Erythritol Tetranitrate [Archive] - The Explosives and Weapons Forum

Axt

September 24th, 2003, 10:58 PM

<CENTER>ERYTHRITOL TETRANITRATE</CENTER>
<center><table border=1><tr><td colspan="2"><center>Properties</center></td><tr><td>Formula</td>
<td>C4H6N4O12</td></tr><tr><td>VOD</td><td>7650*</td></tr><tr><td>Density</td><td>1.6</td></tr><tr><td>%OB</td><td>+5.4</td></tr><tr><td>Gas vol.</td><td>704cc</td></tr><tr><td>Energy</td><td>6439 </td></tr><tr><td>Impact</td><td>2,0Nm</td></tr><tr><td>MP</td><td>61°C</td></tr><tr><td>deflagr.p.</td><td>160°C</td></tr></table></center>

*extrapolated VOD from other nitric esters by Philou, most other figures were given by 'maniak' here.

Its only made passing mention in other threads so this can be its "official thread".

Synthesis via KNO3
60g KNO3 is added to 100ml 95% H2SO4 and cooled to 10°C. 15g Erythritol is added in portions, letting temperature jump between 10-20°C with each addition. Mix is left for 15min after last addition.

The mix, now thick with crystals is poured into 2 litres water, a very fine precipitate will form and float to the bottom. The solution is filtered and added to a further 2 litres of bicarbonate (baking soda) / water solution, filtered again. This is repeated again with water and filtered.

Final yield is about 1.6-1.7g ETN per 1g erythritol, or about 65-70% efficient.

Chemicals (http://rogue.altlist.com/images/etnchems.jpg)
Synthesis (http://rogue.altlist.com/images/etnsynth.jpg)

Ive uploaded an ETN detonation to <a href="http://geocities.com/roguemovies2/">here</a>, about 1/2 film canister lightly compressed, sorry there is no real target but be assured that its quite powerful stuff. Its an interesting explosive that hardly any information is available for. Due to its very fine precipitate, positive OB and sensitivity it should work well as a plastic with something like vaseline.

nbk2000

September 25th, 2003, 04:26 AM

I found a supplier (Newbies, don't ask, SEARCH!) for erythritol for $9/pound and only $5 for shipping, regardless of order size. :)

450 grams x 1.6 = 720+ grams of ETN

At 450/15=30, we'd need 4 pounds of KNO3 (or NHNO3 proportional) and a gallon of sulphuric drain cleaner to convert the pound of E to 1.6 pounds of ETN.

$10 E
$1 Nitrate (AN at $0.2/pound per 50 pound bag)
$20 Sulphuric acid

Adds up to about $20 per pound of EN. Not bad considering how it's a solid with a high VOD and possibly castable. :)

Now if there was some easy way of converting erythritol to pentaerythritol, we'd really be rolling. ;)

Axt

September 25th, 2003, 09:26 PM

Another movie added (http://geocities.com/roguemovies2/).

This charge was about the same size, but taped to a 2" thick hardwood plank, a piece of 1"x2" RHS was also leaned over the charge.

Nothing pretty about the explosions (too much O2), but the results speak for themselves.

<img src="http://ww1.altlist.com/~52497/rogue.altlist.com/images/2x1rhs.jpg">

WTF

September 26th, 2003, 01:00 AM

that's funny that a health food can be used to make an explosive.:) While I was trawling the web to see if it is available in canada I found a bunch of toxicity reports on erythritol, and I think it's hilarious that they overlooked the fact that if it was legalized, it gave people like us access to yet another easly made explosive (though it has yet to be allowed to be sold in canada)

nitric63

September 28th, 2003, 11:02 PM

I've been somewhat curious about ETN myself after hearing of it in a thread on the sciencemadness forum about melting ETN and casting the molten ETN with PETN. Another thing about ETN that seems good is that the positive oxygen balance should be easy to make use of by just adding Al or Mg powder. With NG on the other hand you can't just add powdered metal to it because it would increase it's sensitivity and the metal powder would sink in it anyway. I've looked into erythritol and it seems to be quite new as a low calorie sweetener that is used in some diet foods like candy bars but will likely have to be ordered if you want pure erythritol. I'd expect that it will be carried by healthfood stores and maybe supermarkets within a couple years though.

blindreeper

September 30th, 2003, 03:08 AM

I don't consider myself as a newbie and I did search for erythritol. I am in Australia like Axt so I know it's available. I found this info

Erythritol
Natural sweetener based upon glucose with a caloric value close to zero. Derived in bulk from a fermentation process, it also occurs naturally in many fruits and vegetables. It has properties similar to sucrose with around 70% of its sweetness. Clinical studies have shown it to have no effect on blood glucose and insulin levels.

I am not asking for the source of it because thats spoon feeding which I am strongly against. So would any of you be able to point me in the direction of where to get it? Example would it be likely to be sold in a chemist/pharmacy? If i asked for it would I get a weird look?

Axt - how much did you pay for your erythritol so I know if I am getting ripped off? I sent you an email regarding this so if you get it please add me to msn if you have it.

EDIT: Disregard all of the above because I found a supplier with $5 shipping and $9/pound (same as nbk's I think) and the picture of the Erythritol on their site is exactly the same package as the one on Axt's image.

nbk2000

October 2nd, 2003, 03:51 AM

There's a plastic explosive mentioned in COPAE that's an 80/20 mix of PETN/NG. I wonder if ETN is useable in this formulation, in place of PETN.

If so, that's be a hell of an explosive I'd think, with everything available OTC, very cheaply, and with no complicated chemistry required. :) Oh, it's a moldable plastic with an 8,000 m/s VOD. :D

Blindreeper, the prices may be the same, but I doubt it was the same supplier as the one I found, since mine only services the US.

Axt

October 2nd, 2003, 05:12 AM

The problem there is the %OB's, PETN being O-deficient can make use of the free O in NG, while ETN is even more O positive then NG!. It would be a powerful mix, but its energy would be the average of the components used rather then being enhanced.

For an energetic plastisiser you could use 87:10:3 ETN:NM:NC Its OB will be zero and more user friendly then NG based comps.

blindreeper: I believe its $25US shipping to Australia!, my email doesnt work anymore (nor do I have msn).

blindreeper

October 2nd, 2003, 09:39 PM

$25 US? Thats a fair bit. $25 x 1.6 = $40 AU Then $9 US x 1.6 = 14.4.

Thats around $55 AU for a pound erythritol :eek: Did you pay that much Axt?

Axt

October 3rd, 2003, 01:30 AM

Yeh, something like that. Shipping is cheaper per pound the more you order. Mine was from the US, but I havnt even tried to source it locally so you might be able to just walk into the health food store and buy some / order some, I dont know.

For a home hobbyist price doesnt matter much anyway, its not like we are going to make up 50 pound and take out a government building now are we?

Charlie Workman

October 3rd, 2003, 02:15 PM

What would the ratio for AN be? I have access to a lot of this, but no KNO3. This is the first new really useful HE I've seen in a while. Gets my blood flowing. Did a web search but did not find much of use on it that hasn't already been covered here. Any hard data on reactivity, sensitivity, etc? Oh, by the way, check out United States Patent Application 0030173008. It covers a reformulation of C-4. I didn't think it worth a thread of it's own, but wanted to pass it along.
--------------------------------------------------------------------------------------------------------
"To paraphrase Aristotle, life is a gas!"
-Gidget

knowledgehungry

October 3rd, 2003, 03:46 PM

I'm sorry but I don't quite understand the chemical formula for ETN. C4H6N4O12 doesnt seem to work unless it looks something like this:
*O*O--O*O
./*\/***\/*\
O--N***N--O
***\**/
***H*H
***|**|
*H-C--C--H
***|**|
***C=C
***|**|
***H*H
***/***\
O--N***N--O
.\*/\***/\*/
*O*O--O*O

The H has a 2 bonds because the N donates a pair of elecrons to it, it really doesnt seem quite right though which is why im confused because i can find no other arrangement for this compound. Any help is appreciated. ***** are space fillers.

nitric63

October 3rd, 2003, 04:12 PM

Erythritol Tetranitrate is a really simple compound to figure out. It's very similar in structure to nitroglycerin except it has a long chain and the nitrate groups of ETN alternate sides. An alternate name for erythritol is butanetetraol, which is the next polyol up from propantriol which is a chemically accurate name for glycerol. Anyway this is the structure of ETN:

*****NO2***NO2
******O**H**O***H
******!***!***!***!
***H--C----C---C---C--H
******!***!***!***!
******H**O***H**O
********NO2**** NO2

knowledgehungry

October 3rd, 2003, 11:17 PM

Haha made things too complicated. Didnt think of CONO2 as possible structure.

ALENGOSVIG1

October 4th, 2003, 05:26 PM

This looks very interesting. Someone who isnt me has ordered some erythritol and is looking forward to trying this stuff out in the coming weeks.

I bet a cast of HDN/erythritol tetranitrate would work nicely.

Axt

October 4th, 2003, 11:13 PM

Originally posted by Charlie Workman
What would the ratio for AN be?

Should be same as whats been given for KNO3, which gives excess nitrate assuming you want to make most use of the erythritol.

While the quantities Ive given should work well, the time of the reaction, weight of portions added etc. will have to be worked out for your particular setup, as it will vary greatly with your method of cooling, its efficency etc. Ive left it for an hour with no decrease in yield so dont stringently stick to the times ive given. Make sure its stired every 5 mins or it will solidify.

HDN is very oxygen poor, you would need 14:1 ETN:HDN for 0%OB and its melting point is over ETN's deflag. point. so you would likely lose performance as I dont think it will be mixed intimately enough if cast.

grendel23

October 13th, 2003, 08:19 AM

I had a chance to nitrate some of my newly purchased erythritol a few days ago. The nitration went well, the only problem is that I broke a good thermometer trying to stir the nitration mix when it became very thick. I hate that about using KNO3, next time I will use NH4NO3.

I ended with 25.8g of ETN, nicely in line with Axt's reported yield. My product is somewhat clumpy and not as nice a powder as my PETN, the particle size seems nice and small though. I am going to put it in a desiccator for a day and see if it powders any better when totally dry.

Has anyone recrystalized ETN and compared mass before and after?
I am curious as to the purity of the crude product, and also would like to add a bit of base while it is dissolved to eliminate any trace of acid. The only reason I hesitate is the product of a recrystalization is much larger crystals.

I am going to try to plasticize some ETN with EGDN, I will post my results.

mongo blongo

October 13th, 2003, 01:37 PM

Anyone tried casting it yet?

Jumala

October 14th, 2003, 09:23 PM

Last days I read in my Naoum book the following line
"The method given by Nobel for the preparation of concentrated mixed acids by dissolving saltpeter in sulphuric acid and separating the acid sulphate was little used because of its inconvenience."

This means the separation must be possible somehow.
May it be inconvenient but it would help to prevent the thick syrupy nitration mix.
Befor I waste my acid in useless tests I want to ask if someone knows how the separation can be done.
My only idea is cooling the acid/nitrate mix for some days and wait if the sulphate forms crystals.

ALENGOSVIG1

October 17th, 2003, 03:56 AM

Today i dreamed of preparing some ETN using the KNO3/H2SO4 method, but i got a tan/beige precipitate. After dissolving it in acetone, filtering out the brown nasties, and adding water to precipitate the ETN i ended up with 21g of clear colourless crystals of ETN.

I'd like to dream of using HNO3 next time though. I hate stirring thick nitrating mixtures. I like to swirl. :)

derkaiser

October 17th, 2003, 08:39 AM

Do you think of trying to cast it?? Benny

Jumala

October 17th, 2003, 10:49 PM

What is the name of a chain polyol with 5 C atoms?

I know the polyols with 6 C atoms are the derivates sorbitol, mannitol, dulcit.

nitric63

October 18th, 2003, 12:13 AM

A five carbon chain polyol with five hydroxyls would be properly called pentanepentol however it seems to be better known as arabitol. In my brief google search I saw no mention of it having any common use so I doubt you'd be able to get any very easily however my search was pretty brief so you might have more luck.

Axt

October 18th, 2003, 12:13 AM

Xylitol is a 5 five carbon polyol.

Alen~ Mine comes out beige also, our H2SO4 is the same colour - black. But when recrystalised I always recieve significantly larger crystals then what I started with, did you find this also? and what was the weight of the brown crud filtered out.

ALENGOSVIG1

October 18th, 2003, 03:39 AM

Yes i find the crystals are much larger when recrystallized from acetone. I didnt weigh the brown shit but it looked like atleast a gram.

Today i dreamed of using Ca(NO3)2/H2SO4 to prepare ETN. The nitrating mix was much thinner, and i was able to swirl the mixture easily. The resulting precipitate was not beige, but clear and colourless. I suspect the brown crud was un-nitrated or partially nitrated erythritol. I then ran the same 100 ml of acetone through the filter cake of ETN/CaSO4 while sirring it gently 4 times to extract the ETN from the CaSO4. I washed the cake with another 25 ml of fresh acetone and poured all the acetone into a bunch of water while stirring to precipitate the ETN. This time the yeild was 26g. Im guessing the yeild was better becuase the nitrating mix was less viscous and was easier to mix.

grendel23

October 18th, 2003, 04:32 AM

After about a week, my ETN started to smell like NO2. I had neutralized it with bicarb, but there must have been some acid left anyway.I decided to recrystalize it.

I recrystalized from acetone and crashed it with ice cold water, rapidly stirred. While the ETN was dissolved in the acetone, I added a little bicarb to improve stability. The crystals I have are larger than I started with, but not the millimeter scale ones I have read about.

I then added 2g EGDN to 8G of ETN and was rewarded with a very nice plastic mass. I did have some EGDN seeping out of the ETN, so 20% is more than enough to fill the voids between the grains. Next time I will try 15% EGDN and see if I can eliminate the exudation. The EGDN does not appear to have dissolved in the ETN or vice versa. I wonder if I add a little acetone I can get a homogenous mass? Even as is, this stuff looks nice, good performance and good density without pressing the hell out of it. I may have to try a small SC.

ALENGOSVIG1

October 18th, 2003, 04:36 PM

I just got back from dreaming about detonating a film canister containing 38g of well pressed ETN. The charge was taped to a length of 3/8" dia. rebar and was detonated with 1g AP.

The charge detonated with a very sharp boom and upon inspection i found the rebar had been cleanly severed. :) :D

ALENGOSVIG1

October 20th, 2003, 02:33 AM

I dreamed of attempting a 3x scale reaction today using Ca(NO3)2/H2SO4 but i only got 45g of ETN. Strange. Perhaps I should have let it react longer or something. I'll have to do some more experementation.

I also tried the HNO3 method. 8g of erythritol was dissolved in 50g H2SO4, and was added to 55g HNO3 while keeping temp between 40 and 60. Did the usual wash/recrystallization and im waiting for it to dry. It's probably only 10 or 15g although i may be wrong. So the nitrate/sulphuric is more economic.

Jumala

October 20th, 2003, 08:50 PM

Thanks,
arabitol was the name I needed. In merck´s katalogue it has also the name adonitol.
All these higher polyols seem to have no use as explosive perhaps with the exception of mannitol.
In Urbanski II he stated that erythritoltetranitrate has the same stability and sensitivity like NG.
This means it is more sensitive as PETN.
So be careful with pressing ETN.

ALENGOSVIG1

October 20th, 2003, 08:56 PM

I had to strike ETN quite hard with a hammer to get it to detonate. It was much less sensitive than NG IMO. Perhaps the the ETN that was tested in the literature wasnt recrystallized/recently prepared.

Unknown

October 21st, 2003, 03:30 AM

There is a section on ETN in "The preparatory manual of explosives", by Jared Ledgard. The ETN is prepared by using 110g/98% H2SO4, 20g/Erythritol, 140g/HNO3, 200Ml/10% Sodium carbonate solution for neutralization, and 1000Ml/95% Ethanol.
SWIM tried this method without success. The figures on ETN that this book has are as follows:
Molecular weight - 302.108, VOD - "Similar to PETN", Sensitivity - Moderate, Stability - Good, Flammability - "May flash when ignited", Toxicity - Moderate, Melting point - 61celsius, Soluble in alchohol, ether and glycerol.
The author then goes on to say that ETN is used as a substitute for :PETN "in blasting cords, for use in explosive compositions, and Nitroglycerin free dynamites when mixed with TNT. NC, or Ammonium nitrate.
I hope that this information is helpful to you, and if you want me to post his procedure let me know. I didn't include it because it is similar to the procedure Axt posted except for the addition of the E/H2SO4 solution to the HNO3.

**** It was mentioned that while adding Erythritol to the H2SO4, to keep the temp. below 40 celsius because carbonization will begin. (SWIM found this out the hard way!)

Rhadon

October 21st, 2003, 02:27 PM

There is a section on ETN in "The preparatory manual of explosives", ...
Do you possess that book? If so, do you also possess a scanner ;)? Your answer won't bring any commitments with it :).

Unknown

October 22nd, 2003, 01:27 AM

Yes, I have the book, but I don't have a scanner. I have a digital camera and tried to take some pictures with it, but the writings was illegible. I will try to get the pages(2) copied and on disk somehow and try to create a briefcase in yahoo, then I will post the link here. Sorry, I know it is a teaser to tell you I have the book and not post the pages, but if you have any questions at all about the procedures or whatever, I will post them for you. Hopefully it won' t take me long to get them copied and uploaded.

Rhadon

October 22nd, 2003, 11:25 AM

No hurry. I'm not particularly interested in these two pages but in the whole book, so don't rush things.

Your digital camera doesn't allow you to take close-ups?

Unknown

October 22nd, 2003, 07:02 PM

My digital camera does zoom. In order to zoom enough for the words to be ledgible, you can only focus on a couple of sentences at a time. It would take a long time to do the whole book that way. I am working on getting a combo fax/copier/scanner right now, then I will scan the whole thing for you. Until I get one, there is no way for me to upload anything.

Rhadon

October 22nd, 2003, 09:50 PM

Sounds great :D!

FrankRizzo

October 22nd, 2003, 10:42 PM

UNKNOWN: Does your digital camera have a macro setting (icon looks like a flower)? If so, that's what you want to use when taking pictures closer than ~21" of the lens (depends on mfg.). Also, pressing the shutter button down halfway before making the shot will actvate the autofocus feature of most cameras and make the image much sharper. Just food for though...if you already knew this, just ignore me :)

Unknown

October 23rd, 2003, 12:19 AM

My camera has a macro setting, but the problem is gettng the width of the page to fit in the photo. In order to fit the page width wise, you have to zoom out, and by that point, the words are not ledgible. So if I were to take the pictures from the distance that you could read the words, then the pictures would have to be assembled like a collage to be able to read them.

Chemical_burn

October 23rd, 2003, 12:59 AM

How many megapixels does your cam have? It sounds like you cam sucks. No offence but why dont you get a new one you can get a decent 2 megapixel cam for less than $100 USD nothing great but would work for this. Also you could probably get a webcam with good enough resolution for less than $50 USD. I had an old Logitech webcam that took prety good still frame pics and if it still worked I would make a planitary cam out of it. It was a decent cam had a nice snap shot button on the top just press it and it open the software that came with it and took a still frame pic so it would make a decent planitary cam. Just set it up and focus it on the pages you want a pic of and press the image capture button and turn page and repeat as nessary.

Unknown

October 23rd, 2003, 01:17 AM

My camera is 2.2 megapixels, but the problem is that the writing in the book is small font, so you have to zoom in really close to read it. It doesn' t matter though, tomorrow (western US time) I am going to get a cheap flatbead scanner. I will then be able to scan the whole thing. The only other alternative is to go make copies someplace, and concidering the legal and political climate these days, it would go over like a fart in church!

ALENGOSVIG1

October 25th, 2003, 05:30 PM

Just weighed the final yeild of ETN from the HNO3 method and i only got 15g. :(

On another note i just got back from dreaming of detonating 44g ETN. I strapped the charge to a 1/4" thick piece of aluminum sheet and blew a 6" hole through it! :D

blindreeper

October 25th, 2003, 07:36 PM

I have found blowing holes through metals is extremely hard. I had some 3mm lead sheeting and 35g of APPN only put a 3 inch hole in it and it was a very rough hole. But a 6 inch hole in 1/4 inch aluminium plate! GOD DAMN! Got any pics you can show us?

xyz

October 25th, 2003, 10:33 PM

blindreeper, the reason for that is because APPN is not particularly brisant, whereas ETN would be a lot more brisant.

For solving the oxygen balance problem, has anyone thought of a simple ETNFO mix? Assuming that metal powders are unavailable...

Unknown

October 26th, 2003, 01:22 AM

ALENGOSVIG1,
A friend of mine has been experimenting with the procedures. He found that if you don't add the nitrate to the H2SO4(HNO3) slowly enough and keep the temperature between 30-40 C then the yield goes down. Also, when precipitating the ETN in the water on the final step, the water should be kept in an ice bath/freezer for about 15 minutes before adding the solution. After adding the solution to the water, let it sit for at least 15 minutes. The best yield my friend achieved was by leaving the nitrate/H2SO4(HNO3) solution in the refrigerator overnight. My friend tried the HNO3 method a couple of times which resulted in smaller yields than the H2SO4 method. I am still working on posting the section on ETN from "The preperatory manual of explosives" that I scanned. When I get the pages posted, I will post the address in the "Links and literature>scanned anything lately..." section.

ALENGOSVIG1

October 26th, 2003, 07:09 PM

Upon reinspection of the hole it was only 5" across. Still not too shabby. :cool:

I dreamed of preparing some more ETN today but 5 mins after the erythritol addition i removed the beaker from the icebath to let it react and it took about 40 mins for it to cool from 20 to 15 degrees celsius.

I extracted the ETN out of the ETN/CaSO4 cake and ended up with 28g of recrystallized ETN.
Also, today i strapped a length (maybe 8 or 10 inches) of 1/4" I.D. plastic tube filled with 15g of ETN to a 2.5" diameter tree and severed it. I was very surprised how clean the cut looked. :D

Unknown, are your referring to the first or second edition of "preperatory manual of explosives"? I had the first edition and i dont remember there being a section on ETN.

