the stuff out. Once I let it air dry for a day or so I'll see what my final yield is.
For my next attempt I will definitely try to bring the temperature up to 10C or so and not let it sit for more than 90 minutes.
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karolus28
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I have saved a method Improvised Chaos(yt) used to make etn, he said it's very high yielding. If anyone's curious they can look it up
Attachment: etn improved chaos.txt (3kB)
This file has been downloaded 803 times
Hi, please read about exif data.
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ManyInterests
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I'll definitely give it a look.
It seems like my final yield appears to be granular (crystals) instead of a fine powder. This is probably due to the fact that I used granular
erythritol instead of powder because I heard it here that it was better to use that. But then again, my product isn't dry yet, I could be mistaken.
How safe is it to crush small quantities of the stuff with a rubber spatula?
If it isn't safe, I think for my next synthesis I will grind up the granular erythritol into a fine powder before adding it to the nitrating mixture.
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katyushaslab
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Recrystallize your ETN instead of crushing it to get a different particle size. Fast recryst = small particles, slow recryst = large particles.
Saturated solution of ETN in the minimum amount of hot acetone dumped into ice water (better with stirring) will give you very, very small particles
of ETN.
This also has the benefit of being a mandatory purification step anyway.
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Fulmen
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No, granular erythritol is the right choice as fine powders tend to contain anti-caking agents.
The final grain size will be determined by the crystallization process. This should be covered in detail if you dig a bit through the forum, but IIRC
adding cold water slowly to a hot acetone-solution works well.
We're not banging rocks together here. We know how to put a man back together.
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ManyInterests
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| Quote: | No, granular erythritol is the right choice as fine powders tend to contain anti-caking agents.
The final grain size will be determined by the crystallization process. This should be covered in detail if you dig a bit through the forum, but IIRC
adding cold water slowly to a hot acetone-solution works well.
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Good thing I downloaded the video from Darian Ballard where he showed the process in great detail. As soon as my product is 100% dry I'll do a
recrystalization with acetone.
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ManyInterests
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OK I just learned a VERY important lesson here.
I'm not going to bother increasing the temperature to 10 while waiting for the ETN to finish nitrating. I had a runaway nitration today (my first and
I swear it will be my last) the room was filled with red NO2 gasses but I smelled nothing. It was very light, but the stuff in the beaker was BOILING.
I remembering the thread 'Life after detonation' that described something similar. I had no idea what happened or why there was a runaway. I wanted to
leave the whole thing for 90 minutes. For most of the nitration time it remained close to 10 c. But it just shot up without warning.
I heard a boiling sound like I was boiling water for coffee. But then I went to see what was going on and I saw that my solution turned black and it
was boiling.
I was afraid to touch it. I left my thermometer in it and it was above 100 c. I remembered that dumping it in water was the necessary solution to this
problem, but I didn't want to touch the beaker. Not with my hands or with a tong. What I did was walk past it, opened my balcony door to ventilate it.
Turned on all fans in my apartment, opened all the windows I could, then I dressed up and left. Just didn't want to be there if something happened.
When I returned the temperature had dropped to around 40 or 50 c and the boiling stopped. I put on a pair of vinyl gloves and I picked up the beaker
with a pair of tongs and I removed the plastic wrap I put on top, then I dumped it all in a glass pan full of water. Then I added more water and
started putting in sodium carbonate in order to neutralize everything. I washed out the beaker (it is intact. No sign of cracking or anything). I am
out of carbonate, but I got lots of bicarbonate, so that'll need to do for now.
I am so damn lucky. I need to make more nitric acid and I will be trying for a 3rd ETN synthesis. But this time I will do what I did the first time
and keep everything in sub-zero temperatures and as cold as humanly possible,
The only other difference between this time and the previous was that I used my magnetic stirbar for the ETN, while the last time I mixed everything
by hand with my thermometer. I stirred it for a bit over 10 minutes. I am not sure if that is enough mixing, but next time I will try for more. By
hand if need be.
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