Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1    3
Author: Subject: Erythritol Tetranitrate
Madog
Hazard to Others
***




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 15-11-2003 at 11:45
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.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
rolfiboy
Harmless
*




Posts: 1
Registered: 16-12-2003
Member Is Offline

Mood: No Mood

[*] posted on 16-12-2003 at 02:45
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!!!
View user's profile View All Posts By User
AngelEyes
Hazard to Others
***




Posts: 183
Registered: 24-1-2003
Location: South of England
Member Is Offline

Mood: Skint

[*] posted on 16-12-2003 at 05:59


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?
View user's profile View All Posts By User
Nevermore
Hazard to Others
***




Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline

Mood: shopping businessman

[*] posted on 16-12-2003 at 09:19


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!
View user's profile View All Posts By User
flashpoint
Harmless
*




Posts: 16
Registered: 16-12-2003
Location: USA
Member Is Offline

Mood: No Mood

[*] posted on 16-12-2003 at 22:40


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...
View user's profile View All Posts By User
Nevermore
Hazard to Others
***




Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline

Mood: shopping businessman

[*] posted on 17-12-2003 at 12:27


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!
View user's profile View All Posts By User
Madog
Hazard to Others
***




Posts: 221
Registered: 20-5-2002
Location: USA
Member Is Offline

Mood: lysergic

[*] posted on 17-12-2003 at 14:08


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.
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
flashpoint
Harmless
*




Posts: 16
Registered: 16-12-2003
Location: USA
Member Is Offline

Mood: No Mood

[*] posted on 17-12-2003 at 19:06


damn! You should've blown the CD's up too :D Anyhow...do you use electrical ignition for the straw det's?

[Edited on 18-12-2003 by flashpoint]
View user's profile View All Posts By User
Polverone
Now celebrating 18 years of madness
*********




Posts: 3164
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline

Mood: Waiting for spring

[*] posted on 17-12-2003 at 21:14
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.
View user's profile Visit user's homepage View All Posts By User
flashpoint
Harmless
*




Posts: 16
Registered: 16-12-2003
Location: USA
Member Is Offline

Mood: No Mood

[*] posted on 18-12-2003 at 09:19


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.
View user's profile View All Posts By User
Bob
Harmless
*




Posts: 3
Registered: 28-10-2003
Member Is Offline

Mood: No Mood

[*] posted on 28-6-2004 at 12:39


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]
View user's profile View All Posts By User
DiPentaErythrit
Harmless
*




Posts: 1
Registered: 29-10-2004
Member Is Offline

Mood: No Mood

cool.gif posted on 29-10-2004 at 11:14


So I made a batch of me !!!!!
View user's profile View All Posts By User
The_Davster
A pnictogen
*******




Posts: 2861
Registered: 18-11-2003
Member Is Offline

Mood: .

[*] posted on 29-10-2004 at 13:43


Was that really worth bringing up a 4 month old thread? :mad:



View user's profile View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 19-11-2012 at 08:41


Can anyone post the procedure of making ETN since I have no access to E&W forms please post .
View user's profile View All Posts By User
virgilius1979
Harmless
*




Posts: 37
Registered: 30-9-2011
Member Is Offline

Mood: curious

[*] posted on 19-11-2012 at 11:39


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).
View user's profile View All Posts By User
Swede
National Hazard
****




Posts: 491
Registered: 4-9-2008
Member Is Offline

Mood: No Mood

[*] posted on 19-11-2012 at 12:39


http://www.sciencemadness.org/talk/viewthread.php?tid=20638
View user's profile Visit user's homepage View All Posts By User
ManyInterests
National Hazard
****




Posts: 379
Registered: 19-5-2019
Member Is Offline


[*] posted on 10-11-2021 at 20:17


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.
View user's profile View All Posts By User
fredsci93
Hazard to Self
**




Posts: 84
Registered: 29-12-2017
Member Is Offline

Mood: No Mood

[*] posted on 11-11-2021 at 01:54


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.
View user's profile View All Posts By User
ManyInterests
National Hazard
****




Posts: 379
Registered: 19-5-2019
Member Is Offline


[*] posted on 11-11-2021 at 09:47


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.
View user's profile View All Posts By User
karolus28
Harmless
*




Posts: 37
Registered: 14-4-2019
Location: EU's Brazil
Member Is Offline

Mood: zgrzyt

[*] posted on 11-11-2021 at 11:16


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 200 times




Hi, please read about exif data.
View user's profile View All Posts By User
ManyInterests
National Hazard
****




Posts: 379
Registered: 19-5-2019
Member Is Offline


[*] posted on 11-11-2021 at 11:37


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.
View user's profile View All Posts By User
katyushaslab
Hazard to Self
**




Posts: 81
Registered: 19-1-2021
Member Is Offline

Mood: precipitating

[*] posted on 11-11-2021 at 11:51


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.
View user's profile View All Posts By User
Fulmen
International Hazard
*****




Posts: 1576
Registered: 24-9-2005
Member Is Offline

Mood: Bored

[*] posted on 11-11-2021 at 12:03


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.
View user's profile View All Posts By User
ManyInterests
National Hazard
****




Posts: 379
Registered: 19-5-2019
Member Is Offline


[*] posted on 11-11-2021 at 15:44


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.


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.
View user's profile View All Posts By User
ManyInterests
National Hazard
****




Posts: 379
Registered: 19-5-2019
Member Is Offline


[*] posted on 13-11-2021 at 20:01


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.
View user's profile View All Posts By User
 Pages:  1    3

  Go To Top