Unknown

October 26th, 2003, 09:53 PM

I have the second edition. I've uploaded the two pages to www.x-mail.net (http://www.x-mail.net) . The username is "cheese" and the password is "cake". log into the right side that says, "user login". Once logged in, you will see the e-mails with the scanned pages attached in the inbox.

Chemical_burn

October 27th, 2003, 01:02 AM

Hey ALENGOSVIG1 got any pics and or video of the detcord you made and its effect on the tree. I would love to see it.

I have seen some homemade det cord with AP do the same thing to a tree it was also about 2 1/2" to maybe 3" in diameter and it also severed it pretty clean. It had 37grams of AP wich is a lot more than I would ever handle personally.

Microtek

November 1st, 2003, 07:00 AM

My primary interest in ETN is its use as a castable binder to replace TNT which is too weak and too insensitive for the scale that I work at. As I have been having trouble finding erythritol domestically, I have looked into possible alternatives.
One such alternative is MHN which melts at 112 C, but decomposes ( slowly ) at that temp. To get around that problem, I have combined several nitric esters to achieve a compound with high density low melting point and good mechanical properties:

- 40 parts MHN, 10 parts PETN, 1.25 parts EGDN and 0.1 parts NC are dissolved in acetone mixed until completely homogenous and evaporated to dryness at room temp.

- The resulting waxy mixture melts at 80-85 C, has an oxygen balance of + 5.5 %, a calculated density ( simple average ) of 1.73 g/cc and a calculated VOD of 8550 m/s ( Stine ).
Another semi-empirical equation that has been posted on alt.engr.explosives gave VOD 8560 m/s and detonation pressure 317 kBar.

Edit: I have prepared a sample of the cast composite and measured its density: 1.71 (+- 0.05) g . The sample was very small so the uncertainties are quite large, but it is encouraging that the preliminary results agree with theory.

Trinitrotoluene

November 1st, 2003, 11:34 PM

If someone is looking for an HNO3/H2SO4 method, it would likely be 4 moles of HNO3 to every mole of erthritol.

C4H10O4 +4 HNO3=C4H6N4O12+4 H2O

However I'm not too sure about the amount of H2SO4 that's being used.

Microtek

November 2nd, 2003, 06:33 AM

You are going to need more than the theoretical minimum amount of nitric acid. For PETN 2-3 times as much is used, so 8-12 moles HNO3 per mole erythritol would be closer I think.

knowledgehungry

November 2nd, 2003, 09:31 AM

You must remember that nitrations are equilibrium reactions. You must always use an excess of acid in these reactions, otherwise the reactent you wish to nitrate will not all be nitrated.

Sir Dudalot

November 13th, 2003, 02:08 PM

I used the method Axt posted with NH4NO3 proportionally and got a yield of 20g. The nitration time was 30 minutes. After my product had dried I tried casting it. Difficult but it can be done. I was able to cast a few grams but never got around to detonating it or anything else. I thought the product had very small crystal size similiar to my AP (I use 3% H2O2 which I've read leads to smaller crystals when making AP). Back to casting, I got a piece of aluminum foil and made it into a little V then put a "line" of ETN into it. After that I just held a lighter under it and put more or less heat to the foil and moved it over the powder until it started to melt and flow. It dripped out into the container I had and solidified completely in a few minutes.

In the pdf's Unknown posted they dissolved there erythritol in the sulfuric acid then added it to the nitric acid. In Axt's procedure they made a nitrating mixture then added the erythritol. I don't think it'd matter a whole lot either way but would there be much of a difference if any on what order you put things together? I'm also interested in how well it stores. I left my last batch sitting out for a week and a half it didn't appear to change although I didn't weigh it daily.

nbk2000

November 13th, 2003, 05:53 PM

It's nice to see you putting your heroin smoking skills to more productive use than chasing the dragon. ;)

Though I'd think that such a method would be a quick way to an explosion, due to local overheating if you're even a moment too long o one spot with the lighter.

Why not try using a container with the ETN in it and heating in a pot of hot water instead? Much safer.

Sir Dudalot

November 14th, 2003, 01:21 PM

Yeah...man do I feel dumb. For a good reason though. It would often catch on fire and I'd lose a half a gram that I was trying to cast but it never exploded. Hot water it a much better idea. I'll try casting some of my latest batch that way. I can see why everyone wants to cast explosives now. Before I always it was alright, not great, but good. Now I can see that casting an explosive is very very good.

Okay, it is definitely castable. Putting it in hot water is a hell of a good idea. I'm a jackass. I just heated water until it was almost boiling the put the ETN (in it's casing) in and came back in 30 minutes. When I got back it had melted and rehardened into a nice solid chunk.

mongo blongo

November 14th, 2003, 03:03 PM

Nice to know that it works. :)
The VOD of the cast explosive will be much closer to the theoretical value. I have read about an ETN/PETN cast mixture which would be perfect for shaped charges and EFPs. The liquid ETN is shown to have certain solvent properties towards PETN which makes this a very interesting castable explosive indeed. It's like they are made for each other. :)
Some advice for casting- If I were you I would use water like NBK mentioned and heat it in the actual container you are going to use it in. Rather than heating it and then pouring it in. This way you will get a much better cast without voids.
Damn it! I wish I could get my hands on some Erithritol! It seems it's not available in the UK anywhere! :(

ALENGOSVIG1

November 15th, 2003, 02:35 AM

I dreamed of making some ETN based plastic explosives today. I tried ETN/mineral oil/castor oil which worked well and made a nice plastic mass which didn't crumble. I've read that ETN is soluble in glycerin so i wonder if its soluble in castor or mineral oil. The plastic was ofcousre oily and seeped oil which was a downside. I think NG/EGDN ould have the same plasticizing affect and would ofcourse be more powerful.

I also tried using DNT/mineral oil/castor oil to plasticize ETN and it worked much better. I dissolved the DNT in warm acetone, added the oils, then stirred in the ETN and let the acetone evaporate. I got very moldable plastic blob but when worked in the hands for too long (gloves!) it became too soft. The plastic didn't seep nearly as bad as the first formulation though.

All in all a pleasant dream.

Trinitrotoluene

November 15th, 2003, 03:40 AM

SWIM also made some erythritol trinitrate today, using the ratio used by Axt.
100ml H2SO4
60grams KNO3
15 grams Erythritol

The powdered KNO3 was added to the 400ml beaker filled with 100ml of H2SO4 and cooled in a ice bath. After the temperaure had cooled down to 25*C a small quanity of erythritol was added than stirring, than all the erythritol was poured in it mixture became very hard to stirr, and the temperature shot up to 55*C, but it was suprising that no runaway occured, after vigerous stirring the temperauure went down to 40*C than to 30*C, where it was left in nitration mixture for 1 hour.A solid mass formed and than it was added to 1 liter of water, after waiting a few hours and vigerous stirring the potassium hydrogen sulfate finally dissolved, and the erythritol trinitrate is on the coffee filter filtering, and swim will soon neutralize it, and recrystailize it.

SWIM also took a small sample to cast it, around 2 grams, was placed into a beaker and boiling water was poured into it, the erythritol trinitrate melted, and it's a peach colored liquid, that still haven't solidified yet.

Axt

November 15th, 2003, 07:14 AM

Keep it cooler, slow down on the additions and stir every 5 minutes for as long as its in the acids. The ratio given should get syrupy but not solid unless it gets too hot.

I'll amalgamate and add to some info on ETN ive posted in other threads to make this one more complete.

The ETN/NM/NC composite mixed to 87/10/3 (%OB about -0.2) by some coincidence actually did form a very plastic mix, much better plasticity then AN/NM/NC probably due to NM's solvent effect on the ETN. Mix the composite by adding excess NM and evaporating back to the correct weight, then seal. Obvious problem being the volatility of NM, also if its kneaded you will end up with a layer of NM on your hand, which once dry becomes a layer of ETN stuck fast with NC thats hard to get off. Effect of detonation is seen in the shaped charge (http://geocities.com/roguemovie3/).

Drop test gives ETN a steel on steel sensitivity of 30-35cm with 3kg weight, compared to PETN which was 40-45cm on the same testing rig (http://geocities.com/roguemovie3/).

Nice to see everyone elses experiances, keep damage reports coming in... and hopefully im not the only dope to post pictures ;)

Unknown

November 25th, 2003, 08:37 PM

I was just looking through the COPE, and when I got to page 235, I saw "Nitroerythrite" with (Erythritol Tetranitrate) next to it. I don't know about you guys, but I didn't know that it was in there until last night. I figured I would post this since I haven' t seen any references to ETN being in the COPE. Don't get too excited though, because the paragraph dedicated to ETN is disapointingly short.

Rosco Bodine

November 26th, 2003, 12:28 PM

Actually it was that reference in COPAE that first got me curious
about ETN . Sounded like a good explosive , the development
of which had been abandoned some years ago because the
expense of erythritol in those days made it uneconomical for
use , even though the technical merits for the explosive were
recognized . After learning that erythritol later became cheaply
available by new methods of manufacture and was an OTC
sugar substitute , I decided to experiment with ETN as a material
for which research should be renewed due to the vastly improved
economics for its manufacture in the present time . It seems
many people got the same "bright idea" about the same time ,
and adopted the orphaned research concerning ETN , pleasantly
discovering it to be a very versatile and powerful , easily made
energetic material . Since the original research didn't get very far
because of the expense , most of what is known about ETN is being
reported online , by experimenters who are sharing whatever
they learn , in experiments which very possibly are entirely new ,
learning what was never known by anyone before . That's DISCOVERY .
That's good science . So I second what Axt said , keep the
"damage reports" coming ! The book on ETN is a book we
are writing ourselves with the reported results from each experiment
finding anything new .

A technical observation I can share is that a cosolvent system of
about one part acetone to two or three parts denatured alcohol
seems to be in the ball park for a good working volume for
doing recrystallization . Acetone alone seems too powerful a
solvent and traces of it can remain in the ETN , although it evaporates
from the melt . Denatured alcohol alone takes too much volume
of solvent to be economical because it isn't quite good enough
a solvent for the ETN , so that is why the strategy for a cosolvent
system . There is probably an optimum mix and temperature
from which the the ETN can be precipitated by gradual water addition ,
which results in nice crisp well formed crystals of correct melting point
direct from drying . When time permits , I will work out the best
procedure or anyone else feel free to go ahead and report on this
if they work it out before I do .

Rolfiboy

December 16th, 2003, 07:44 AM

Hi first of all i would like to excuse my english!

I have made this fine explosive, but i have the same problem, the synthesis are almost solid after 30min and i stir the mixture all the time, have any one tryed to put maybe 20ml water i the mixture before you put the Erythritol in it?:confused:

It burns like nitrocelullose, it is shocksensitive, and it is not a liquid!

Do any one know if it has a DtD rate?

Lets say we have 2g in a confined tube and we lit it in one end, would it built enoung pressure to detonate the rest?

That would be interresting for blasting caps!

I am very sorry for my english, I am Danish.

Oh the secondary explosives DtD in confined space idea, dit i get last friday, when me and 2 of my homies made a 20cm long 3mm steel tube with 3mm steel endplugs glued with some steel activator glue, loadet with some(100g) presset commercial granulated nitrocelullose(easy to buy legal in Denmark) and a electrical match, and surely it detonated with af very big boom and made a big crater i the frozen earth, me and my friends were about 50m away and were almost knocket down by the shockwave!!

FinnBell

December 17th, 2003, 03:42 AM

Okay, in other words you made a pipe bomb. So let me get this straight, you filled a steel tube with nitrocellulose and from 50 meters away the shockwave almost knocked you down? Correct me if Im wrong but I didnt think pipe bombs detonated. Because its not an actual high explosive, therefore it doesnt send off a shockwave. I dunno. Maybe you meant something else or maybe Im thinking about something else. And what about shrapnel?

Rolfiboy

December 17th, 2003, 07:50 AM

First of all i have made many steel pipe bombs before with NC and this was 10 times more powerfull than any thing i have made with NC before, the bomb was placed 3m behind a three, so the three where in our direction to cover for shrapnel, the funny thing where that no shrapnel was found only small holes in the three. that was a detonation for sure!!!

grendel23

December 17th, 2003, 07:54 AM

Adding water to the nitration mix would kill the yield. I know its a pain to stir after it turns to fudge, I have wanted to try it with NH3HNO3, that should be more liquid.

ETN and NC are both secondary explosives, they need to be initiated with a suitable primary to reliably detonate.

The fact that your pipe bomb went "boom" does not mean that the NC (smokeless powder I assume) detonated. It is designed to burn under high pressure in a firearm not detonate. If you want to detonate it you need to learn to make blasting caps.

Rolfiboy

December 17th, 2003, 08:18 AM

yes you are right about the yields. i know it need to be detonated but like many other secondary explosive that just a matter of deploying enough energy to the explosive, and NC(mine NC are not smokeless powder but a pure HE made for blasting purposses just Granulated NC) are both a LE and a HE, if you let the LE make enough energy like pressure(alot of pressure), it could detonate the HE, in a firearm the presure seeks the weakest spot.

The point is, if ETN also is a LE like NC and are more sensitive than NC, like NG i would be much easyer to detonate, NG will detonate if you deploy energy like much heat!!!

Rolfiboy

December 17th, 2003, 08:53 AM

another thing, you need a shockwave to detonate a secondary HE, but isnt a shockwave just pressurize air??? In Fact, to detonate a secondary HE you just need alot of presserure fast, and some secondary are more sensitive than other, like NG and ETN, i dont know how sensitive NC are but it will detonate if it are applyed enough pressure fast! If you understand this fact you could make very safe and storeable blasting caps!

Another thing: Have you recrystallised the ETN in acetone? Because my ETN and acetone mix have made some kind of liqued layer on the bottom of the mix but no crystals!!!??? very odd or are it supposed to do that? in the acetone/ETN mix ive put 1g sodiumbicarbonate to neutralize rest of the acid!

Microtek

December 17th, 2003, 12:28 PM

Rolfiboy: I would very much like to know where you obtained erythritol in Denmark as I haven't been able to find it OTC anywhere ( you can email the answer to me if you feel uncomfortable sharing it publicly ). Also, how do you purchase nitrocellulose around here ? Maybe you have a license that allows you to buy it ? I'm just curious, as I would prefer not going on record with that kind of purchase even if I could.

Many secondary explosives are capable of burning to detonation ( making DDT ) under certain conditions; inositol hexanitrate was used in a patent about a blasting cap without primary explosive ( inositol is cyclohexanehexol ). Also PETN has been used for this, but must be treated in a certain manner to give it a very porous structure. I have achieved partial detonations by igniting heavily contained MHN with a thermite mixture, but have since abandoned experiments of this nature.

FinnBell

December 17th, 2003, 01:05 PM

I didnt know NC was considered a secondary explosive. I thought it was just a deflagragant. If it can be initiated by a primary to detonate then why doesnt it detonate in a gun? A great deal of rifle primers contain something like lead azide or mercury fulminate dont they? Cause I know someone whos uncle owned a gunshop and he took a couple of packs of primers and soaked them in something to seperate it from tiny caps and it all started floating on the surface. It still wasnt much but it was just an experiment. But the point is that I thought that the rifle primers are about the equivilant to the shock of a primary, thus it would make the NC detonate if it could do so. Or is this too little of an amount to make it do that?

Rosco Bodine

December 17th, 2003, 01:38 PM

Originally posted by Microtek
Many secondary explosives are capable of burning to detonation ( making DDT ) under certain conditions; inositol hexanitrate was used in a patent about a blasting cap without primary explosive ( inositol is cyclohexanehexol ). Also PETN has been used for this, but must be treated in a certain manner to give it a very porous structure. I have achieved partial detonations by igniting heavily contained MHN with a thermite mixture, but have since abandoned experiments of this nature.

Von Herz had similar but earlier patents for detonators which used flame sensitive
secondary explosive base charges fired only by a hot igniter charge and not
initiated in the conventional way by shock from an unequivocal primary explosive .
ETN was one of the materials cited by Von Herz as useful in such detonators .
This is probably not a DDT effect which causes detonation , but rather a
"cooking off" of the secondary by a sudden and intense thermal shock .
Certain igniters which burn very fast and hot , are good for producing this
"cook-off" effect on sensitive secondaries with strong confinement . But this
unconventional method of intitation is not as sure and reliable as the more
conventional methods using a three stage firing train of low order DDT flash igniter , high order primary , sensitive secondary ( as the base charge itself or
as a booster for a fourth and final low sensitivity but high output base charge )
Such sequential firing trains give the highest performance and reliability .

The original patents of Von Herz are GB331162 and US1878652
The patent using inositol hexanitrate in the "cook-off" scenario is US1951595
Related patents are
US1751438 Sorbitol Hexanitrate
US1928208
US2195032
US2422043

Nitrolactose has also been reported to be a good base charge ,
but I do not know how it would perform in a "cook-off" scenario .

US1759565 Nitrolactose

Nitrostarch has also found usefulness as a detonator base charge
US1462075

Axt

December 17th, 2003, 06:13 PM

ETN will readily detonate if dropped onto a red hot surface often jumping around going pfft .. pfft ... pfft ... BANG!, less heat (less then red hot) it will often melt, evolve red fumes before detonating, even less heat it will melt before deflagrating. It does seem quite sensitive to thermal shock.

nbk2000

December 17th, 2003, 09:30 PM

Perhaps the addition of methylene chloride would thin things up a bit. :) After all, DCM is used in extraction of anhydrous HNO3 via freezing, so it's obviously inert to it.

Rolfiboy

December 18th, 2003, 05:10 AM

Microtek: I obtained erythritol from SOURCE REMOVED , I dont know if erythritol is legalized in Denmark, but Denmark isnt the fastest coutry, you know.
I buy nitrocelullose(I buy 3Kg every time) from the owner of this site(but be careful, I will send you an email): http://www.explosive.dk/ , I do think nitrocelullose is legal to buy in Denmark without a permission, many magic shop also sell out to normal peoble, anyway I would never use it to harm any one!

Well my electrical match is a commercial type that make a 1600celsius hot flame it could mabye detonate the ETN, I will try that later.

The second layer are gone and alot of crystals are created. When you make the acetone/ETN mix what color is it? mine are yellow to orange.

PhoeniX_KEA

December 29th, 2003, 12:54 AM

Xylitol is a completely natural sugar alcohol and it's in my local store where Erythritol isn't. I can't find and info regarding the applicability of this substance as a subsitute. Does anyone have any specific knowledge regarding the use of Xylitol?

blindreeper

January 1st, 2004, 11:00 PM

SOURCE REMOVED is the page on Xylitol Sorbitol, Mannitol, Maltitol, Isomalt, Xylitol and Erythritol are listed on their site as low carb sugars. You will notice that Sorbitol, Mannitol and Erythritol form well know explosives, SHN, MHN and ETN. My guess is that xylitol would to. To back this up there is a section in COPAE (page 242 for those who have it) They call is xylose which I am fairly sure is the same as xylitol, is states the nitration of d-xylose yeilds xylose tetranitrate.

Microtek

January 2nd, 2004, 05:00 AM

Actually, xylose is HOCH2-(CHOH)3-CH=O while xylitol is HOCH2-(CHOH)3-CH2OH so xylose will give a tetranitrate but xylitol will give a pentanitrate.

Nevermore

January 2nd, 2004, 06:57 AM

Originally posted by Rolfiboy
Microtek: I obtained erythritol from SOURCE REMOVED , I dont know if erythritol is legalized in Denmark, but Denmark isnt the fastest coutry, you know.
.

since Denmark is part of the EU i can tell you Erythritol has not been approved for OTC sell as a sugar substitute so it is not easy, i really don't know if is illegal to import or not, but they could give you troubles for that...
Make me know when you get if they opened the package to check or is the "smart" at ***rition wrote on the package that E is inside...

Anath

January 2nd, 2004, 08:33 AM

I think if they wrote that 'E' was inside it would definitely get confiscated!!

You should have no trouble importing Erythritol. Pretend you're a hippy, or diabetic or something, and make a fuss. It's only sugar substitute, after all. ;)
I take it that this supplier is made public now?

ALENGOSVIG1

January 2nd, 2004, 05:54 PM

Do we really need to post a source for every idiot who couldn't be bothered to type "erythritol" into a search engine? The answer is NO, we don't. Therefore i've removed all mention of ***rition from all above posts.

Jetex Kid

January 30th, 2004, 07:35 PM

I am excited about tne because here in the US, erythritol is commonly available while pentaerythritol and mannitol are not (contrary to some postings). Before I even began dreaming of explosives I believed nitric acid would be the big hurdle, but I now believe that there are damn few fuels available to create nitro-explosives if one wants it all: affordability, availability, stability, insensitivity, energy, brisance and possibly even castability. But erythritol might be able to do it all.

However, the book Explosives by Meyer, Kohler & Homburg, Fifth Edition (2002), says of etn: “It crystallizes out of alcohol as colorless plates. … The pure substance is extremely sensitive to shock and friction.” This sentence scares me. Even though the book is brim-full of typos and other errors it is a mainstream book by a big-name publisher (Wiley).

On the other hand, Paul W. Cooper in “Explosives Engineering,” (1996) says of etn: “It is not nearly as impact sensitive as nitroglycerine or the other liquids mentioned.”

Yet again, Jumala quotes Urbanski II as saying etn is similar to nitroglycerine.

I have yet to hear mention of isomers - could there be unstable ones? Or maybe etn typically contains sufficient erythritol TRInitrate to be insensitive.

(Incidentally, inositol was mentioned in this thread as a candidate for hexanitration, and while a cyclical structure sounds good for stability, be aware that the inositol sold at health-food stores is myo-inositol which is optically inactive and therefore supposedly not suitable for this purpose.)

The most encouraging thing I’ve heard concerning tne’s insensitivity is Roscoe Bodine’s statement that until recently erythritol was too expensive to allow much consideration to be given to tne. Thus it is possible that price was the only reason for the world’s avoidance of tne.

And incidentally would anybody know why erythritol is so named, when “eryth” means “red” in Greek?

TNE is 63.6% oxygen and it’s all available for aluminum. I like loud noises and their reverberations, and wanna hear what a stoichiometric mixture of 58% etn and 42% two-micron aluminum sounds like.

Microtek

February 1st, 2004, 07:20 AM

Very few pure nitric esters can be said to be insensitive, and none of those are very powerful. Anyways, whether an energetic material is said to be "very" sensitive or "somewhat" sensitive is something that depends a lot on what the material is compared to. Older sources will generally compare to things like NG while newer sources more often compare to TNT or RDX.
So, where does ETN ( which is the established acronym on this forum ) lie ? Well most likely it has mechanical sensitivities that are almost identical to MHN or NG, meaning that you won't be able to set it off with ordinary careful handling, but a not-too-severe hammerblow will do it.

Rosco Bodine

February 1st, 2004, 01:51 PM

Originally posted by Jetex Kid
I am excited about tne because here in the US, erythritol is commonly available while pentaerythritol and mannitol are not (contrary to some postings). Before I even began dreaming of explosives I believed nitric acid would be the big hurdle, but I now believe that there are damn few fuels available to create nitro-explosives if one wants it all: affordability, availability, stability, insensitivity, energy, brisance and possibly even castability. But erythritol might be able to do it all.

You got that right . Exactly why ETN fits the bill
as a desirable explosive .

However, the book Explosives by Meyer, Kohler & Homburg, Fifth Edition (2002), says of etn: ?It crystallizes out of alcohol as colorless plates. ? The pure substance is extremely sensitive to shock and friction.? This sentence scares me. Even though the book is brim-full of typos and other errors it is a mainstream book by a big-name publisher (Wiley).

On the other hand, Paul W. Cooper in ?Explosives Engineering,? (1996) says of etn: ?It is not nearly as impact sensitive as nitroglycerine or the other liquids mentioned.?

Yet again, Jumala quotes Urbanski II as saying etn is similar to nitroglycerine.

Trust the second source . ETN is about a third more sensitive than PETN and that is not unduly sensitive for safe handling .

I have yet to hear mention of isomers - could there be unstable ones? Or maybe etn typically contains sufficient erythritol TRInitrate to be insensitive.

ETN is one hundred percent the tetranitrate , confirmed by melting point , crystal and explosive properties .

(Incidentally, inositol was mentioned in this thread as a candidate for hexanitration, and while a cyclical structure sounds good for stability, be aware that the inositol sold at health-food stores is myo-inositol which is optically inactive and therefore supposedly not suitable for this purpose.)

Do you have information from experimental results
or literature which reveals the myo isomer of inositol
as being unsuitable for nitration , or are you
only speculating that only optically active isomers
may be nitrated to the hexanitrate ? I have on hand
some myo-inositol but I have not attempted to nitrate it .
It would seem that dissolving inositol in sulfuric acid
prior to nitration would perhaps tend to make isomer distinctions for the precursor moot . I would guess
that the extreme conditon presented by such a sulfonation would either lead to a common sulfonation intermediate by rearrangement , or else would dehydrate and carbonize the inositol . Please elaborate on your reported unsuitability of myo-inositol as a candidate for nitration .

The most encouraging thing I?ve heard concerning tne?s insensitivity is Roscoe Bodine?s statement that until recently erythritol was too expensive to allow much consideration to be given to tne. Thus it is possible that price was the only reason for the world?s avoidance of tne.

Economy was indeed the principal reason that the usefulness of ETN was never fully researched following its discovery .
ETN was recognized as a fine explosive , but just
too expensive for use given the former high cost
of the main precursor .

And incidentally would anybody know why erythritol is so named, when ?eryth? means ?red? in Greek?

I don't know for certain about the name origin ,
but my guess would be that the plant from which it was isolated was probably a red algae , moss , or seaweeed .

TNE is 63.6% oxygen and it?s all available for aluminum. I like loud noises and their reverberations, and wanna hear what a stoichiometric mixture of 58% etn and 42% two-micron aluminum sounds like.

More interesting yet is the exploitation of oxygen deficient explosives as part of a melt mixed together with ETN to form Oxygen Balanced cast mixtures , some of which may
be solids or plastics at ordinary temperatures .

Jetex Kid

February 1st, 2004, 02:11 PM

I am excited about tne because here in the US, erythritol is commonly available while pentaerythritol and mannitol are not (contrary to some postings). Before I even began dreaming of explosives, I believed concentrated nitric acid would be the only problem, but I now see that there are very few fuels with which to create nitro-explosives if one wants it all: affordability, availability, stability, insensitivity, energy, brisance and possibly castability. Erythritol could fill the bill.

However, the book Explosives by Meyer, Kohler & Homburg, Fifth Edition (2002), says of etn: “It crystallizes out of alcohol as colorless plates. … The pure substance is extremely sensitive to shock and friction.” This scares me. Even though the book is brim-full of typos and other errors, it is a mainstream book by a big-name publisher (Wiley).

On the other hand, Paul W. Cooper in “Explosives Engineering,” (1996) says of etn: “It is not nearly as impact sensitive as nitroglycerine or the other liquids mentioned.” Yet again, Jumala quotes Urbanski II as saying etn is similar to nitroglycerine. (With no bubbles or ice crystals, ng is quite insensitive.)

I have yet to hear mention of isomers - could there be unstable ones? Or maybe etn typically contains sufficient erythritol TRInitrate to be insensitive.

(Incidentally, inositol was mentioned in this thread as a candidate for hexanitration, and while a cyclical structure sounds good for stability, be aware that the inositol sold at health-food stores is myo-inositol which is optically inactive, so supposedly unsuitable for this purpose.)

Roscoe Bodine notes that until recently erythritol was too expensive to allow much consideration of tne. Thus price could have been the only reason why the world has avoided tne.

And incidentally would anybody know why erythritol is so named, when “eryth” means “red” in Greek?

TNE is 63.6% oxygen and could be used in flash powder, with 42%/58% aluminum/etn constituting a stoichiometric mix with 2,850 cal/g. It wouldn’t be brisant but it would be loud, and I like loud.

Well, I thought I should mention that a current book claims that tne is “extremely sensitive.”

Jetex Kid

February 1st, 2004, 03:58 PM

Rosco, US Patent 1850225 specifies optically active inositol as the precursor to hni. I dunno why.

They say if you don't hexanitrate optically inactive inositol, it is good for your cell walls.

Rosco Bodine

February 1st, 2004, 05:24 PM

Originally posted by Jetex Kid
Rosco, US Patent 1850225 specifies optically active inositol as the precursor to hni. I dunno why.

They say if you don't hexanitrate optically inactive inositol, it is good for your cell walls.

The patent is in front of me , and while it is true
that the patent claims only mention optical isomers ,
there is no mention made to exclude the possibility
of other isomers such as myo-inositol also being
nitratable to a hexanitrate . Here again is a possible
example of economics being the operative consideration , since a synthetic method was described for producing an optically active form of inositol from a waste product
of the natural rubber industry , quebrachitol . Actually quebrachitol itself forms a useful explosive after nitration . The emphasis of the patent seems to be making use
of an industrial waste product , and does not explore the nitration of the dietary form of inositol or myo-inositol ,
which was probably an expensive material then , and still is expensive today . However , there seems to be no really obvious reason why regular myo-inositol should not form
a hexanitrate . I think you may be reading something between the lines of the patent that isn't really there .
So lets not "presume facts not in evidence" where chemistry is involved . A person who may just assume you know what you are talking about might be disuaded from doing
a valid synthesis for believing it won't work , when it could work just fine . Also I think you should check your OB figures for ETN , because not all of the oxygen is available as surplus . For greatest brisance usually the mix is optimized
so that carbon is converted to carbon monoxide and not all the way to carbon dioxide , as would be what most people think is oxygen balanced .

Rosco Bodine

February 1st, 2004, 08:30 PM

Lets put the inositol isomer question to rest
by referencing a later patent US1951595
by the same inventor , Mr. Crater :cool:
( gotta love an explosives chemist named
so appropriately ) :D

According to Mr. Crater , i-inositol forms a
useful hexanitrate , ( and i-inositol is the same
as myo-inositol or meso-inositol , otherwise
known as "dietary inositol" , all the same isomer )

See line 41 of the patent US1951595 .

Time for humble pie Jetex Kid ;)
myo-inositol works just fine !

Just ask Mr. Crater :)

Jetex Kid

February 2nd, 2004, 02:46 AM

Rosco, you are 100% right and I must thank you for saving me from eating my very expensive i-inositol. Mr. Crater filed one patent in 1930 based on optically-active inositol, and the same patent three years later for optically-inactive inositol. I did not read his second patent because I was discouraged by his first. I’m glad you did. Humble enough for you?

That HNI can be initiated by flash powder would be a big plus for the indoor lab, eliminating lead or mercury. :cool:

Regarding a relationship between brisance and evolution of CO or CO2, Explosives Engineering by Cooper lists PETN (CO2) as having the highest Gurney constant of classical explosives, including HMX. I know Gurney is not brisance, but it may be a better figure of merit for HE than brisance.

Bert

February 4th, 2004, 12:37 PM

I recall seeing a recent discusion on stabilizing ETN for longer term storage by recrystalizing with a urea and bicarbonate solution on the forum somewhere. But it's not in the main thread, and I've been unable to locate it by searching. Can anyone point me to it? Thanks! Also, any reason not to use diphenylamine???

(edit)
Sorry, it was on Science Madness
ETN / PETN ( 2 / 5 ) Melt Composition by Mr. Anonymous (http://www.sciencemadness.org/talk/viewthread.php?tid=890) posted by Axt on 11/16/03

Still wondering about using diphenylamine though- Anyone got an idea about that? It's highly soluble in alcohol, will it precipitate properly with ETN?

Boomer

February 5th, 2004, 10:31 AM

I am 99% sure that I read about dephenylamine as a stabiliser for either MHN or nitrostarch in some patent or book. It works by absorbing the NOx thus preventing autocatalysis. There is no reason why it should not work for ETN, even if it is not perfectly distributed between the crystals.

Bert

February 5th, 2004, 01:40 PM

I was looking at a site for a company making military and pyrotechnic chemicals. They claimed that diphenylamine was NOT compatible with nitroglycerine. I've never heard that said before- Does anyone have any idea what that might be about? I'd like to understand this, and wonder if ETN might be similarly incompatible?

Here's the source of the claim- PROPELLANT STABILIZERS (http://www.cinadra.com.br/propellantstabilizers.htm)

If there isn't a thread here on the theory and techniques of stabilizing explosives here, it might be a good thing. There's some information distributed throughout the site piecemeal, I'd love to see a central repository of information to assess stability & storage issues.

grendel23

February 6th, 2004, 06:52 AM

I have a bottle of Alliant Bullseye in front of me and the ingredient list includes diphenylamine along with ethyl centralite as stabilizers.

Bullseye has one of the highest percentages of NG of any DBSP, so I would tend to discount the claims of Cinadra.

I agree that a thread on stability would be great, I tend to enjoy synthesis more than the use of energetic compounds, so I often have more around than I should.

Bert

February 6th, 2004, 10:05 AM

I've got several of my father's books, including one by Roberts with VERY detailed process information on the making of commercial spherical DB powders. It quite definitely calls for the use of diphenylamine as a stabilizer incorporated into the finished propellants. That's why I was amazed to see a professional supplier of these formulations claiming it was incompatible.

(edit)

OK- I've started a new thread on Purification, stabilizatin and storage of explosives (http://www.roguesci.org/theforum/showthread.php?s=&threadid=3704) in the chemistry related section. Please feel free to add to it-

In the meantime, SWIM has re-crystalized ETN from denatured alcohol with an additional 2% of diphenylamine. If he has time and can get access to a lab oven, he may do a time & temperature study of decomposition.

atlas#11

March 11th, 2004, 04:21 PM

No one has said any thing on this in a while so I'll just wake it up again.

Any ways, I dreamed this on a half batch with NH4NO3 and got a fairly bad yield, 5.6g for 7.5 g of erythritol before recrystilization. I let it sit for a good 30 min. before dumping and It only reached 15C. I didn't waste more that a gram with filtering so I don't know what the hell went wrong. Recrystilization was easy and I didn't lose too much so no harm done their. Maby colder reaction temp?

The price on ***rition has gone down as well so this will be a fun and cheap explosive to make. Im out of nitrate(except barium and strontium) so I will have to get a 50lb bag of it some where and continue experimenting. With the stuff I already have I'll cast it into detonators and see how it preforms. Or, maby make some mini shaped charges and post some pics hopefully. Either way, I'll be dreaming about this one for a while.

Rosco Bodine

April 8th, 2004, 08:04 AM

The use of NH4NO3 as a substitute for sodium or potassium nitrates
has not produced yields as good for me in nitrations of this sort .
Why the metallic nitrates give better results is unknown to me .
I speculate that the equilibrium for producing free nitric acid from
NH4NO3 is more favorable for distillations of the nitric acid from
its mixture with sulfuric acid , than is that equilibrium favorable
for direct nitrations by the mixture .

Regarding the matter of using melt cast ETN alone or mixed with
PETN or other crystalline explosives to provide a dense , high output
charge , there is an old Nobel patent confirming the technical merit
of the strategy for improving the energy output of detonator base
charges . Melt cast ETN is mentioned by the patent , in Example 3 .

GB297853

The use of RDX as a filler in melt cast ETN mixtures would probably
also result in an extremely powerful composition , similarly as is true
for the ETN/PETN melt cast composite .

Using Inositol Hexanitrate as a filler in an ETN melt cast mixture
could possibly provide a melt castable detonator base charge
which can be fired by the " cook off " method , providing a
high output detonator in which it is not essential for there to be
present the usually required primary explosive such as an azide .

Mr Cool

April 8th, 2004, 09:11 AM

Porous explosives tend to work better if using that method - I'm not sure how easy it would be to get it to work with the solid, flat surface provided by melt casting the explosive.
Although I suppose they are very sensitive...

atlas#11

April 8th, 2004, 02:14 PM

I would prefer to use a primary, the det. is more instant and probably more reliable. Plus you would probably lose power (not that it matters with etn, it's powerful enough) because of losses to combustion. Maby the added safety is worth it.

As far as NH4NO3 not giving good yeilds, I just use more of it and a little more acid, the avalibility in this area makes it much more cost effective. I havent been able to find ammonium nitrate in any chain store yet aside from as cold packs, but if you dress up like a hick and drive an old truck in to an old farm supply store thats ran by an old timer you can buy as much as you can fit on your truck and no one would suspect any thing. Just don't go in there wearing a towel on your head and you should be able to get some.

My last batch suffered a runaway quite badly due to insuffecient coolingso the yeild realy sucked. I was going with a double batch using AXT's method and my ice bath was too small, like an inch to low so the batch rose about an inch above the ice/water. The cold pack I was using had exactly 117 g of nitrate in it, it's as if they intended for me to make etn with it. Any ways the yeild was 11.6 grams from 30g of erythritol. It was still enough to make a decient boom. I have to burry my charges now, some asshole idiots moved in just up the road and their prety easy to scare. Plus, the police have been up here snooping around so I have to watch it.

fulminans

April 8th, 2004, 05:20 PM

However, the book Explosives by Meyer, Kohler & Homburg, Fifth Edition (2002), says of etn: “It crystallizes out of alcohol as colorless plates. … The pure substance is extremely sensitive to shock and friction.” This scares me. Even though the book is brim-full of typos and other errors, it is a mainstream book by a big-name publisher (Wiley).

On the other hand, Paul W. Cooper in Explosives Engineering,” (1996) says of etn: “It is not nearly as impact sensitive as nitroglycerine or the other liquids mentioned.” Yet again, Jumala quotes Urbanski II as saying etn is similar to nitroglycerine. (With no bubbles or ice crystals, ng is quite insensitive.)

If you compare the data given for impact sensitivity in Meyers book with data given for NG and PETN you have a clear statement: ETN 2 Nm; NG 0.2 Nm ;PETN 3 Nm!!!!! So the statement of extremely sensitive is relative.......
This tells nothing about friction sensitivity of ETN, PETN is the " borderline Explosive" between primarys and secondarys. Perform a simple test in a Mortar and Pestle experiment with ETN and PETN and you'll get a rough imagination about friction sensitivity.
In my opinion the stuff is perfectly suitable for small shaped charges in combination with PETN or alone. Another use could be the manufacture of dets like mentioned somewhere in sciencemadness forum by mr anonymous. The only difference I would go for is the capability of DDT with this stuff. This means base charge of molten ETN ( with or without PETN) 0,5-0,8 g, intermediate charge of ETN or PETN 0,3- 0,5 g compressed to approx density of 1- 1,3 g/ccm and DDT charge ( 0,3 g) of a mixture of ETN or PETN, and Potassium Picrate/ Potassium perchlorate 8:1:1 like mentioned in Patent WO26603. With the higher mass of explosive you'll compensate for bad confinement and get a perfectly safe and reliable detonator, without the use of sensitive primaries. Sensitive means also sensitivity towards electrostatic discharge, the most ones tend to ignore this problem when constructing their blasting caps!!!

Rosco Bodine

April 9th, 2004, 12:25 AM

Mannitol Hexanitrate is the proverbial "borderline explosive" , not PETN .
The "nitromannite" is a good bet also for doing the neat trick of
cooking off , that is detonating directly from thermal shock .
Nitroglycerin can easily cook off too . Tetracene and Nitromannite
blended together form a high energy composite which is a primary
and capable of initiating secondary high explosives . It seems to me
that a similar performing composite might result from mixing basic
lead picrate or other "low order detonating" primaries with nitromannite .
Such a composite could possibly substitute for azides as an initiator .

The actual sensitivity to impact for ETN is about a third greater than PETN ,
meaning the drop hammer will only need fall from about two thirds the height
for ETN as is needed for PETN . Loose crystalline ETN is not unduly sensitive .
For cast ETN the sensitivity decreases considerably , and the same for
composites made using ETN as a fusible binder . ETN / PETN composite
is more difficult to initiate by shock , than is compressed crystalline PETN
of the same sample as used for making the composite .

Mannitol Hexanitrate and ETN might make an interesting melt cast .
It would be more sensitive than ETN / PETN . Because the ETN has
an oxygen surplus , TNT could be another useful material for mixtures
which could be melt cast . Some of these mixtures might be useful
as very high output cast charges . There is plenty of room for experiments
yet to be done with ETN compositions .

Mr Cool

April 9th, 2004, 08:57 AM

Rosco Bodine

April 9th, 2004, 01:04 PM

"The "nitromannite" is a good bet also
for doing the neat trick of cooking off , that is detonating
directly from thermal shock."

Is it just the thermal shock provided by the igniting charge,
or does the MHN undergo a DDT at an increased rate due
to the heat and pressure created by the igniting charge?
I've noticed that MHN is a lot more flammable with a
small amount of charcoal added (I was using the charcoal
originally to ensure even mixing with another white powder),
and so this may help it undergo DDT...

I briefly used MHN with a little silver acetylide nitrate (~15%,
but it's a compromise between minimum reliable quantity and power)
as a primary, it was very powerful and detonated even in tiny quantities.
I'm sure other easy to initiate, yet low power primaries, eg basic lead picrate,
would work just as well.

Yeah , *thermal shock alone* is all it takes for some of these sensitive
secondary high explosives to go directly to high order detonation ,
skipping completely over any ignition or deflagration to detonation
accelleration scheme . Axt described what happens when dropping
ETN onto hot steel , and when particles fall upon the steel which is
at the right temperature , they detonate on contact , just as is true for nitro and
a few other explosives that can cook off when heated very hot very suddenly .

Mixing a very hot and fast flash igniter with such a sensitive secondary
can provoke its detonation , even if the flash igniter is not itself an explosive
but something like a very fast burning thermite will do the trick , and
so will low order detonating flash igniters which burn hot enough .
The sudden heat alone is what provokes the detonation , while other
effects capable of causing the detonation may be regarded as redundancy .

fulminans

April 9th, 2004, 04:53 PM

energi

April 9th, 2004, 10:10 PM

So why not an improvised detonator conisting of
.5 gram flash powder pressed onto 2 grams ETN.

kclo4/al|ETN

The 2 gram ETN should be highly pressed inside a metal cap, and then .5 gram kclo4/Al flash tamped directly untop of it.
If ETN is capable of a thermal detonation, kclo4/Al would do it. This flash is the most powerful LOW explosive(borderline high order), and creates and EXTREMELY INTENSE pulse of heat energy, and even pushes out gas at a force probably equivalent to a hammer blow.
This detonator consists of no incredibly sensitive and unreliable primaries, could be easily manufactured, and stored for long periods of time.
We can aruge theory all day but is anyone willing to experiment on this, can the energy from a powerul low explosive in direct contact set off a semi-sensitive HE?

Rosco Bodine

April 10th, 2004, 11:24 AM

[QUOTE=Rosco Bodine]Mannitol Hexanitrate is the proverbial "borderline explosive" , not PETN .
The "nitromannite" is a good bet also for doing the neat trick of
cooking off , that is detonating directly from thermal shock .
Nitroglycerin can easily cook off too . Tetracene and Nitromannite
blended together form a high energy composite which is a primary
and capable of initiating secondary high explosives . It seems to me
that a similar performing composite might result from mixing basic
lead picrate or other "low order detonating" primaries with nitromannite .
Such a composite could possibly substitute for azides as an initiator .

QUOTE]

Look at the Patent given above, this is exactly what you do with Potassium Picrate/ KClO4 /PETN 1:1:8 , but safer than lead picrate or tetrazene, and much easier and more safe to prepare. The potassium picrate is capable of detonation under certain conditions ( uncompressed powder), therefore it is no longer used in pyrotechnic whistle compositions. The problem with this stuff is that it´s burning rate decreases with increasing pressure. Thats not good for DDT transfer, therefore you add KClO4 and get a perfectly safe solution. The same will work with fast thermite, and other HEP = (High energy pyrotechnics) The only difference is the rigidity of the cap material needed. I´m not a big friend of nitromannite because of it`s poor stability. I don`t know the stability of ETN. O.K. this will depend on crystallization procedure/neutralization of trace acid and addition of stabilizers like diphenylamine. The oxygen deficiency of PETN (- 10,1 %) will perfectly compensate for oxygen excess of etn (+5,3%) in a 2:1 mixture. TNT is a lame duck and melts at low temperature. Why mixing two low melting substances???

TNT may be useful in forming melt cast composites as an explosive fuel
and a crystallization modifier for the melt .

The other problem is stability of etn! It is known that PETN stability in Pentolite is much lower than in pure state. PETN is the most stable nitric ester, because of it`s highly symetric structure, etn is linear and more unsymetric, therefore less stable. It´s more similar to NG than to PETN.

If ETN stability suffers in combination with TNT used as a crystallization
modifier for composites using ETN as a fusible binder , then don't use
TNT as an additive . I have done no experiments using the TNT as an
additive , so I can offer no data as to how the stability is affected .

The "cook off" is another subject, but pressure plays a more significant role.

In a DDT scenario pressure builds from deflagration . Cook off from
thermal shock is very different .

What do you get when energetic material is heated very fast= pressure due to decomposition and vaporization. In some cases DDT works under slight confinement in others only under rigid confinement.

When tiny particles detonate on contact with a hot surface , there
must be a different mechanism than DDT , since there is an insufficient
mass present to proceed to detonation via DDT .

I`ve tried long time ago a few mg of NG wrapped in Al-foil on a preheated hotplate. Gives very nice boom and Al-layer on hotplate and people start asking how you`ve done this. The same works with HMPD. PETN didn`t work under this conditions.....
Slow heating is a different matter from "thermal shock" .

Therefore I call it borderline explosive, and it`s also called so in some german literature ( Houben Weyl). MHN is definitely a primary explosive and there`s no way of being borderline. It`ll undergo DDT transfer easily, but even more efficient with addition of some pressurizing mixture or thermal shock applications.
Smokeless powder will demonstrate DDT , and so will many other secondary
high explosives .....but they are not primary explosives , and neither is MHN .
In COPAE , Davis writes concerning nitromannite :
"It is not fired by the spit of a fuse , but is made to detonate by the flame of
a match which causes local overheating . It is *almost* , but not quite ,
a primary explosive ."

How we manage this is just a question of personal preferences. I like potassium picrate and barsty, you like tetracene and basic lead picrate :-))).
I have never even made tetracene and therefore have no preference
nor recommendation for it . I simply referenced tetracene as a mild
primary , which will form a powerful mix having the properties of a
primary for the mixture , when combined in mixture with MHN .
If MHN was already a primary , there would be no need for composite
mixtures whose purpose it is to make it a primary .

Rosco Bodine

April 10th, 2004, 12:13 PM

We can aruge theory all day but is anyone willing
to experiment on this, can the energy from a powerul low explosive
in direct contact set off a semi-sensitive HE?

Yes it can work , and has been done , using pyrotechnic flash powders
as an initiator for a base charge in detonators . There is at least one patent
concerning this . IIRC , a magnesium / perchlorate flash powder was used
to initiate a progessively increasing density PETN base charge which had
some special confinement provided by a strong steel sleeve designed to
focus the detonation wave . But the process was a shock detonation scenario .

For MHN , there would probably be no need for such special confinement .
MHN is as sensitive as nitroglycerin , and at the right diameter , the
shock produced by a pyrotechnic flash powder would very likely be
sufficient to detonate the MHN , it being a combined mechanism
for such an initiation , of concussion and thermal shock .

The pyrotechnic "flash powders" are hot for sure , but whether they are
hot enough for a certain sensitive secondary to cook off , is a matter
for experiment . There are some compositions mentioned in patents
which will do the trick , but I don't recall regular flash powder as being
one of those compositions . After doing some thinking about it , it
was my conclusion that firing trains based upon pyrotechnic initiators
would have to be constructed on a larger dimension to be reliable ,
than detonators of usual size . Generally , the less energetic is the primary ,
the larger becomes the "critical diameter" for it to function as an initiator .
What may not work for a 6 mm diameter column , may work every time
for a column diameter of 10 mm . That should be kept in mind for
any experiments in this area .

fulminans

April 10th, 2004, 04:05 PM

Yes it can work , and has been done , using pyrotechnic flash powders
as an initiator for a base charge in detonators . There is at least one patent
concerning this . IIRC , a magnesium / perchlorate flash powder was used
to initiate a progessively increasing density PETN base charge which had
some special confinement provided by a strong steel sleeve designed to
focus the detonation wave . But the process was a shock detonation scenario .

For MHN , there would probably be no need for such special confinement .
MHN is as sensitive as nitroglycerin , and at the right diameter , the
shock produced by a pyrotechnic flash powder would very likely be
sufficient to detonate the MHN , it being a combined mechanism
for such an initiation , of concussion and thermal shock .

The pyrotechnic "flash powders" are hot for sure , but whether they are
hot enough for a certain sensitive secondary to cook off , is a matter
for experiment . There are some compositions mentioned in patents
which will do the trick , but I don't recall regular flash powder as being
one of those compositions . After doing some thinking about it , it
was my conclusion that firing trains based upon pyrotechnic initiators
would have to be constructed on a larger dimension to be reliable ,
than detonators of usual size . Generally , the less energetic is the primary ,
the larger becomes the "critical diameter" for it to function as an initiator .
What may not work for a 6 mm diameter column , may work every time
for a column diameter of 10 mm . That should be kept in mind for
any experiments in this area .

Thats absolutely right, here's a newer Patent given for this subject:

United States Patent 5,945,627
Arpin , et al. August 31, 1999

--------------------------------------------------------------------------------
Detonators comprising a high energy pyrotechnic

Abstract
In-hole and surface detonators are provided which are essentially free from primary explosives. The detonators utilize a high energy pyrotechnic mixture of a fuel and an oxidizer for initiation of a base charge enclosed in the detonator, or for the initiation of an adjacent shock tube. Improved safety during manufacture of detonators is achieved.

fulminans

April 10th, 2004, 04:32 PM

TNT may be useful in forming melt cast composites as an explosive fuel
and a crystallization modifier for the melt .

If ETN stability suffers in combination with TNT used as a crystallization
modifier for composites using ETN as a fusible binder , then don't use
TNT as an additive . I have done no experiments using the TNT as an
additive , so I can offer no data as to how the stability is affected .

In a DDT scenario pressure builds from deflagration . Cook off from
thermal shock is very different .

When tiny particles detonate on contact with a hot surface , there
must be a different mechanism than DDT , since there is an insufficient
mass present to proceed to detonation via DDT .

Slow heating is a different matter from "thermal shock" .

Smokeless powder will demonstrate DDT , and so will many other secondary
high explosives .....but they are not primary explosives , and neither is MHN .
In COPAE , Davis writes concerning nitromannite :
"It is not fired by the spit of a fuse , but is made to detonate by the flame of
a match which causes local overheating . It is *almost* , but not quite ,
a primary explosive ."

I have never even made tetracene and therefore have no preference
nor recommendation for it . I simply referenced tetracene as a mild
primary , which will form a powerful mix having the properties of a
primary for the mixture , when combined in mixture with MHN .
If MHN was already a primary , there would be no need for composite
mixtures whose purpose it is to make it a primary .

A crystrallization modifier for TNT is HNS. It prevents formation of large crystals during cooling and resolidification of the melt. ETN/TNT will form something similar to pentolite, but lower melting and has anyway less problems with formation of cavities. I tryed pentolite 50:50 with 1 % Wax and it works fine.
The rest of this discussion may be a little bit too theoretic, nearly every energetic material will undergo cook off or DDT under the right conditions. I'm reloading different calibers of ammunition and had a bad experience with reduced loads of relatively progressive propellant in a large rifle shell. The load was 5 gr or 0,324g of smokeless powder, it wrecked my expensive rifle and gave me a new feeling about power of relatively safe NC propellant.
Energi is right, it's time for experiments and real world data......, Patents mostly tell only a part of truth.

Rosco Bodine

April 10th, 2004, 08:23 PM

Patents which are accurate in their disclosure of information
can be an extremely valuable resource , much better for
very specific details than is the usually more generalized
information provided by textbooks for example .

There is an interesting patent which I happened to recently
read which contains some information relevant to clarifying
the gray area between primary and secondary explosives ,
in terms of the concept of a firing train . The substance
described is a relatively obscure explosive called
guanyl azide picrate , or diazoguanidine picrate .
It powerfully detonates from heating or from shock and
yet it is used as a base charge in a detonator where it
functions as a *secondary* . It possibly could be a *primary*
but because of the difficulty of ignition which is one of its
deficiencies , a more easily ignited primary is used as a top charge .
The same strategy has been applied to tetracene and also to
lead styphnate in firing trains where they are made to function
better as a sensitive base charge , since their performance as
initiating primaries is "borderline" . Certain explosives are evidently
"crossovers" between categories of primary or secondary , and can
actually function as either one depending on the way they are used .

GB470418 detonator using a base charge of guanyl azide picrate

pdb

April 11th, 2004, 07:01 AM

Cyanuric triazide is a crossover as well.

Boomer

April 13th, 2004, 01:25 PM

IMO cooking off NG or MHN is not reliable in a detonator! I used to make dets from an aluminium pipe filled with pressed MHN, with a resistor in the middle that melted and finally (10 sec.) exploded the MHN. Though they worked every time for straight (NG) dynamite, they were much less powerful than the same type with some silver fulminate around the resistor.

The MHN definitely detonated (it cannot explosively deflagrate as it hardly burns without being molten first), but it was a low order detonation. The pipe was blown into a few pieces only, while with 20mg fulminate added it was literally pulverised. :D

I also made those pyrotechnic/MHN caps some time ago. With a strong housing (metal pipe with 1mm wall, crimped) 1g Armstrongs mix on top of 1g MHN worked reliable. The MHN was mixed with ground glass to make it more sensitive to the shock from the Armstrongs.
Do I have to say that pressing them was scary as hell, and that they should not be stored? :p

Now I concentrate on EBW caps. They are by far the safest caps possible, you could probably give them to your children to play with without danger (unless they hammer them flat)! They dont even go from a car battery or mains socket as they need 1 million watts, reached within 1 microsecond to detonate.
The b-box for them is ready, it is the size of a 5 1/4" HDD, charging 20 seconds.
If you want I can post schematics, but better in the EBW threat.

Mr Cool

April 13th, 2004, 02:07 PM

Please post schematics in the EBW thread. Thanks!

FinnBell

May 4th, 2004, 02:30 AM

Okay, so check this out right. Earlier today I attempted to use axts method for ETN.
I used 100 ml of H2SO4
60 grams of KN03
15 grams of Erythritol

I started by cooling the acid pretty cool in my fridge. I didnt check the temp but It was pretty cold so I added the 60 grams of potassium nitrate slowly, it did get pretty warm at times. When it got really warm I stopped adding and put it back in to cool it down. After that was all over I added the 15 grams very slowly making sure to keep it nice and cool. I would add a bit, cool it down then add more until it was completely mixed. I let it sit in the fridge for about fifteen mins then I took it out and poured water into the beaker with it and it got hot as hell and let off tons of red fumes. I just poured it all into a coffee filter and continued to pour water through it until the only thing left were small crystals. It was a very small amount. Now the thing is, I dont know if this is ETN or not. I took a little of it after it dried and lit it with a lighter but it didnt even light, it just melted and nothing else. I thought ETN was supposed to burn like NC. What did I do wrong? Am I missing something? :confused:

Bert

May 4th, 2004, 03:08 AM

Yes, you missed several things. Go back and re-read Axt's synthesis, especialy the instructions regarding temperatures, times and order of additions. Also read the subsequent posts, and observe the instructions for maximizing yields.

You are lucky not to have been treated to a nice hot acid shower.
NEVER add water to a concentrated acid. ALLWAYS add the acid to the water. I hope you wear eye/face protection and other protective gear.

Nitration or other reaction descriptions that call for a specific temperature range do so for a reason. Attempting to follow such procedures without use of a thermometer and/or any specified temperature control mechanisms is asking for failure at best, injury or death at worst.

The procedures described on this site are often inherrantly dangerous. If you do not understand the procedures and the principals underlying them fully, you should not attempt them. Your post demonstrates your lack of a full understanding of the procedure you attempted. You will do well to study more carefully any such operations you may consider undertaking as your health and survival are on the line. Luck is not a dependable survival mechanism...

FinnBell

May 4th, 2004, 01:54 PM

Okay, first of all, I know I messed up with the whole water into acid thing but with everything else I did follow directions. I added the water to the acid because it was soo thick it wouldnt pour out of the container. I didnt use a thermometer for the addition of the kno3 because it doesnt actually say to. It says add the kno3 and cool it. During the addition of the Erythritol however I DID use a thermometer. And I controlled the temperature just as said in Axts method. So as far as temperatures, times and additions I did everything right. Now Im not trying to be disrespectful at all to you Bert, Im just trying to be clear. (and yes I do have proper protection ie. gloves goggles etc.) I know I was very vague on my description on my attempted synthesis and for that I apologize. I do however appreciate your criticism. I also find axt synthesis sort of vague as well. Is the mixtures supposed to be cooled DURING the addition of the KNO3, or add the KNO3 THEN cool? Because it says "add the kno3 and cool"

Boomer

May 5th, 2004, 12:48 PM

I never cool during the addition of the nitrate. If you start at room temp, using e.g. 300ml SA and 200g AN, it gets to about 60-65C and dissolves fast. Just don't let it get so hot that the NA starts to distill off, and cover the vessel with aluminium foil after addition!

It is especially good if you need the mix for distilling NA, you save a lot of cooling and re-heating. If you need it for a nitration (nitric esters), you have to cool it down anyway. I put it in the freezer over night, it gets the mix down to -25C on the coldest setting. This is good, as you can add A LOT of glycerine / erythritol / mannitol before it even comes close to the 15-20C limit and you have to cool it back.

Starting at this starting temperature, you can even dump the glycerine in, in two portions, without watching the temp. Due to the thermal mass it simply CANNOT jump up 55C from each addition. No need to say that you have to stirr/shake/swirl like hell to avoid hot spots, and that you will probably DO watch the temp, at least put a hand on the vessel to know whether it is still cooler than the room. :D

With mannitol, I always add it ALL AT ONCE, shake well and put it back in the freezer. At -25C the mannitol disolves so slowly, and is therefore nitrated over HOURS, that you hardly feel the temperature rise at all. Just shake it every hour and leave it cold for 1-2 days, then dump in a bucket of water. Yield is 50-60%, and work is little without long stirring, making an ice bath etc.

Do NOT try this while starting from a warmer temp. If ALL the mannitol is added at once, the runaway starts at ZERO C, not at +30C! I once let it come up to about 0C before putting it back in the freezer. It still felt OK, did not seem to get warmer, but 30 minutes later my kitchen was full of orange fumes, and the content of my fridge poisoned. :o

I do not know how fast erythritol dissolves, so maybe this method is not good for ETN. But it is worth a test, for the time saving is great. Just don't use your mothers fridge! :p

FinnBell

May 5th, 2004, 02:07 PM

That definitely is a good way to do things sometimes. I usually do that with my acetone peroxide synthesis. I put it in my little fridge in my room and it gets so cold its almost frozen but not quite. So when I add the acid I can add it all at once and the temperature doesnt rise fast enough to make a difference. Although with ETN, I do the same thing with the H2S04 KNO3 mixture, and it gets very cold but when I add the eythritol I can only add about4 grams before I can start to feel it actually warm up. It doesnt get hot, but I think it would if I added any more. During the nitrate addition to the S2H04 I keep that very cool as well and it gives me much better yeilds. My first attempt with ETN I didnt cool during the nitrate addition and I only got like 6 or 7 grams but when I cooled through the entire synthesis I got like 20 grams. Still not the best yield, but much much better.

dave

May 6th, 2004, 08:08 PM

I just received my Erythritol to day. I then proceeded to manufacture ETN. All i can say is this is the best explosive i have synthisized so far. I knew this was just a test run and i kept the temperature at 15c. After i finished the process I ended up with brownish looking powder in my filter. I took a tiny amount and lit it with my torch.

I was thinking that it probably didn't work out cause I used drain cleaner acid without even concentrationg it first. It melted quite quickly and I thought, Wow it melted like ETN is suppose to. Next after it solidified it was a clear solid and so I decided to give it a good hard whack with a hammer. It then went POW.

Sweet this is the best explosive I ever synthisized. Very simple, the nitration was done in a very slipshod manner and I still worked. Unlike NG the temperature was very easy to regulate. Now all I have to do is let it dry. I nitrated about 8g of erythritol. The yield seems very nice.

FinnBell

May 9th, 2004, 05:38 PM

I just synthesized a small batch of ETN by Axt method. There is relatively very little posted on the forum about this explosive so I figured I would take pictures of my nitration. The pictures are here. ETN SYNTHESIS (http://hometown.aol.com/MrPapaGeorgio36/ETNnitration/ )THey are in order by numbers, with the exception of the yield picture. Note:that is only part of the final yield. I skipped a few steps, like washing, filtering, and weighing but it should be okay.
The pictures were way too big to put directly on the post so I just linked them. I dont know how to resize the images yet but I'll figure it out soon. Sorry 56kers.

atlas#11

May 10th, 2004, 01:09 PM

I did another somewhat larger batch and got about 70g which is ok for the 45g of erythritol used. I will cast it with some other equaly larger batches and use the charge to refrack my dads well later on this week. This explosive beats the hell out of picric acid, A. it is more easly castable, B. it is much less toxic, and C. it is about 70% more powerfull.

In the future however, I will probably use xylitol as it is avalible in 3lb bags at the vitamin cottage for 11USD, and would be easier to decant because of higher density. Plus PNX sounds cool :cool: .

FinnBell

May 10th, 2004, 08:16 PM

For some reason,whenver I synthesize ETN, I usually dont get very good yields, if I try to make a bigger batch, it seems like the bigger the batch, the lower the yield. When I made a batch and used 15 grams of erythritol I got back around 20 but when I used 30 grams of erythritol in another batch, I got back even less. I dont know what thats all about. The only thing I think it might be is my acid. I use Rooto drain opener. Maybe I should purify it first. But yeah, ETN is definitly good stuff. VERY easy to cast.

Spleenman

May 10th, 2004, 09:01 PM

After calling some local health food stores, it seem I have no OTC source of erythritol. I can, however, obtain xylitol for around $4/lb., and will be trying this synth as soon as I get a chance to take a shopping trip. Just out of curiosity, does anyone know what the VoD or OB of xylitol pentanitrate is? BTW, wouldn't the acronym be XPN (Xylitol PentaNitrate) not PNX?

blindreeper

May 11th, 2004, 08:35 AM

Yes it would be XPN. Has anyone tried setting of ETN with LS from primers and how much is needed? These would make awsome caps in small Al tubes (6mm) :)

Bert

May 11th, 2004, 11:11 AM

Has anyone tried setting of ETN with LS from primers
SWIM tried it. 300 mg of LS based priming compound removed from .22 LR shells and compacted with hand pressure only onto a 5mm Dia. column of compressed ETN was reported to rupture the capsule in the area of the LS, and leave the majority of the ETN unaffected in the remains of the capsule. The procedure of collecting the LS mix was so tedious, no higher amounts were attempted.

A careful reading of the Lead styphnate thread (http://www.roguesci.org/theforum/showthread.php?t=386&highlight=lead+styphnate) will reveal the unsuitability of LS as a stand alone primary for BC use, and its suitability as an igniter for OTHER less flame sensitive primaries... Most commonly Lead azide.

atlas#11

May 11th, 2004, 01:06 PM

FinnBell, How long do you let it react? I find that the longer it reacts the more I get. Unfortunatly my only thermometer was broken about a week ago so I cant tell you what temp mine reacted at. With 190g ammonium nitrate and 300ml H2SO4 and 45g erythritol my batch was slightly thinner that freshly mixed concrete. My yeild was about 70g, I weighed it when not completly dry and lost about 3-4g during washing.

It's not your acid, I use the same stuff right out of the jug. Where do you get your nitrate from? Mine is from instant cold packs, that is, until I convince my parents that I need a 50lb bag, then i'll be making bangs for a long time.

For xpn, I assume that the procedure would be about the same except for needing more nitrate, and in effect more h2SO4. I didn't know that the order was important in the acronym, please fill me in on that one.

FinnBell

May 11th, 2004, 02:37 PM

When I synthesize ETN I use very finely powdered KNO3. I got it from a pyro supplier so I know its good stuff. To tell you the truth Ive never even tried using ammonium nitrate. I have a bunch of that stuff too. One day just decided to buy like ten packs of it at Wal Mart. (Made up some BS story to the cashier about it being for my football team.) But I didnt think the KN03 and ammonium nitrate would make that big a difference. I know its not temp. I keep it at a steady 18*C pretty much the whole time. (I just broke my theremometer last night too though) Second time that happened.

Bert

May 11th, 2004, 02:45 PM

(I just broke my theremometer last night too though) Second time that happened.

Jeez, you guys are sure hard on your lab thermometers (http://www.sciplus.com/category.cfm?subsection=4&category=44)

FinnBell

May 11th, 2004, 03:10 PM

Holy crap thanks Bert! Those prices are nice. 3.50 for a lab thermometer. Dont laugh but I paid 15 bucks for my last thermometer. Oh and by the way atlas I usually let it react for about 30 mins. On axts method it says 15 mins but that seems too short.

Spleenman

May 12th, 2004, 04:58 PM

First attempt at making xpn failed completely...I used Santeen S-T drain opener acid, NH4NO3, and granulated xylitol. Though I only let it react for 15 minutes as stated in the synth, I would think that, even if it isn't long enough, I would have at least gotten measureable yields. Since I observed that the xylitol didn't seem to dissolve in the nitration mix very much, I am wondering if perhaps the large particle size prevented most of the xylitol from being nitrated. I will try again with finely ground xylitol and let it react for 30 minutes, and if that fails, I must assume the drain opener acid is to blame.

atlas#11

May 12th, 2004, 05:02 PM

I was doing a batch of hmtd and it snowed over the beaker and all. It was killed with a snow shovel. Next time, I'll bring it in with me. What I'm really bad with is those glass stirrers. Shit, I must have broken a dozen of them in the first week, I think their cursed.

Use ammonium nitrate, it is easier to stir. I never even grind the prills as they disolve slowly enough to prevent boiling off the nitric. The key is stiring, If you sit their and stir it for an hour as you add the erythritol slowly then you will get much better yeilds. If you have a magnetic stirrer then use it. I've got nothing better to do, just pull up a lawn chair and relax, (except for the carpotunnel which will set in after your third or fourth batch, you'll be fine! :rolleyes: ).

Rosco Bodine

May 16th, 2004, 12:41 AM

There are several other of the polyols , or "sugar alcohols"
which should be interesting candidates for nitration experiments .

Dulcitol Hexanitrate , mp 94-95 C , has been mentioned in the literature .

Xylitol Pentanitrate is obscure enough that I can't find any reference for it .

Maltitol Nonanitrate ( Nine nitro groups ! ) No references either .
Here's a structure for maltitol . Looks thirsty for nitro groups to me .

http://apps3.fao.org/jecfa/additive_specs/docs/4/additive-0626.htm

Anybody know of any references or done any experiments with these ?

Spleenman

May 16th, 2004, 07:17 PM

Second attempt using Sorbitol ground to the consistency of flour, and reacted for a little over one hour also gave me nonexistant yields. I am now almost certain the acid is to blame. I will attempt to locate a source of better H2SO4 (Such as this "Liquid Fire" I have read about), and try again.

FinnBell

May 16th, 2004, 08:24 PM

Oh for sure, liquid fire is the shit. I think its like 90 something percent pure. Works great for everything I use it for. I get it from Ace. Rooto is also good stuff, comes in a white bottle. Very clear, seems to be quite pure.

atlas#11

May 19th, 2004, 11:03 AM

Spleenman, I suggest more time for nitrations. Your acid is more than likely a major contributor to your problem but if it says it contains concentrated H2SO4 then you would get a yeild just not a very good one. Let it react for an hour at least. The colder the temp. the slower the reaction, raising the temp is dangerous but increasing the time only risks your yeild and not your health.

Edit: on my last post I was talking about my thermometer. For some reason it won't let me edit that post.

FinnBell

May 19th, 2004, 02:01 PM

I thought increasing nitration time gives you better yields :confused: Axt method says to let it react for 15 mins and I usually let it react for about half an hour and sometimes more, and it seems to give me pretty good yeilds.

nbk2000

May 20th, 2004, 08:28 PM

Timing is everything.

Let the stuff sit in acid too long and it can hydrolyze into crap-ola. :(

Boomer

May 25th, 2004, 06:22 AM

Timing is everything.

Let the stuff sit in acid too long and it can hydrolyze into crap-ola. :(

What nitrations are you referring to? According to Escales, the "esterification" is reversible, meaning the nitrate ester is formed while at the same time the reverse reaction takes place. He (and some of my other sources like Stettbacher, Kast, K+M, COPAE etc) mentions that the spent acid even gives off some more product over the next week or so (after the immediate yield was separated and processed), and that people used to pump the NG off through the top of conical tanks every day for some time before acid recovery. He also says to avoid NG from forming after separation, a few percent water should be added.

I experienced the same, even if leaving the top layer in the (tall) beaker, the amount increased approx. 10% between one hour and one day after the end of glycerine addition (at 10C in the fridge). More time did not improve the yield further for NG, but for solid esters:

I made some tests with MHN, under exactly the same conditions, using the nitrate method, and got a crappy yield of 25% after one hour, 45% after a day, and 55% after three days at –20C. For more info see my posts in “MHN yield”.

I fully agree with you saying “… hydrolyze into crap” as soon as water is added (see above), and maybe also if the acid is too weak, which I never tried (using distilled NA).
The perfect spent acid is 70% SA, 15% NA and 15% water (Escales), at 10C it dissolves approx. 3% product, 2% recoverably dissolved, 1% decomposed (numbers IIRC). It can form more NG, especially on cooling, up to approx. 70% SA, 11% NA and 19% water. Adding 20% more water can destroy the complete yield if you start with a 2:1 mix of drain cleaner + boiled down NA (65%).

I guess this is one reason why beginners get low yields: They dump the mix into MUCH too little water. I remember one saying “it heated up a lot and gave off some yellow gas” ! Why use so little water, when one litre dissolves less than a ml NG, a 10l bucket less than a gram PETN.

Rosco Bodine

May 26th, 2004, 01:27 PM

Knowing few references are available related to ETN ,
there is another patent which so far as I know has not
yet been mentioned .

US1744693 describes the use of ETN in detonators , ect .

The above patent is a followup to the earlier patent

US1691954

I noticed the application date for this '954 DuPont patent seems coincidental ,
within two weeks of a Nobel patent filed in Britain ,

GB297853 see example 3 , detonator using cast loaded ETN .

Even given the expense of the precursor erythritol seventy-five years ago ,
it says something positive for an explosive that both DuPont and Nobel
would simultaneously be trying to secure a patent within days of each other
on opposite sides of the Atlantic , for an explosive which at the time was
not yet commercially feasible .

Bert

May 26th, 2004, 02:57 PM

Even given the expense of the precursor erythritol seventy-five years ago ,
it says something positive for an explosive that both DuPont and Nobel
would simultaneously be trying to secure a patent within days of each other
on opposite sides of the Atlantic , for an explosive which at the time was
not yet commercially feasible .

Of particular interest is his example of a cast base charge of ETN-

500 mg of cast ETN with 30 mg of Lead azo clathrate hand pressed.
Witness plates are .020" T-1 (soft) Aluminum, 4" X 4" squares.
Scale in inches.

nbk2000

May 26th, 2004, 05:38 PM

Bert, when posting such pictures, please include information on what the target material is made of, thickness, etc.

Glad to see you included a scale, but is it inches or centimeters? I'm assuming that, as an american, you're not using the poxed metric, but good ol' imperial, correct? ;)

JoeJablomy

May 26th, 2004, 07:43 PM

Just look at the divisions: if they're decimal (ten short lines between each space in the long ones), it's probably metric; if it's divided into halves, quarters, eigths, etc., it's almost certainly in inches, as in the picture.

+++++++++++

Best to never assume anything. NBK

0EZ0

May 27th, 2004, 01:18 AM

I must ask Bert, is that a sheet of roofing aluminium that you used as the witness plate;)? I have heard that it is very useful for testing the performance of an explosive charge in small amounts. I may have a picture that looks similar to yours somewhere... Albeit not as impressive.

May I ask as to the origin of the charge casing you used? Indentations such as seen in the picture suggest that it was of a soft nature such as plastic or paper or simply that the charge was case less. Of course this is just my personal assumption. I would never have carried out such a test, myself.

(Edit) Did the aluminium come on a roll? Copper you say, it does show the same effects with high end VoD explosives. It does exhibit some intriguing properties under high stress(think EFP's and SC's). Apart from using a varnish or Nitrocellulose film, you may wish to consider electroplating a less reactive metal onto those cases if you feel they are unsafe as they are.

Yes, I am quite aware of the various tests used to categorize the performance of energetic materials. The 1x85x85mm Aluminium witness plate in the attachment was subjected to <200mg TATP hand pressed near 1g/cc. in a standard .22 caliber brass shell electrically fired in a blast-proof enclosure without a primary pyrotechnic initiator. The test was not carried out by myself so I only have limited information on the results. I was told it was part of series of experiments to see the breaching effects of detonation in a pressurized submerged container (rather nifty crushing effect:)). (Edit/)

Bert

May 27th, 2004, 01:51 AM

The soft Aluminum is a general purpose item, sold in a local hardware store. Witness plates are a classic testing method for caps, see COPAE for more information. The cap had a metal case. (http://www.roguesci.org/theforum/showthread.php?t=3601&highlight=capsule)

Rosco Bodine

May 30th, 2004, 11:26 AM

Of particular interest is his example of a cast base charge of ETN-

500 mg of cast ETN with 30 mg of Lead azo clathrate hand pressed.
Witness plates are .020" T-1 (soft) Aluminum, 4" X 4" squares.
Scale in inches.

That is a fine example of what good results can be achieved by
a combination of materials which work well together . Caps using
that particular loading of materials are very interesting indeed .
High grade detonators are the result of a method requiring no
elaborate loading press . That is a real advantage .

By using a metallic capsule , you needed a much smaller amount of
initiator , compared with the amount of initiator required if a plastic
casing is used . ETN used alone as a base charge is something which
I never even tested . For some reason I simply considered its value
in terms of a meltable binder for other energetic materials used as a
filler . But evidently , the ETN is quite a good base charge all by itself ,
and more sensitive to intiation than its composites with other materials .

According to the patent , the ETN is sensitive enough to initiation ,
that even a relatively mild initiator like mercury fulminate can be used
without requiring a reenforcing cap for extra confinement . So , a
very good cap could be made using ETN and mercury fulminate , for
those who may have no access to the precursors or tools for making
the azo-clathrate . Whether a "hand pressed" initiator of mercury fulminate
would fare as well as the azo-clathrate is unproven , but probably using
a somewhat larger amount of fulminate , it would work as well , without
requiring any extreme pin pressure for loading . Of course a cap using
mercury fulminate for the primary would not have the decades long
storage life that would be the advantage for the azo-clathrate , but
for shorter term storage life it would be more improvisable and still
retain reasonable safety and practicality for more near term use .

A word for the inexperienced concerning "hand pressing" of initiators .
Realizing that only "hand pressed" initiators are adequate for an ETN base
charge , there is a temptation for people to *avoid* actually using their
hands as the loading fixture , but for safety to use a loading jig for
keeping hands at a safe distance during compression of the primary and
removal of the ram , be it a wooden dowel or metal rod . Understanding
that by the term "hand pressed" it is meant that no great mechanical
advantage compression loading is required , not to recommend that
bare hands should be used as the loading fixture itself . A new block
of wood can easily be replaced if an accident should ever occur ,
but a hand is another matter entirely . When I think of these type
combinations that can be effective when "hand pressed" , I usually
think in terms of a simple loading fixture based on a caulking gun ,
or a wooden box with a hole drilled through a block of wood and
a dowel or a metal rod going through it to a "capsule holder" inside ,
as contrasted with an arbor press or a hydraulic press using
shielded fixtures which are more elaborate and develop great
mechanical force to accomplish high loading pressures .

nbk2000

June 1st, 2004, 12:45 PM

When using a dowel to hand-press, you hold it with your palm parallel to the dowel, with the free end sticking out of your hand, not pressing down on it with your palm.

This way, if (when) the primary goes off and launches the dowel out of the loading block like a bullet, your hand doesn't get skewered by it. :eek:

pdb

June 2nd, 2004, 06:16 AM

To come back on Axt's genuine synthesis method that started this thread, I find it a bit "costly" in H2SO4 96%, with on top of that a mediocre yield: 184g SA for a 25g crop...

I guess ETN can be prepared also with HNO3 100% only, in a way similar to PETN. But it's pretty costly as well, given the excess in acid required to keep concentration high enough.

However, looking for making a more balanced use of my acids, I would favor a method using H2SO4 AND HNO3 (100% or diluated), as Blaster did for PETN. Somebody on this forum wrote earlier that the yield was inferior to the Axt's method, which I somewhat doubt.

Has anyone really experimented with mixed acids ? If so, can we get the details ? Thanks.

Rosco Bodine

June 2nd, 2004, 10:31 AM

The identical method as using straight nitric acid was used
by me in side by side comparison for PETN and ETN , and
while the yield for PETN was extremely high >98 % , the yield
for ETN using the exact same molecular proportions and conditions
was *very poor * on the order of a third the yield of PETN .

The difference that I noticed is that when pentaerythritol is added
in small portions to well stirred HNO3 d. 1.5 containing about
a half per cent of urea nitrate , the PETN precipitates from the acid
as it forms , until the mixture is thick with crystals and difficult
to stir . When erythritol is nitrated under the same conditions ,
the ETN being produced remains dissolved in the nitric acid ,
until the acid is saturated with dissolved ETN and that establishes
an endpoint for the nitration by an unfavorable equilibrium due
to the dissolved end product . Until I drowned the mixture , I expected
that a similar amount of ETN would be obtained when it dropped out
of solution , but that was wishful thinking . It became clear that
for ETN yields to be improved , that sulfuric acid was going to be needed
as part of the nitration process in order to decrease the ETN solubility
and cause it to precipitate from the nitration mixture . In what order
of addition it is most efficient to do the addition of sulfuric I do not know ,
having done no further experiments .

Before Axt described the method of using solid KNO3 with sulfuric acid ,
I also experimented with a similar method , but using NH4NO3 as the nitrate
in experiments to produce both PETN and ETN . The yields for PETN
were poor as compared with the method using straight nitric acid d 1.5 ,
on the order of 65 % yield versus 98 % for the nitric acid method .
The yield for ETN was much lower than for PETN , but was however
a better yield than obtained using the straight nitric acid method .

The method I used was to first dissolve the polyhydric alcohol precursor
in the 92.5 % sulfuric acid and then add the solid nitrate in small portions
to the well stirred mixture , while monitoring the temperature of the mixture .

The yield for such nitrations has always been significantly lower using
NH4NO3 as the nitrate , than using sodium or potassium nitrates , even
though the mixture is thinner and easier to stir using the NH4NO3 .
Here again , I would theorize that the solubility is unfavorable for the
efficiency of the reaction , by shifting the reaction equilibrium in the wrong
direction , but in this case it is the solubility of the acid sulfate byproduct
which is the culprit .

Conclusions from these experiments are that ETN is more fickle about
nitration conditions than is PETN . Sulfuric acid is needed for the ETN
to be produced in decent yield . And *alkali* nitrates will produce a better
yield if the nitrate / sulfuric method is used for either PETN or ETN ,
than will be obtained using NH4NO3 as the nitrate .

I did not test the method of adding the polyhydric alcohol in small portions
to the already mixed nitrate / sulfuric nitration mixture . There may be
a difference by the order of addition which could be applied there ,
for the polyhydric alcohol to not be sulfonated in advance of nitration .

It is evident however that the strategy which is best for one polyhydric
alcohol nitration is not necessarily the best method for a different polyhydric
alcohol , as is plainly the case for PETN and ETN .

pdb

June 2nd, 2004, 12:16 PM

Rosco, as always, your reply is of great interest.

In Axt's method, about 16ml out of 100ml H2SO4 serve to generate nitric acid from the 60g KNO3; have you ever tried to substitude 25 ml HNO3 d1.5 to the [16ml H2SO4, 60g KNO3] combinaison ? i.e. 84ml H2SO4, 25ml HNO3 and 15g erythrol ?

Did you experiment enough to confirm that the proportions mentioned by Axt are the best ? I still have the feeling H2SO4 is in excess, compared for example to NG synthesis.

pdb

June 2nd, 2004, 12:18 PM

Rosco, as always, your reply is of great interest.

In Axt's method, about 16ml out of 100ml H2SO4 serve to generate nitric acid from the 60g KNO3; have you ever tried to substitute 25 ml HNO3 d1.5 to the [16ml H2SO4, 60g KNO3] combinaison ? i.e. 84ml H2SO4, 25ml HNO3 and 15g erythritol ?

Did you have a chance to experiment enough to confirm that the proportions mentioned by Axt are the best ? I still have the feeling H2SO4 is in excess, compared for example to NG synthesis.

Rosco Bodine

June 2nd, 2004, 01:51 PM

All the experimenting I did is what I already described .
From working with various nitrations I have found that
for each nitration of a specific material there is a "sweet spot"
concerning the economics of the nitration , and another
"sweet spot" regarding maximum yield from the precursor ,
and perhaps yet another optimum reaction condition as
regards the purity of the product . So it depends upon
what is the most desired result what choice of materials and
method will be used , to achieve what is defined as "optimum"
results . You have to experiment and chart the results to
arrive at what you consider the "best" method of synthesis .

Jetex Kid

June 2nd, 2004, 06:32 PM

In Axt's method, about 16ml out of 100ml H2SO4 serve to generate nitric acid from the 60g KNO3; have you ever tried to substitute 25 ml HNO3 d1.5 to the [16ml H2SO4, 60g KNO3] combinaison ? i.e. 84ml H2SO4, 25ml HNO3 and 15g erythritol ?

My calculations indicate that you assume the following reaction:
2KNO3 + H2SO4 = K2SO4 + 2 HNO3
I used to make that mistake. :D

The prevalent reaction is:
KNO3 + H2SO4 = KHSO4 + HNO3

If you use NaNO3, something like 25% of the reaction will be the first reaction.

2,4,6-TNP

September 26th, 2004, 03:45 PM

I have a question about this topic.

The melting point of ETN has been given 61C or 141.8F I was trying to discern the safest method and also the most uniform method of casting the ETN into the 6mm Aluminum tubing I'm using. I was thinking that I might crimp an end, pour in the correct amount of powdered ETN and then apply the cap to hot water or hot oil bath to melt the ETN. Is this safe? I could try to melt the ETN and then pour it into the tube but I think it will stick to the sides and won't be very uniform. When I have acomplished this I will use straight Lead azide atop the cast ETN. I will use a mixture of 35% straight lead azide and 65% sodium nitrate and powdered sugar for an ignition mixture. I do plan eventually to make some basic Lead picrate and just use a similar mixture for an ignition mixture, but this should work for now. I think the basic Lead Picrate 65%/Straight Lead Azide 35% mixture atop Staight lead Azide atop cast ETN in a 6mm Aluminum tube will make a cap that should be as storage stable for long periods of time as the azo clathrate would be. Anyway any ideas about the casting of ETN?

Thanks

Also for my reaction I have been using Sodium nitrate(17% less than Axt's potassium nitrate but the same amount of Rooto drain cleaner and a granulated form of erythritol. First I ground the Erythritol into a powdered sugar consistancy but soon learned that leaving it granular works the best. Yeild not as good as axt's but I may need to react mixture longer before precipitating. I tried mixing the sulfuric acid and sodium nitrate together then adding the erythritol and also I tried sulfinating it first. It didn't make much difference in yield but the average reaction temperature changed a bit which may have led to a slightly lower yield. Has anyone gotten the best yield with a particular nitrate salt? Is ammonium Nitrate any better than sodium?

Sir Dudalot

September 26th, 2004, 10:20 PM

Anytime I cast ETN I just filled up the desired container with ETN then put it in hot water to melt. I just microwave the water until it's boiling then wait about a minute and put the powdered ETN/container in the water bath to melt. I come back in about thirty minutes and it's cast and hardened. I suspect some decomposition however because the resulting cast block smells like nitric acid vapors. Perhaps a lower casting temperature would correct this problem (if it's major enough to worry about).

September 27th, 2004, 12:38 AM

Has anyone gotten the best yield with a particular nitrate salt? Is ammonium Nitrate any better than sodium?

Sodium nitrate in H2SO4 can leave some insoluble precipitates which can become annoying. KNO3 does not leave too much, but ammonium nitrate seems to be the best as far as that problem.

I don't know specifically what will happen as per the reaction with erythritol though, but in regards to the matter of precipitates there it is.

pdb

September 27th, 2004, 10:23 AM

2,4,6-TNP: I have conducted tests in 6mm Al tubes (real deto cases), by filling with 1g ETN in granular form and then melting it in hot water. The problem is that such caps are by far much weaker than the 0.8g PETN ones, possibly because of a greater critical diameter with ETN. As Rosco Bodine reported it earlier, ETN and PETN demonstrate similar strengths beyond a minimal amount only, which he suspects to be aroud 2g IIRC, which in too much to fill a standard cap. This is why somes on this forum have undertaken trials with mix ETN/PETN amounts. For my part, the results have not been convincing so far: it doesn't beat the traditional compressed PETN charge...

Boomer

September 27th, 2004, 12:03 PM

I guess the low power of cast ETN detonators is due to them detonating at the low end of their VoD range.

I remember using NG-plasticised MHN with a small primary charge, taped to a test plate and buried under soil for noise reduction. It created by far the biggest under-earth chamber of all tested cap, but also by far the smallest dent on the plate (the caps with compressed MHN powder had sometimes even shredded the plate). This shows the heaving power of low VoD.

This is the same effect seen with aged/clear blasting gelatine, which goes at 1500 m/s instead of 8000 m/s for fresh/milky gelatine. It misses micro gas bubbles (or crystal surfaces in case of the ETN) to propagate detonation.

So casting or melting the base charge into the cap defies the purpose of increasing VoD through increased density. Perhaps casting the lower section, and pressing some on top would help. But then you could as well compress the first half amount with a vice to near crystal density, put the rest on top at approx. 1.5 g/ccm, and add a little hand compressed stuff beneath the primary. This is what works for me all the time.
And believe me, the power increase against hand pressed base charges is incredible. I posted a photo of a steel pipe, which was only slightly dented versa partially shredded using the same amount, hand compressed at 500 PSI versa vice compressed at 20000 PSI (IIRC). Cannot find the thread though, could have been archived. :confused:

BTW I would bet money that (at least small diameter) MHN caps are stronger than PETN caps, because MHN has a lower critical diameter, and better self-acceleration. It will go at 8000+ m/s where PETN still needs bigger columns. Plus, you safe primaries, and get EBWs easier to work.

Microtek

September 29th, 2004, 09:41 AM

According to one of the big ones ( I can't remember if it was Davis or Urbanski or someone else ) PETN detonates at almost maximal velocity ( > 7000 m/s ) regardless of diameter ( < 1 mm ) or confinement ( paper ). I'm sure MHN does also...

Rosco Bodine

September 29th, 2004, 01:10 PM

Crystalline form and particle size and the density of the charge
has a very significant effect on the sensitivity and output for
any charge , and it becomes more noticeable for small charges
where the dimensions and distances are limiting , requiring very
quick accellerations of the detonation through the small charges
to achieve the most complete and instantaneous release of energy .

Small crystalline size is desirable to a lower limit where a decrease
in density makes any smaller particle size counterproductive . The
advantage of small crystals is easier initiation and better propogation
in small diameter , at higher velocity . Cast charges may benefit
from crystal modification as occurs with some eutectics , which
deposit a finer grained crystalline structure upon solidification .
95 ETN / 5 PETN is a eutectic mentioned in PATR .

Composite cast charges which consist of a desirable small crystalline
filler slurried in a molten matrix , can provide very high output , but
can also be *much* harder to initiate at the high output velocity which
they are capable . The absence of occluded air between particles
which would be present in a compressed particulate charge , deprives
the charge column of the sensitizing effect of those internal "hot spots"
which would occur when such air pockets are compressed and heated
by a detonation wave . It is for this reason that blocks of cast TNT or
cast Picric Acid cannot be detonated by a cap , but must be detonated
by an intermediate booster of compressed crystalline TNT or PA which
is cap sensitive .

For much more senstive materials like ETN , it is possible to intitiate
the cast material directly , but my own observation of an ETN / PETN
composite is that there is a possibility of a feeble low order detonation
if the amount of initiator used is not greatly increased beyond what would
be needed for a compressed particulate charge having occluded air .
In that regard , the comparison of an ETN cast does compare well with
blasting gelatine . My experiments with this phenomena are not extensive ,
but this was my observation in preliminary experiments . The key to
getting the cast composite to positively go "high order" was to "hit it
with a bigger hammer" , and using a large excess of initiator produced
the desired effect . If using the minimum amount of intitator is your
goal , then you don't want to be attempting to directly intitate a cast
charge . An intermediate layer of the compressed particulate charge
atop the cast charge would be a good design strategy .

As to what degree a cast charge is more difficult to initiate , well it
depends upon the material or materials involved and the crystalline
size , and the column diameter and confinement . But the effect
is sufficiently great that some explosives ordinarily not considered
insensitive enough for safe use in artillery shells for example ,
if used in pure crystalline form as a compressed charge , may be used
in composites where that sensitivity is reduced in melts or plastiques
or colloids based on the same explosive .

The literature describes ETN based caps as being powerful , about as good
for the purpose as alternatives . That is probably true for an ETN cap
whether the material is cast or pressed , alone or as part of a composite .
Experiments and tests can be performed to reveal what is optimum for
the design of detonators using ETN in various forms , the same as is true
for other energetic materials . There are likely several different configurations
which will be found to consistently give good results . My own interest
in ETN tends to remain primarily upon its usefulness as a fusible energetic
matrix in composites . I look forward to testing ETN as a melt binder
for RDX and also for inositol hexanitrate , and possibly other polyol nitrates ,
where possible eutectics or composites having useful properties may be
found . The nitrates of lactitol and maltitol are two which seem good
prospects for experimentation . Cyclodextrin , resistant maltodextrin ,
inulin , microcrystalline cellulose , agar , and hemicellulose are other materials
which may produce nitrates which could form useful compositions with
ETN . There are a great many experiments which are possible with ETN .

yarrak

January 10th, 2005, 03:19 PM

There is a drug called Danitrin. There is 20 mg Pentaeritritol tetranitrate and 200 mg Meprobamat in each tablette. I wonder if I can make use of this drug. Any ideas?

pdb

January 13th, 2005, 05:17 AM

Boomer: subsequent testing of various caps solutions, all using ETN/PETN mixtures, did not lead to a satisfacting process. As Rosco stated, I could observe a better brisance, thanks to higher VoD, when doubling or tripling the primary charge (DPNA). However, my conclusion is that it will not beat the traditionnal pressed-PETN detonators. I am therefore back to square one, as I started ETN experiments in order to avoid the incertainty related to detonators' performance due to dispersion in obtained HE densities because of use of improvised press tools. BTW, didn't you open a thread about in-house press devices (can't remember if it was someone else) ? What mechanical device did you design to press your detonators ?

Boomer

January 13th, 2005, 08:00 AM

That was not me, but I remember it. I made a similar press, but even simpler: Two 2x4s and a door hinge, plus a hole in each 2x4 for cap/dowel. Just to get hands+face some feet away. Also useful for AP crackers! For metal caps I stand behind a corner.

About density differences: I found it varies very little once you get to 10 kPSI. When I use my vice, which is capable of 60000 PSI, it turned out that above 15000 PSI density stays constant, instead the metal pipe expands! For soft, "smeary" crystals like MHN this is already near crystal density anyway, approx. 1.7 g/ccm or a little above (hard to calculate from v = 1 +/- 0.05 ccm and m = 1.7 +/- 0.05g).

A way to get it reproducable is to measure the torque on the vice (by pulling with a spring). For the lever press it is even more simple: Step on a scale and press until you loose xy pounds. Then calculate PSI from the length ration and dowel area. Or you put a known amount in each cap, then press to a mark on the dowel. Add the next amount and press to the second mark ...

pdb

January 13th, 2005, 11:09 AM

I agree that beyond a certain pressure level, which depends on HE and its crystals size, it is useless to appy even more pressure for amateurism needs.

So far, I have been using a wooden stick as a dowel and a standard desk vice. But the cap not being surrounded in a strong cylinder, its would start twisting when a few tenths of Kg/cm2 only are applied. The alternatives would be to switch to stronger pipes iso real deto cases, or to complexify the device in order to avoid early deformation. I'm not enthusiastic about any of them...

nbk2000

January 13th, 2005, 03:31 PM

The article on ETN from "Preparatory Manual of Explosives".

pdb

January 24th, 2005, 07:27 AM

That was not me, but I remember it. I made a similar press, but even simpler: Two 2x4s and a door hinge, plus a hole in each 2x4 for cap/dowel.

Can you be more specific about how the cap is held while you pull out the dowel after compression ? I have tried several gripping systems without finding a really satisfying one. Best would be to insert the cap in a metal cylinder made of two half-cylinders (along longitudinal axis). When the cap is pressed, it would twist and thus adhere strongly to the cylinder, allowing dowel to come out when pulled. Then the cap would be retrieved by separating the two half-cylinders...

detcord77

February 19th, 2005, 12:21 PM

pdb

February 20th, 2005, 06:16 PM

Can you help me with finding a OTC source for erythritol in Europe (mainland),maybe a web supplyer of special sugars, because i can only find such a dealer in the U.S. and the shipment costs a lot. Thanks for the help.

I didn t find any, and ordered from the US. Conversely, mannitol is available in pharmacies under the brand name Manicol.

detcord77

February 21st, 2005, 05:39 AM

And if you know, what is the use of Manicol (is it an artificial sugar for diabetics or what), will they ask unpleasant questions if i try to purchase it :) ? Do you think that they sell this sugar in all of the pharmacies in Europe, or just specificly like in France, UK,.... Sorry because of the slight off topic question...

trinitride3

March 6th, 2005, 12:50 PM

I was wondering if anyone could give me an idea of the optimal nitration mixture for erythritol using 70% HNO3 and 96% H2SO4. I searched the entire site and all of the web but couldn't find a (conclusive) ratio for the mixed acid nitration of erythritol.

pdb

June 30th, 2005, 11:51 AM

pdb

June 30th, 2005, 11:51 AM

FUTI

June 30th, 2005, 04:47 PM

can erythritol be made by reduction of tartaric acid?

FUTI

June 30th, 2005, 04:47 PM

can erythritol be made by reduction of tartaric acid?

Jetex Kid

June 30th, 2005, 06:59 PM

Although kept in total darkness in a cool place, the bottle of ETN prepared about six months ago is full with NO2... Looking back at my preparation notes, I recall that I precipitated it from bicarbonated acetone twice. My feeling is that residual HNO3 is far more difficult to remove than with PETN.

At one time I believed that ETN was the answer to all my explosive needs. Erythritol is inexpensive and readily available in the US. The tetranitrate is very powerful, sufficiently insensitive, easy to make, and efficient in its use of precursors.

So it is disappointing to me to hear that ETN is unstable. Instability seems to be the fatal flaw for all nitric acid esters with the exception of PETN.

Nobel corporation still keeps Ascanio Sobrero’s original bottle of nitroglycerin, made in 1847. It is washed periodically - yearly, if I recall. I’m sure Nobel’s chemists do a good job of washing it, so the fact that they do it repeatedly indicates their distrust of NG’s stability.

Some workers believe that mannitol hexanitrate cannot be stabilized. Meyer, Kohler, et al, however, state merely that it is “difficult to stabilize.” In any case, it must be washed many, many times.

And highly-nitrated cellulose always requires addition of a stabilizer, no matter how thoroughly it is cleaned and washed.

(Also, oddly enough, Rosco recounted in the Forum how ETN as a secondary failed to explode under the influence of a blasting cap that he felt would have detonated PETN.)

But I will say this for nitric esters: They do last longer than AP!

It is a sad, but if you want to keep a high explosive safely packed away and ready for use, the only realistic choice is a ring-based nitro compound. And I have yet to find one that is energetic, has available precursors, and is somewhat easy to make. But I will.

Jetex Kid

June 30th, 2005, 06:59 PM

Rosco Bodine

July 1st, 2005, 12:08 AM

If you are having stability problems with ETN , then it is
for one or a combination of three likely reasons .

It is an incompletely nitrated and or incompletely purified product ,
upon which no stabilizer like urea or dicyandiamide was used in
the final crystallization bath .

It has been stored at too high a temperature .

It has been contaminated by something which has adversely
affected its stability .

I have ETN samples stored under harsh conditions deliberately
to observe the stability . And the stability for my samples
has been excellent , even after exposure to two summers
of outdoor tropical heat , sunlight and humidity . No color
change nor odor , no change in weight or melting point ,
and no change in explosive properties . What I am seeing is
excellent stability under outdoor storage conditions .

The way I purified my ETN was dissolving in an acetone / alcohol
mixed solvent with warming , suspending in the stirred solution
a little baking soda , and adding a little ammonium hydroxide ,
and a little urea . Into this stirred hot solution was gradually
added a stream of water containing about a half per cent urea ,
and some ice was added initially , with more ice towards the end .

The filtered and dried product has the correct melting point
for pure ETN and it is storage stable under conditions that
aren't too extreme , although it isn't as stable as PETN .
ETN is a lot like smokeless powder in terms of stability .

Rosco Bodine

July 1st, 2005, 12:08 AM

Nope

July 8th, 2005, 08:55 PM

Nope

July 8th, 2005, 08:55 PM

hereno

July 8th, 2005, 09:16 PM

Hello ppl... I was about to make ETN but I gave it up. My supplier said that the only source of getting erythritol is a company in US and if I'd like to purchase 100g I'll have to pay... 260 euros! S**t?

Now that would have to be some more exotic isomer! presumably you were trying to go through a chem supply company. Their meso-erythritol is a very expensive way to go :p

I guess that brings up the question, which isomer is that which is used in food?

hereno

July 8th, 2005, 09:16 PM

Nope

July 9th, 2005, 09:11 AM

Exactly. Chemical supply. They also said If I'd like erythritol for HPLC or something like that... :S

So, if I want to get just erythritol and no its isomers, how I have to ask for it? "Erythritol for ETN usage"? :P

Nope

July 9th, 2005, 09:11 AM

nbk2000

July 11th, 2005, 11:14 AM

http://www.sugarlessshop.com/2000/sugarsubstitutes.htm

Erythritol, sorbital, and mannitol. :)

nbk2000

July 11th, 2005, 11:14 AM

http://www.sugarlessshop.com/2000/sugarsubstitutes.htm

Erythritol, sorbital, and mannitol. :)

Nope

July 11th, 2005, 11:43 AM

Hmm... yeah. Maybe I should try mannitol. NM is a good primary :) But, purchasing mannitol would be suspicious or not?

Nope

July 11th, 2005, 11:43 AM

Hmm... yeah. Maybe I should try mannitol. NM is a good primary :) But, purchasing mannitol would be suspicious or not?

Bert

July 12th, 2005, 10:58 PM

If you are having stability problems with ETN , then it is
for one or a combination of three likely reasons ..
SWIM tried recrystalizing ETN with an additional 2% of diphenylamine rather than urea, the bicarbonate neutralization, solvent and precipitation being modeled on Rosco's procedure. After about a year of storage at outdoor temperatures in the upper midwest it turned olive brownish, started to sweat inside tne container and changed the color of a piece of PH paper taped inside the lid of the container. The sample was then destroyed... I understand that the color change is an indication that the diphenylamine is doing it's job.

Bert

July 12th, 2005, 10:58 PM

al93535

August 24th, 2005, 07:32 AM

A very promising explosive! I obtained 1 lb of erythritol and tried a few experiemtns. Below you can read my lab notes. A very strange thing happened with my first try. Maybe someone here knows what its all about. I did test it and the dry stuff burned somewhat like NG, but without its color.
I intend to try a few experiements with detonators, and with aluminized ETN. I will be testing 1 gram ETN dets with double salts as the primary, as well as flash 70/30 perc/aluminum as an initiator. Once these det tests are complete I will be comparing aluminuzed ETN with varying amount of al to standard ETN. These charges will most likely be pressed, but perhaps plasticized. I got very good yields with my last procedure, and this is the one I will be following from now on.

Lab notes attempt #1:

ETN

20 ml of 97% H2SO4 chilled to 12 degrees.
5 grams of Erythritol added pretty quickly, less then one minute with slight warming to 16 degrees.
1 hr 15 minutes for the erythirtol to dissolve.
25 ml of 100% clear HNO3 chilled to 10 degrees.
H2SO4/Erythritol slowly added to nitric acid over 2 minutes, with stirring.
temperature rose to 18 via mixing of HNO3 and H2SO4/erythritol.
temperature raised to 35 degrees with hot water bath.
Mixture stirred/swirled vigorously at least every 5 minutes for one hour after last addition. solution kept between 25-35 degrees during first 30 minutes, and kept at 35-40 for the next 30 minutes.
The mixture went from completely colorless and transparent to cloudy at 38 minutes after final mixing of acids/erythirtol.
Mixture sat for 15 additional minutes with occasional stirring.
Mixture dumped into 500 ml of ice cold water.
Instant precipitation of ETN.
Washed with 500 ml of water, then 500 ml of water/bicarbonate, and finally with 500 ml of water.
When the mix was dumped into water it got strange. I obtained hard chunks which were flat from settling to the bottom of the beaker. Almost as if the stuff was molten, then poured into cold water. It was strange. I obtained about 3 big chunks and a few small ones. About 6 grams total. This stuff was left to dry in an old car to keep dust off of it. The stuff melted completely into the filter, with small unmelted chunks in it!! Very strange, considering the temp here got to only about 95 degrees F, and the car windows were opened.

Attempt #2 yielded no product, which I believe was from weak HNO3 thought to be 70%, but must be way lower as many times it has failed me.

Lab notes attempt #3:

ETN

60 ml of H2SO4 added to 40 ml of 100% HNO3
Acids cooled to 10 degrees in ice bath
155 grains (10.04 grams) erythritol added to acids over 4 minutes temperature rose to 21 degrees
During addition the mixture became very think with snowy white crystals, they began to appear within 30 seconds of first erythritol addition
Mix was stirred continously during addition, and frequently for 20 minutes after last addition.
After the 20 minutes Mix was dumped into 900 ml water
Instant precipitation of ETN
ETN filtered and washed with 1 liter of water, and 500 ml of sodium bicarbonate solution, then an additional 500 ml water.
ETN is dried and dissolved into 150 ML of acetone with bicarbonate added, it is then filtered. 100% of the crude ETN dissolves into the acetone
ETN is then crashed out with 1 liter of water, filtered and washed with 1 liter of water
ETN is then dried

Final dry yield: 291.5 grains (18.88 grams)

After the recrystalization I have small chunks of ETN. Is it relatively safe to crush these into a fine powder when dry if I do a few grams at a time?

quicksilver

August 24th, 2005, 12:21 PM

After the recrystalization I have small chunks of ETN. Is it relatively safe to crush these into a fine powder when dry if I do a few grams at a time?

"Relatively safe"?

Personally I would be hesitant to crush any newly made ETN/PETN collective dry crystiline mass in that the element of friction bearing on the "crushing" may be too great. Perhaps whetting w/ acetone - then applying slow pressure would create the needed effect. I like to err on the side of safety...after all, it -=IS=- a nitric ester.

Child-of-Bodom

August 24th, 2005, 08:48 PM

Very interesting, ETN shouldn't melt at 95°F (That is around 40°C right?), but at a much higher temp...

You can better crash the ETN when wet, that's a lot safer than when dry, it is still a relative sensitive HE, and a 'few grams' have enough power to make your hand(s) fingerless. Another suggestion would be to dissolve the ETN agian in acetone, and add that slowly to ice cold water, which is stirred strongly to obtain small cristals, and prevent caking.

I think 100% HNO3 is a bit a waste to use on ETN, but that's from the perspective of someone who has only a small, limited amount available...

FinnBell

September 8th, 2005, 12:54 AM

I'd have to agree with Child-of-Bodom, I think that HNO3 is kind of a waste to use on ETN. Dont get me wrong I love ETN, Ive synthesized it a few times now and got decent, not great but decent yields from H2S04 and a nitrate. Granted HNO3 gives you a killer yield compared to H2S04 + Xnitrate but the cost of the alternate method is probably a fourth of the cost of the HN03 (for me anyway). And I think distilling your own HN03 is just a bit too much time and trouble just to use it for ETN. I guess its good though if you could find a very cheap source of HNO3. I pay a good $30 a liter for it and thats only 70%.

al93535

September 8th, 2005, 05:08 AM

Quite a few people have said that about each procedure I have posted that uses nitric, except RDX. I have a weak solution of HNO3, then I have distilled HNO3. The weak stuff is not good for anything except double salts and mercury fulminate. I'm sure as hell not going to dilute the distilled acid. And I like using mixed acids rather then sulfuric and a nitrate salt. Its easier to stir and usually gets a higher yield. It may seem like a waste to others but it's not for me. I enjoy the chemistry, and preperations just as much, if not more then the final product. Distilling fuming nitric for use in reactions is just fine.

I pay $1.60 for 454 grams of KNO3. For every mole of KNO3 I use for distillation I get one mole of HNO3. So 101 grams of KNO3 gives me 63 grams of acid. Thats 189 ml of 98-99% nitric for $1.60. In practice I would guess 165 ml to be safe. So I pay $9.70 for every liter of nearly anhydrous acid. Plus the almost negligible cost for H2SO4, about $2.27 a liter for 96%+ sulfuric.

Lets talk about ETN, and not who wastes what. What kind of yields do you get Finnbell?

Also, my ETN which has been stored for only a little while has developed NO2 in the bottle. It has been stored in the dark, but in a relatively hot place. I am going to re-neutralize and recrystalize and do a PH test. I was also thinking of adding a bit of urea to the recrystalization bath for stabilization, as has been suggested. I did a good job of washing and neutralization when it was made, but perhaps I did something wrong. Any suggestions as to what else I can do?

FinnBell

September 9th, 2005, 12:04 AM

Yeah I guess thats my problem, I get KN02 for about $2 a lb and I get NH4N03 for about $3 a lb which isnt bad at all. (althought I prefer NH4NO3) But the acids, damnit the acids are what are expensive for me, I have to pay out the ass for them and I only have a shitty little 1000ml retort so distilling my own is a pain. But yeah if you can get it cheap then hell yeah, use it up.

As for the ETN I usually get about 8 grams for every 10 grams used, sometimes for some reason when I do the reaction in large quantities I get shitty yields so I dont know what thats all about. Oh and by the way, you were talking about N02 forming with your stored ETN and I think thats weird cause I had the same thing happen to me and I was positive I had cleaned it throroughly I used litmus papers on them until they showed no acid and I still get the N02 fumes. Maybe its something else? But what?

al93535

September 9th, 2005, 12:34 AM

Strange, How many other people who have made and stored ETN have also seen the NO2 forming in the bottle? I am positive I washed it well, and neutralized it. But I am going to get ahold of some urea and see if that helps with stabilization. Does anyone know if the ETN becomes more sensitive after NO2 starts to develop?

8 grams of ETN from 10 grams Erythritol? Wow, I would have thought it would be better then that. Others have stated pretty good yields from a nitrate salt. Looks like my ratio is 1:1.8, so I guess thats not bad.

FinnBell

September 9th, 2005, 01:51 AM

Well like I said "usually", there have been times where Ive had great yields but for some reason when I scale it up my yields go to shit. Besides I only had 2 lbs of erythritol to play around with.

KrIsPy

April 8th, 2007, 01:26 AM

Unfortunately none of my local health food stores carry pure erythritol so I purchased . It contains mainly erithritol and some "natural flavors". Could these hinder the reaction, cause unwanted effects, or reduce the yield? And if so, is there a way, without knowing what natural flavors the sugar contains, to remove them? I assume the natural flavors are in very small amounts, but it could be a problem.

Also, are there many compounds that can be made from ETN besides plastics. For example, you can make AN dynamite with NG (I know its a bad example) but could ETN be used as a type of "filler"? I've heard of tiny additions of urea, but that was just for stability I believe...

Charles Owlen Picket

April 13th, 2007, 12:56 PM

Unfortunately none of my local health food stores carry pure erythritol so I purchased . It contains mainly erithritol and some "natural flavors"....

There is no question that any material in a prescribed reaction outside those of the ones specified will alter the resultant. One must always know the elements of a reaction to work within it's parameters.

KrIsPy

April 13th, 2007, 04:45 PM

There is no question that any material in a prescribed reaction outside those of the ones specified will alter the resultant. One must always know the elements of a reaction to work within it's parameters.
USE
Yeah. I know. It is a dumb question since if you don't know what the natural flavors are (I know they are derived from plants, which I believe refers to various fruits).
PARAGRAPH
My concern is that it could be dangerous, but I'll lead the way for those with similar problems and try a small synth with this impure erythritol.
BREAKS
I melted the erythritol and some stuff smoked away. I was wondering if it might have been the flavors. I also tried dissolving in water, but everything dissolved, so that won't purify it either.
NBK
I'll report back with results and later maybe a detonation video if it works. Thanks for the help. (I don't mean to interrupt the thread with questions like these, so sorry...)

Shalashaska

June 19th, 2007, 01:15 AM

I melted the erythritol and some stuff smoked away. I was wondering if it might have been the flavors.

I don't think that natural flavoring (mainly sugars) would be removed by melting.
In any case, I've heard of nitration of almost every sugar there is, so whatever may be in your erythritol shouldn't reduce the ETN yield by too much as long as erythritol is above 95%.

Rbick

July 6th, 2007, 02:08 PM

I would just like to say that ETN is an awesome explosive. I made my first batch a couple days ago. I ordered my Erythritol from an online health food store for 12 USD per 1.5 lbs (approx 680g). It is 100% pure with no flavors or additives.

For my nitration, I used 8g Erythritol, 55ml 98% ACS grade H2SO4, and 30g purified NH4NO3. I first added the AN (ground into fine powder) to the H2SO4 slowly at a constant rate. The temp got up to about 35 C. I then placed it in a salt/ice bath and let it cool to 10 C. I then added the Erythritol while stirring over a period of about 15 minutes. The temperature never went above 20 C and was very easy to control. It was left to sit in the bath for about 45 minutes with stirring every 10 minutes. At the end of 45 minutes, the nitration mix became thick with white ETN crystals. I crashed it into 500ml of ice cold water and filtered, and then recrystalized from Acetone. All of the filtered crystals readily disolved in Acetone, which I think means almost all of the Erythritol was nitrated.

When dried, the final yield was about 10g. I may have lost some in the filtering and recrystalization. As a side note with nitrating mixtures; I would recommend using AN. It has done the best for me so far as opposed to other nitrates. Especially KNO3, which thickens into syrup, making nitration difficult. AN is the way too go, as the mixture stayed thin for the entire process (up until the addition of Erythritol of course). I prefer swirling as oppsed to breaking stirring rods in thick nitration mixtures...

This is definatley one of the cheaper and easier explosives to prepare. Plus it has a good yield and its performance is awesome. I used 5g for impact tests, flame tests, ect. My charge was 5g which I initiated with .3g of pressed AP. Very brisant and powerful. I'll be using it in place of the usual Picric Acid or ANNM for small cutting charges and as a booster for larger AN based charges to remove stumps :cool:

Charles Owlen Picket

July 7th, 2007, 10:58 AM

If you have just begun to discover the immensity of the uses ETN may be available for....you are going to really appreciate it even more as time goes on!

Some "little thoughts" for the happy ETN experiment:
Ethanol is the better re-crystallization solvent. Best crystals in terms of size uniformity, and consistency. I avoid acetone as it's actually too effective a solvent and the resultant crystals are of a lower quality.

Pull all moisture out of the final product. If necessary, use a desiccant; it's worth it. Lack of moisture improves initiation.

AN does appear to be the solid nitrate of choice for those types of nitrations. However some have reported that successful results were achieved with calcium nitrate....(I have not tried this myself)

ETN can be used to sensitize PETN based plastique to a unique degree. Pure ETN plastique has been formulated with polybutene, et al - And was extremely successful.

Shelf life on some samples has been over 3 yrs with zero NO or any break down what-so-ever.

Rbick

July 7th, 2007, 06:42 PM

Charles,

I noticed that Acetone does result in larger and more difficult to handle crystals. I will be trying it with ethanol in my next batch.

I just checked e-bay and you can buy calcium nitrate in 15 pound bags for 7 US dollars. The shipping is 20 dollars however. I'll probably just find some at the local hardware store and test it out.

How do you go about drying your ETN with a desiccant? I have 2 bags of a desiccant (not sure what exactly) in my large storage bin where I keep my chemicals to keep my hygroscopic materials dry. Do you place the ETN directly next to it?

I have been searching the internet recently for information on ETN and I noticed it is very limited. So I started a page (http://en.wikipedia.org/wiki/ETN) for it on wikipedia.org if anyone is interested. If you see any information that is wrong or you want to add some, please edit it.

Shalashaska

July 8th, 2007, 01:12 AM

Just as a quick question to save me a little cash if possible, does anyone know if concentrated Isopropanol (~98-9%) would dissolve ETN as readily and completely as Ethanol?
When I made TNP, I successfully substituted it for Ethyl alcohol to dissolve the ASA and it worked out pretty fine. Shitty TNP yield though, but aren't they all. (using xNO3/H2SO4 anyways)

I guess it could end up like acetone either way, but it'd save money and effort

And has anyone used this in the stead of Ethanol successfully, and with nice crystal size?

Charles Owlen Picket

July 8th, 2007, 02:16 PM

Rbick and Shalashaska; please let me respond to those questions as I actually feel comfortable giving some feed-back on them...

Drying the ETN via desiccants is efficiently setup by placing the crystals in their filter paper (squeezed to pull as much water as you can to begin with) in a simple "breathable" drying procedure. I use a hot enclosed automobile, and set the filter-paper enclosed fresh ETN on top of some desiccant within a PAPER enclosure (cardboard). The combination creates a chimney effect and the drying effect is fantastic. Leave the car window open a tiny bit and it will take less than a couple of hours and you will have the best looking material you could imagine if the crystals were formed via ethanol.

I will ONLY use ethanol as a re-crystallization material. I have seen the difference and it's incredible. Some of the original work done with ETN by DuPont was ethanol re-crystallization based. I have tried Isopropanol (91%) and while a little better than acetone it's not as good as Everclear! I have also seen re-crystallizations done with methanol and it is better than Isopropanol - in terms of WHAT SHAPE & structure the final product crystals are. I strongly recommend 1st ethanol, methanol - then other alcohols and last; acetone. It's just too powerful a solvent....as strange as it sounds.

I do have some unique ETN material floating around. If you pm me with a Email I'll send it to you. I THINK I still have the old DuPont stuff and some lab notes that you may find fascinating. You CAN control crystal size, structure, shape, density. It's all been done back in the 1920's but cost factors for the base material kept ETN from reaching the public. It would have bee quite popular as testing revealed it to be more workable than may of it's contemporaries.

Enkidu

July 8th, 2007, 02:23 PM

@Shalashaska: I'm not sure what Rbick means by 'big crystals' (big is a relative term) when using acetone, but, using proper procedure, you should be able to avoid big crystals. ETN is not soluble in water, but it is soluble in acetone. Water and acetone are miscible. Therefore, when you pour an ETN/acetone solution in water, you succeed in precipitating the ETN.

If you pour a thin stream of ETN/acetone solution into a container of water under rapid agitation or stirring, you should precipitate small crystals.

As Charles said (he posted while I was typing), ethanol is the solvent of choice. Make sure your ETN is properly neutralized if you intend to store it.

These links don't directly answer your question, but they are informative anyway.

http://xsorbit29.com/users5/crucible/index.php?topic=130.0
http://xsorbit29.com/users5/crucible/index.php?topic=118.0

@Charles: I would be very interested in seeing the contents of your folder. Would you please up it to MiHD? You could send me a PM with the link. :)

Rbick

July 8th, 2007, 03:19 PM

The crystals appear to be somewhat like flat discs. They can easily be crushed though. I think my problem may be that I'm not stirring enough. Regardless, when I press the ETN into the charge it doesn't matter anway. It was mentioned earlier in this thread of casting ETN into the casing. I think I may start doing this as to get a higher density.

I made a 10g charge of ETN yesterday initiated by a .4g AP cap and cut a tree in half. When this one went off, it reminded me of the breaching charges I used in the military. You really feel the shock hit your body, unlike with AN charges of equal mass. This is obviously due to the greater VoD and brisance, but it is very noticeable.

The tree (on the left) was about 7.5cm (3 inches) wide. The smaller tree on the right was blown clean through and thrown somewhere in the woods. I watched it fly by, as I was taking cover behind a large tree only 30 ft. away :eek:. I have a video, but it isn't good enough to post. I didn't center the tree properly in the shot.

It is hard to scale the pic, but you'll have to take my word for it. ;)

Before pic (http://i164.photobucket.com/albums/u6/pudgedog69/10gETNBefore.jpg)

After pic (http://i164.photobucket.com/albums/u6/pudgedog69/10gETNAfter.jpg)

EDIT: I would also like to add that my yield for my last ETN synthesis was 21g erythritol resulting in 29.5g ETN using the sulfuric acid/nitrate method

Tinton

July 8th, 2007, 08:44 PM

This sounds like an amazing explosive for simple cutting plastique explosives. You could probably use nitroglycerine (15%/20%) to form a nice malleable plastic explosive. But DO NOT handle with bare hands, NITRO HEADACHE. (edit) Then again, 2 oxygen rich explosives mixed.....

I have pellet-like potassium nitrate. It is chemical grade, and about 2 mm in diameter. I tried to powder-ize it by putting it in a ball mill, for nearly 8 hours. Around 40% of the KNO3 powderized, or formed granules less than 1 mm in diameter. The rest remained at its original size. Any suggestions?
I haven't tried to synthesize PA/NG/ETN with KNO3 and I am curious as to whether or not the granules (2 mm ones) will be dissolved by the acid.

The only reason I haven't tried myself yet is due to the current lack of H2SO4.
I checked Lowe's, Home Depot, Some other store, and Wal-Mart.
Wal mart was the only store to carry H2SO4 Drain opener. I didn't buy it because i had no clue how concentrated it was.

I also don't have any nitric, considering my retort hasn't arrived yet.

Rbick

July 8th, 2007, 10:20 PM

Yes the KNO3 will eventually dissolve in the acid, but its a pain and takes too long for me. I would recommend just getting a coffee grinder. That is what I use to powder my AN and anything else I have in the form of pellets and it works great.

If you can, I would also recommend using AN as your nitrate. I have had bad experiences with KNO3 making the mix too thick and ruining my synthesis.

Also, for your chemicals: If you are over 18 years of age, order your chemicals from chemical suppliers. You can do it over the internet or the phone. That is where I get a majority of my chemicals, as I like to have them as high quality as possible. Don't worry about government watch lists, they arn't going to track you for ordering 2.5L of H2SO4 and some Ammonium Nitrate. When you order 150 kilos of AN and 37,000 litres of Nitro Methane, then they may give you a visit. :D

Charles Owlen Picket

July 9th, 2007, 02:27 PM

A quality issue I have seen was the diminishment of ETN crystals in size and weight in impact tests. What I had read was that when the weight goes below 5.mg (which is DAMN small) and one is still getting a serious exposition from impact tests - you have a winner in your synth.

I have seen an ETN crystal smaller than the asterisk (*) when folded in Al foil and smacked with a hammer on an anvil give a report as loud as a .22! I am NOT exaggerating. That material was fantastic. It was an H2SO4/AN synth using ethanol as recrystallization solvent. These crystals are platelets, unlike the rhomboids that methanol makes. So what happens is they pack down a great deal.

The two issues of re-crystallization are shape and individual weight. Apparently these can be controlled and are key to utility. ETN provides one of the most unique ingredients to a plastique. The platelets can compress to a phenomenonly high degree, thus making the plastic VERY dense. What's more is that ETN can sensitize other secondaries in a plastique formulation......

Rbick

July 10th, 2007, 10:50 AM

Platelets is a good way to describe the crystals, never thought of that... But I have been using ETN in my caps as of late, and it makes a world of difference. I no longer get unsuccessful ANNM dets! I usually use 1g ETN and .4-.5g of AP. Its funny because the AP takes up twice the room as the ETN which is at greater mass.

So has anyone tried using ETN in a plastique mixture? It would be interesting to try. Or how about replacing PETN with ETN in semtex? This could balance the O considering RDX is somewhat O defficient. The possibilites are endless.

I'm going to figure out the proper O balance with ETN and RDX just for fun, so I can dream... :D

C3H6N6O6 ----> 3CO2 + 3H2O + 3N2 - 1 1/2 O2

So it needs 3 mols of O to balance. Every mol of ETN releases 1 mol of O

C4H6N4O12 ----> 4CO2 + 3H2O + 2N2 + 1/2O2

so we need 3 mols ETN to 1 mol RDX.

Molar mass: ETN = 306
RDX = 222

306(3) + 222 = 1140
222/1140 = 19% RDX

A mix of approx 20% RDX and 80% ETN would give you an oxygen balanced composition with an already really high VoD and nice brisance! Plus, as Charles mentioned, the ETN can be highly compressed in the composition and sensitize it to a great degree. Sounds like the next thing on my to do list...

Charles Owlen Picket

July 11th, 2007, 11:37 AM

From what I have read; perhaps one of the most interesting things about energetic materials in what happens when their physical make-up is altered via re-crystallization. A granular crystal is formed through re-crystallization with methanol, a flat platelet is formed with ethanol. These have differing responses to initiation. However using the ethanol technique the resultant will "pack down" to such a degree that the density level can be astounding.

The density result is quite astounding, especially when using 2x4 wood attached with a hinge, making a press and using same around a corner of a building for safety, etc. is employed.

In the OTC thread there is some material regarding plasiques.....and (I think) provides the information you seek. Plastics make from ETN as a replacement is VERY easy to initiate. However the level of tackifier, etc to energetic is much less than PETN/RDX. It takes a very small amount to bind the material to a "play-dough" like consistency.

I haven't forgotten the written material; I have to get to another machine to dig them up :-)

Tinton

July 13th, 2007, 01:51 AM

Speaking of plastics made out of ETN....
Considering how extremely oxygen rich it is, what liquid explosives are plausible for making plastics.
MEKP sounds great ; not only 100% hardware store materials, but an oxygen deficiency. BUT it dissolves plastics and its extremely harmful, so not only will you get nitro headaches from handling it, but some nasty hands.

Nitroglycerine would compliment ETN's power, giving probably 8000 m/s VoD. BUT nitro is nearly as oxygen rich as ETN. If you add ammonium nitrate, you might stabalize it, but lose the high Vod...

Both NG and MEKP are sensitive to extent, and mixed with something 1/3 the insensitivity of PETN... I'm not so keen on treating it like plah-doh

Shalashaska

July 13th, 2007, 03:01 AM

I wouldn't think of a perfect OB so much as a requirement as much as a luxury. If you have NG and ETN, 20:80 (respectively) would make for an incredible explosive, regardless of OB; particularly since it's positive rather than negative (although it does feel weird letting all that oxygen go to waste)
If you can think of something that really fits into the slot, then by all means go for it... I really can't at the moment, my mind's quite fatigued from lack of sleep.

PS, just reading over again... unless I'm going completely daffy, wouldn't NH4NO3 just keep it on the positive side?

Rbick

July 13th, 2007, 11:28 AM

Adding AN would definatley make the OB more positive, Its 20% +OB. Oxygen balance is a luxury, but it also adds to the explosives ability to "do work". It increases heat of formation and increases the volume of gas output of the explosive.

TNT for example by itself releases 3 1/2 mols of Carbon which has no oxygen to bond to, since TNT is very oxygen defficient. That is why TNT is said to have a very sooty after effect. So oxidizing the extra Carbon to at least CO would result in the release of 3 1/2 more mols gas instead of just Carbon.

So in my attempt to make my charges as efficient as possible, I try to balance the oxygen, along with packing the charge correctly, mixing components into them correctly, ect. Plus OB is easy to figure out on paper. I'm still trying to figure out the Hess Law (http://en.wikipedia.org/wiki/Hess%27s_law), but I still havn't gotten it down! I wish I had more formal education on chemistry rather than trying to teach myself. :(

I agree with you though. Letting all that O in ETN go to waste feels weird. Its always fun to figure out what stuff can be mixed in to balance it out :)

Vitalis

July 13th, 2007, 01:15 PM

If the H2SO4 from wal-mart was "Liquid Lightning" the MSDS claims it is 94.19% by weight. No idea what else is in there though, like others have said, maybe if dealing with small quantities a chem supplier would be best.

Shalashaska

July 13th, 2007, 01:35 PM

Oxygen balance is a luxury, but it also adds to the explosives ability to "do work". It increases heat of formation and increases the volume of gas output of the explosive.

Haha, being the cheapass I am, I'd say to throw in some 2 micron Al and be done with it. :)

Deceitful_Frank

July 13th, 2007, 03:03 PM

Haha, being the cheapass I am, I'd say to throw in some 2 micron Al and be done with it. :)

Hell yeah!

A 60:20:20 mix of ETN, NG and 600 mesh flake Al makes a monstously powerful mix, both in blast pressure, velocity and brisance. The addition of 20% Al extends the pressure pulse by reacting with the detonation products of the ETN and NG after and behind the detonation shock front, partially reducing the CO2 and H2O to CO and H2 and releasing enormous quantities of heat. This is of course at slight detriment of velocity and maximum detonation pressure but I believe the added impulse given by the sustained pressure makes this explosive mix ideal for defeating anything but solid steel or for use in a shaped charge where absolute detonation pressure and brisance is more important than sustained energy output. In these situations leave out the 600 mesh flake Al for maximum velocity and brisance.

The clip shows some ETN followed by the detonation of just 45 grams of aluminized ETN and nitroglycerin paste. Due to the dissolution of ETN in NG the ratio does need tweaking as it was a little runny but you get the idea! :D

http://media.putfile.com/ETNNGAl

stupid939

July 13th, 2007, 05:24 PM

Shalashaska - I wanted to say that too, but the point was made that Mg and Al will sensitize the explosive(s) and we don't really want that.

I just got done searching around for negative oxygen balanced liquid explosives, and the best candidate seems to be PGDN. In the PGDN thread, they discussed making plastics with it and ETN.

http://www.roguesci.org/theforum/showthread.php?t=3353

From what I read in the thread, propylene glycol can be obtained in the form of some anti-freezes. I will look around, and if I find some, I will post the results.

A friend of mine recently made ETN and after he recrystallized it from ethanol, he obtained white pearl-like (shiny) crystals. It took quite a bit of ethanol (and light heating) to dissolve the ETN, and after he added water and filtered the ETN, he distilled off the ethanol and was left with water with quite a few ETN crystals. Only about half of the ETN was filtered out the first time, and he was wondering if any of you have had this problem when recrystallizing.

Enkidu

July 13th, 2007, 07:27 PM

It took quite a bit of ethanol (and light heating) to dissolve the ETN, and after he added water and filtered the ETN, he distilled off the ethanol and was left with water with quite a few ETN crystals. Only about half of the ETN was filtered out the first time, and he was wondering if any of you have had this problem when recrystallizing.

Swiy's procedure is rather wrong. If swiy does it correctly, swiy won't need near as much ethanol. I posted some O. Chem. books in the rapidshare links threads a while back. The links are still good.

Charles Owlen Picket

July 14th, 2007, 10:08 AM

Ethanol needs to be at or near boiling point via (very) hot water bath _before_ you begin. Bring the ethanol to a near boil (or AT a boil) and then put in the raw ETN. The solution should be at saturation level - and after a period of time wherein there is complete solvency; drowned in cold distilled water. Methanol; same technique.

stupid939

July 14th, 2007, 05:31 PM

Yes, I found that out, but I sent a PM to Enkidu and I did not feel it was necessary to make another post. Thank you for your help because there are others who may make my same mistake.

I will look around for some propylene glycol this weekend, and hopefully I will be able to do some tests.

Rbick

July 19th, 2007, 05:58 PM

I didn't see this until today:

I just got done searching around for negative oxygen balanced liquid explosives, and the best candidate seems to be PGDN

What about Nitromethane? It is very oxygen defficient and would hopefully be sensitized to a resonable level by ETN. 1 mol NM needs 3/4 O2 (1 1/2 O) mols to be fully oxidized. So 1 1/2 mols ETN would satisfy it. Molecular weight of ETN is 306 and NM is 61. The proper mixture would be 88% ETN to 12% NM for oxygen balance. 12% NM wouldn't make the mix too thin I don't think.

I'll give it a try tonight and let you guys know :cool:

EDIT: Yeah I tried a 15g charge of 88% ETN 12% NM and it wasn't sensitive enough to be initiated by 1g pressed AP. I'll try with a larger cap and maybe less NM, as the mix did turn very thin. That was my last bit of ETN too! Time for another batch...

Charles Owlen Picket

July 20th, 2007, 11:14 AM

That should have worked.....however HMTD is a better initiator than AP. There is a thread (an oldie, IIRC) that involved the lowest level of energetic material that could be initiated and I would be willing to bet that with nitrated polyols 15 grams is enough to shoot.

Could there have been another issue entirely? I think it was a Russian study from their published papers on energetics that indicated that proximity and surface contact had deeply influencing factors with sheet explos. It could get as small as sub millimeter width that would initiate with proper placement.

Los Alamos research papers (I think available freely via a google) also have some published results on initiation. There are one or two factors that must be met for small amounts of secondary. But 15 grams should be ample.

The reason I mention sheet material is it's relationship to initiation contact surface; not that you have a sheet construction obviously. But perhaps it's a proximity issue or simply that AP is just not as efficient as another example.

Rbick

July 20th, 2007, 12:15 PM

Good points Charles, thank you for pointing those out. I probably shouldn't abandon the 12% NM mix so quickly without testing it further. Perhaps I will try a .5g AP with 1g ETN as a cap, which has worked wonders for me with successfully detonating ANNM. So if I'm getting a good det. with 1g, I know 15 is definatley enough. I love ETN...

I'm leaving the country for a week or so, but when I return I'll retest it and post the results. I'll try different percentages too, and larger charges. Along with videos of course :)

Rbick

July 30th, 2007, 02:39 PM

I found this video (http://www.youtube.com/watch?v=vz0zo8yQIFY) on YouTube of an ETN/NM/NC shaped charge. It doesn't say the percentages used, but I am obviously not the first one to test NM with ETN. Calculating for proper O balance will be easy enough.

The addition of NC is a good idea as I think it would make a nice gel. There is so much stuff I want to test, and so little time!

My previous post is too old and it won't let me edit it, so I had to make a new one. Sorry...

FireBomb

July 30th, 2007, 09:23 PM

Hmm if I'm not mistaken that video was made by Axt (now baned) it has already been posted I believe in the SC charge thread he started several years back.

You should look for the thread its very good lots of information on Shape Charges and ETN mixtures as this explosive was favored by him.

On a small side note I wish he hadn't been baned, but he was given a one week probation period.

He violated it so while it is sad that he is gone. He had some very good ideas it is his own fault to think that a senior member is immune to the rules.

Shalashaska

July 31st, 2007, 12:05 AM

Ahhhhhh! So Axtran is Axt! I guess I should have put that together myself...

From his youtube channel, he appears to be more of an advanced chem guy, rather than a 500 pounds of ANFO guy :P

It is unfortunate that he was banned, and I couldn't find anything on why he was banned... He did appear to be a pretty valuable member here, but rules are there for a reason.

FireBomb

July 31st, 2007, 12:17 AM

NBK gave him one week probation period for I believe asking a question that could have been solved by a search or something like that...

Anyway he was told not to post anything for one week or he would be banned and he ignored NBK's warning.

Anyway enough of that we should get back on track here.

I'm thinking of giving ETN a try but still researching into it.

This thread has been invaluable to me and I hope to give it a try here in a few weeks.

I will keep you all informed of my progress.

Charles Owlen Picket

July 31st, 2007, 10:31 AM

I have heard of an experiment wherein someone made up some microscope slides of various energetic materials (which were more macro than micro by the way) for a specific machine at 75x dual view.

The concept was not only photography and crystal structure comparison but longevity....ETN pulled equal with PETN and PEN as after 4 years there were NO signs of decomposition, etc. Pretty damn amazing stuff.

stupid939

August 1st, 2007, 09:01 PM

OK boys and girls (most likely just boys), I found some propylene glycol in the form of Sierra Antifreeze/Coolant - Safer Formula. It costs $9.00 at my local Ace Hardware.

Picture:
http://www.sierraantifreeze.com/images/art_sierrabottle2.jpg

MSDS:
http://www.peakantifreeze.com/msds/msds_sierra.pdf

It turns out that it is around 95% PG, and a simple distillation would take care of the dyes and most of the water (PG's boiling point is 188.2°C).

OK, now we need to find out how much we would need to mix with ETN for PGDN to be fully oxidized.

PGDN

Molecular Weight - 166.1
Chemical Formula - C3H6N2O6
Decomposition - C3H6N2O6 -> N2 + 3H2O + 3CO

So we need 3 moles of oxygen to fully oxidize one mole of PGDN.

ETN

Molecular Weight - 302.1
Chemical Formula - C4H6N4O12
Decomposition - C4H6N4O12 -> 2N2 + 3H2O + 4CO2 + O

Oxygen balanced decomposition reaction:

C3H6N2O6 + 3C4H6N4O12 -> 7N2 + 12H2O + 15CO2

(Mass of PGDN x 100%)/(Mass of PGDN + Mass of ETN) = (166.1 x 100%)/(166.1 + 906.3) = 15.5% PGDN

This means that 15.5% PGDN and 84.5% ETN would be oxygen balanced.

(I did this for the less experienced, plus I like putting my skills to work. Let me know if I made any mistakes)

Hopefully I can find a friend to test this mixture and report its placticity, power, and ease of use. ;)

Deceitful_Frank

August 2nd, 2007, 03:38 AM

I Don't mean to piss on anyones bonfire here but I feel I should point out that ETN is highly soluble in PGDN and the composition mentioned above is likely to become rather wet, particularly if the ETN's particle size is small or it is excessively stirred.

PGDN is however a wonderful energetic liquid with good power and excellent stability, mixed with 60% finely powdered AN, makes a simple, "safe", powerful and nearly oxygen balanced dynamite with much higher denonation pressure than 3:1 ANNM, due to higher cap-sensitive densities and higher velocity. If you cant get hold of NM at a reasonable price and want to increase your life expectancy, for medium to tough blasting work, this IMHO is deffinately the way to go!

Besides, whats this obsession with oxygen balance all about? Trust me, I have been blasting around for years and unless your explosive is VERY oxygen defficient or rich (tens of %) or you are working in confined areas where the fumes could become a problem, oxygen balance doesn't mean shit. You want DENSITY, VELOCITY and ENERGY. These are what give you detonation pressure, of which brisance is a function.

So go mix 60 grams of ETN with 20 grams of good ol' nitro. Let the nitro dissolve a little of the ETN and then throw in 20 grams of 600 mesh german flake Al. Sure, it may be 4% oxygen rich before the Al gets hold of the detonation products but density and sheer power are second to none.

Alexires

August 2nd, 2007, 05:08 AM

Deceitful_Frank - You will find that on this forum, a lot of the members tend to go by the motto "If it works, tweak it" and I'd rather like to think that this goes for all of us.

Speaking for myself, when I am working on anything (whether it be physics, chemistry, energetic materials or just navigation) I first of all worry about getting it to work. If it works, then I try and get it perfect.

I think that you will find that deep down, most of the members of this forum are, to some degree, perfectionists. They care if there is 1% of impurity in their final product if they can do anything about it.

If a PGDN/ETN mix is too sloppy to be useful for non sealed detonators, then screw with the ratio's and throw a plasticizing agent in there. As I'm guessing that ETN and PGDN are relatively non-polar, maybe use NC as a plasticizer and compensate accordingly.

Those old Axt movies of ETN is rather impressive, especially that shaped charge one mentioned earlier.

I suppose someone could always set up a series of shaped charges with graduated Oxygen deficiencies and surplus to see what effects oxygen balance really does have.

Would be nice to have a guideline to those kind of effects.

Rbick

August 2nd, 2007, 10:33 AM

You're right about the perfectionism thing. I spent two hours last night scraping a container used to recrystallize some ETN to make sure I got every last bit of it to improve my yield. I came out with a nice yield and product by the way :cool:. (30g erythritol into 38g ETN using the nitrating salt method).

While I have never conducted hands on testing with Oxygen Balance, from what I have come to understand it improves performance in a few ways. One being heat of formation (http://en.wikipedia.org/wiki/Standard_enthalpy_change_of_formation). If a mol of TNT detonates leaving 3 1/2 mols of C unoxidized, no more heat is produced by these atoms. If there is Oxygen for it to bond to, becoming CO2, then more energy will be produced during "formation". I'm not very good at explaining, so check out the link. Wikipedia is awesome.

It also helps improve gas output. The C released by TNT (I'm using TNT as an example because it is 74% oxygen defficient) is a solid, resulting in what could be described as a "sooty" explosion. If the C is bonded with Oxygen and made into gas, you're gas output has just increased and left you with much less solid byproduct. At STP (standard temperature and pressure. Described here as 0 degrees C and 1 atm), 1 mol of gas takes up 22.4 dm3. So to find gas output of an explosive, you first count the mols of gas released. This is AN.

NH4NO3 ---> 2H2O + N2 + 1/2O2

Water will obviously come out as steam, and is counted. So 1 mol of AN produces 31/2 mols of gas.

31/2 (22.4) = 78.4

Take this divided by molecular mass of AN, which is 80 g/mol

78.4/80 = .98 dm3g/mol -1

AN has a pretty high gas output, as we can see. This is why it is described as having more heaving power. RDX is at about .908. TNT unoxidized is at .74. Oxidized it would be 1.08, which is quite an improvement in gas outputand means more energy. You'd have to account for the added mass of the oxidizing compound, which would take the 1.08 down a bit, but it would still be much greater than .74.

Here are also a couple quotes from Wikipedia.

The sensitivity, strength, and brisance of an explosive are all somewhat dependent upon oxygen balance and tend to approach their maximums as oxygen balance approaches zero.

Because sensitivity, brisance, and strength are properties resulting from a complex explosive chemical reaction, a simple relationship such as oxygen balance cannot be depended upon to yield universally consistent results.

So while its not everything, I think it helps to try and balance it if you can. Again the perfectionism thing... I also think that since it is one of the easier calculations to make, people (such as myself) like to figure it out for fun, and it is one of the few things we can control in the reaction itself, sort of. So thats my thing on O balance...

As for ETN, I'm going to continue mixing it with NM and doing some test with it.

stupid939

August 14th, 2007, 02:29 AM

Well, SWIM killed two birds with one explosive device. He made some PGDN awhile ago, and because he has been experimenting with shaped charges, it seemed optimal to use ETN/PGDN in the 85:15 ratio.

From his experience, it is hard to blend the mixture completely. It ends up semi-lumpy unless it is compressed quite a bit. If it is highly compressed (in a 1 ton arbor press) the resulting mixture is hard to detonate (even with 2g of AP) when in planular(?) contact (see the link at the bottom for a better understanding of the type of blasting caps and charges used). Perhaps it could be highly compressed, and then broken up and pressed with less force (this is, of course, if the blasting cap is in planular contact with it).

For reference, when pressed to about the pressure that can you could physically exert on a small rod (he did try hand pressing a time or two with caution), it detonated quite nicely and with good brisance.

The mixture is actually quite nice to work with and it resembles damp ETN. I think that mixing in a small bit of NG, while increasing the amount PGDN according to OB, would make the plasticity better, and it would be even nicer to work with.

Here is the link to my long post on the copper wire shaped charge I designed.
http://www.roguesci.org/theforum/showthread.php?p=93549#post93549

LibertyOrDeath

September 21st, 2007, 04:59 PM

I had a daydream today about making ETN for the first time, and I thought I'd share it with the board. I'm not completely sure how successful this daydream was, as I'm still daydreaming about most of the material drying. But here's what has happened so far, and any comments are appreciated.

100 mL of H2SO4 (Rooto drain cleaner straight from the bottle, supposedly 93.2% conc.) was put into a 250 mL beaker. Initial acid temp was about 25 deg C.

48 grams of NH4NO3 (taken from an instant cold pack and then ground into fairly small grains with a mortar and pestle) was added fairly rapidly to the acid and stirred. The temp rose to about 40 deg C, and white fumes began to form. A fan was used to keep these away. The AN dissolved quite easily in the acid.

The beaker was then put into an ice bath until the temp fell to about 15 deg C. Then 15 grams of erythritol was added -- in small amounts at first, then more rapidly due to a lack of significant temperature increase.

The mix was stirred vigorously at first, then periodically over an hour while keeping an eye on the temp. It stayed between 10 and 20 deg C the whole time. The mix got slightly thick, but it was never difficult to stir. It looked a little like melted vanilla ice cream.

After an hour, the mix was poured into 2 L of water with some ice in it. A white powder could be seen floating in the water, with some settling on the bottom of the jar. This was then filtered through a coffee filter into another jar (that took about an hour).

A white paste was left in the filter. The filter was squeezed to remove some of the remaining water, and then the paste was dissolved in 95% ethanol. This was filtered again with another coffee filter. This was done to help the product dry more quickly. The still-wet product weighed about 28 grams.

I didn't bother to recrystallize or neutralize because I didn't want to take the trouble without being sure I actually had ETN first. In the future, once I know I'm doing everything else right, I will take those steps.

After letting the "ETN" (if that's what it was) dry a bit, but not completely, I held a flame to a tiny lump of it. The alcohol still in the ETN caught fire and burned slowly with a mostly blue flame as the lump of ETN melted into a clear, slightly brownish fluid. When the brownish fluid solidified, a flame was held to that as well. It burned pretty violently, with lots of popping and snapping sounds, but didn't go "bang."

Next I tried some hammer testing. One small lump that was apparently completely dry did clearly go BANG (about as loud as a small firecracker) when hit somewhat hard with a hammer; however, I was not able to get it to happen again on repeated tries.

So anyway, the daydream continues, and further testing will be done when the ethanol has completely evaporated from the sample.

I do have a few quick questions if someone doesn't mind answering:

(1) Is it normal for the ETN to look like a clumpy paste when it's wet?
(2) What is a reasonable drying time in open air? A day or two for ~70 deg F temps?
(3) All in all, does it sound like I succeeded in making ETN in the above daydream? More specifically, does ETN only detonate from shock when totally dry, and does it deflagrate somewhat violently (but "sputtering" a bit) when exposed to flame?

Thanks, guys. I plan on experimenting much more with this stuff (in my dreams) in the future. I really should dream about making some primary as well in order to test this stuff properly.

Rbick

September 21st, 2007, 06:48 PM

That sounds like a success to me. One way to make sure it is ETN is to dissolve it in a ketone or alcohol. Plain Erythritol I know for a fact does not dissolve in acetone. This is how I filter out any un-nitrated products in my ETN batches. I dissolve the product in acetone and run it through a coffee filter. The un-nitrated material is caught in the filter while the dissolved ETN passes through without problem into the cold water, recrystallizing into find powder. I then rinse the product with Sodium Bicarbonate, rinse, and put it out to dry.

When you place a flame to the ETN, it should melt into a brownish/yellow clear color. A quick burst of flame afterwards usually marks a good product. The "Sputtering" you talk about is probably due to water that still hasn't evaporated.

When drying, I place mine under a heat lamp for about 8 hours, and it is usually dry enough at this point. Just make sure you don't put any heat source too close, just to be safe.

ETN is quite sensitive. You should have no problem detonating a 20g + charge with only .4g of AP. However, it is still stable enough to press quite well safely. When you do try your first ETN charge, let us know how it goes :cool:

LibertyOrDeath

September 21st, 2007, 08:27 PM

First, a huge thanks to Rbick for that very helpful information. I'd uprate you again if I could. :) I'll get some acetone ASAP and do as you describe.

Next: I just got back from dreaming about further flame testing (with product that's still slightly damp and smelling of ethanol). It was done as follows. A lump of product was placed on a piece of aluminum foil, and a flame was held underneath the foil. The lump of product melted quickly into the brownish-clear fluid, which then started to boil and hiss as the flame was held under it. Then the fluid started to flare up a bit, with some snapping and popping while burning almost like a small blowtorch, and the product was finally consumed with a FOOMP!

I also did some more hammer testing, but there was only a BANG! a couple of times out of at least 50 fairly solid hits (about as hard as you'd hit a nail with) on tiny amounts of product. Perhaps that's because it's still a bit wet. But I guess the fact that it went BANG! at all is promising.

Yes, I will definitely share any further results of interest with the board. I'm particularly interested in casting this stuff into a container at some point. It does melt very easily, and with my stuff at least, a flame had to be held under it for at least a couple of seconds to get it to flare up (direct flame contact with the liquid makes it deflagrate immediately, though).

EDIT, reply to Rbick below:

Thanks for the further note. Yup, I actually read this whole thread before my dream and saw that point about using hot water to cast it. That's definitely the way to go -- I sure wouldn't want to try to melt any significant amount of this stuff with a flame. :)

Rbick

September 21st, 2007, 10:35 PM

Sounds like you produced some good stuff. I know there are 9 pages to this thing, but just look back and I know somewhere in here they discuss casting ETN. It has a fairly low decomp (160 *C) and an even lower melting point of 60 *C, so you have to be careful.

I think NBK talks about placing the container in boiling water which would melt the ETN, but not reach decomp. Just take a look, its in here somewhere.

LibertyOrDeath

October 4th, 2007, 04:52 PM

I had another dream about ETN in which I did some more experimentation, though I still haven't had the opportunity to detonate a significant charge yet. :(

Product was produced as in my earlier post, only this time I followed Rbick's advice and purified the product by (1) dissolving it in some acetone, (2) pouring the acetone through a coffee filter, (3) discarding the filter, and (4) pouring the acetone that went through the filter into about 2 L of ice-cold water and allowing the crystals to precipitate. The crystals were then removed from the water by another filtration and allowed to dry for a couple of days. (I skipped the sodium bicarbonate step this time, but if I ever want to store this for any considerable length of time, I will do the neutralization.)

The crystals thus formed were extremely small -- like white powder -- but tended to stick together in brittle clumps. The following properties have not changed over the course of a week of storage in the open air (a little testing was done on most days):

Castability: Sure enough, my stuff seems to melt reasonably quickly (within a minute or two) within a brass rifle cartridge case held partially submerged in a water bath with a temp of 70 deg C. When the melting stopped, I checked the water temp again and saw that it had fallen just below 60 deg C (melting point of ETN is 61 deg C). So the stuff is quite easy to cast this way, at least in small amounts.

Shock sensitivity: Surprisingly low -- considerably lower than I've read. Confining an amount about a quarter the size of a match head in some Al foil required at least ten very hard hits with a hammer against a stout concrete floor to cause detonation. (Ear protection and goggles are definitely recommended for this! You'll also likely be sprayed with tiny flakes of aluminum.) The foil was flattened completely with the first hit, and subsequent hits were against the flat foil, putting slight dents into the floor before the detonation.

I suspect, however, that larger crystals would be easier to detonate, as might a casting. So anyone who makes ETN for the first time should NOT take my dream as as a license to handle this stuff carelessly!

Friction sensitivity: Rubbing a small amount of powder vigorously into concrete with the head of a hammer had no effect. A mortar and pestle might set it off, but I don't have one that I want to put any chips in from detonation.

Flame sensitivity: Here's where it got interesting. I've been able to get a small lump (about the size of a quarter of a match head) to detonate consistently by putting it on a sheet of Al foil, folding the foil over it a couple of times for confinement, and holding a lit match for a couple of seconds to the foil where the lump is. The ETN explodes with a loud BANG, and tiny bits of foil (many as small as pieces of glitter) get sprayed everywhere. The tiny size of many of the Al pieces reminded me of the great brisance of this explosive.

When unconfined, the same amount of ETN burns quickly but rather unimpressively when a flame is held directly to it. But if that same amount of ETN is merely placed on top of a sheet of Al foil (unconfined) and a lit match is held underneath, it either burns rapidly with a "snap" or, less often, melts and then fully detonates. Larger lumps seem more likely to detonate when subjected to this test. Be careful: this stuff is powerful indeed.

The fact that a small amount of ETN can be made to detonate when so confined leads me to believe that effective detonators can be made from this explosive without the need for much more dangerous primaries. This is something I want to dream of experimenting with more in the future.

I hope the above info is helpful to anyone considering giving ETN a try. I'm very impressed with this explosive. In addition to its power, it seems very difficult to detonate accidentally but quite easy to detonate deliberately. Again, though, I caution people to test their product for themselves, as factors such as purity and crystal size may have a significant effect on sensitivity.

Rbick

October 4th, 2007, 08:37 PM

You're correct in your assumption that ETN is a good replacement for primaries in blasting caps. I actually use ETN in all my caps. I use as little as .1 grams of AP pressed lightly onto 1-2g of ETN in a straw for a very effective blasting cap. This eliminates handling large amounts of dangerous stuff like AP!

Something interesting I read in either the PETN thread or NG thread is the mixing of PETN and Nitroglycerine. The mix was said to be 20% NG and 80% PETN, and could be adjusted to as much as 30% NG. I would imagine that the PETN could be replaced with ETN for the same effect. This would be a very powerful mixture with the potential to oxidize an added fuel, considering NG and ETN are Oxygen positive. The result of the mixture was said to be a moldable plastique that leaked minimal amounts of NG. This is on my to do list... :)

Charles Owlen Picket

October 4th, 2007, 09:50 PM

From what little I know about ETN the crystalline structure are generally platelets (if EtOH is used for re-crystallization) or hexagonal (if methanol is used....don't use acetone as it is actually TOO soluble in acetone and the re-crystallization is less than ideal). I have some wonderful pictures of ETN somewhere illustrating these issues. PETN is most often needles unless acted upon by a crystal modifier.

Therefore, the variables in ETN usage first start with the form that the material is in. I have heard of it used as a sensitizer in plastiques & I have heard of it used in conjunction with NG, etc...however it is very close to the same sensitivity level as NG but more importantly NG softens the crystal and the final product allows the NG to "run" and "weep" from the solid.

In so saying, the final product may not be what is expected due to a lower level of absorbency of the ETN. This may be improved by adding a material that is active and maintains solidity such as ammonium nitrate (60:20:20, is the example I have heard referenced).

*** I will dig the pics up; I've been saying this for too long and procrastinating!

Enkidu

October 4th, 2007, 10:23 PM

@Charles: If you ever come across those files, please send 'em my way.

nbk2000

October 4th, 2007, 11:10 PM

How about sending 'em OUR way, collectively, not individually? ;)

Hinckleyforpresident

October 5th, 2007, 01:42 AM

I’m not sure if this has already been discussed, I read almost the whole thread and do not believe that it has, if I am wrong then I apologize.

Something rather curious happened to my ETN when I was recrystallizing it; it came out of solution molten.

First, I dissolved 48 grams of impure ETN in 300 ml of near-boiling acetone. The acetone turned a sort of yellow tint.
Second, the acetone solution was poured into 600 ml of water (cool, not cold) and formed two distinct layers. The top layer was sort of white foggy, the bottom was a yellowish/whitish blob. As I poured the filtered acetone solution into the water little bloblets of molten ETN dropped to the bottom, just like the crystals do in other recrystallizations.

At first I was not only puzzled but alarmed. I was not sure if something unknown and possibly hazardous (not thinking molten ETN at first) had been made accidentally.

Soon after the last of the acetone was added I cooled the solution with some ice. Then I suctioned off the molten ETN bottom layer (clogging my turkey baster later on when it solidified) and put it in a separate beaker and added more ice.

Slowly the molten ETN solidified into crystal ETN over the course of about 10 minutes.

I am thinking that this could be used to both cast and purify ETN all at once.

LibertyOrDeath

October 5th, 2007, 05:07 AM

Rbick:

Yeah, I noticed from your other posts that you were frequently using caps filled primarily with ETN, with just a little primary in there. That's certainly a smart idea, since it seems reasonable to assume that the less primary you have, the lower the probability of some going off at the wrong time. But alas, if for some reason even that small bit of AP goes off accidentally in the detonator, the whole thing still goes off.

Because I'm really anal about safety, what I'm actually most interested in is the possibility of a detonator that contains no primary at all -- only ETN. Since I've found ETN to be reliably detonable by heat even in small amounts when confined in Al foil, with the heat applied for a second or two to the outside of the foil, I'm pondering the idea of inserting a bridgewire into the ETN melt during casting with the two leads sticking out. When current is applied, it will rapidly heat the ETN around the wire, which is of course confined within the rest of the ETN casting, thus leading to detonation.

Do you think this could work? If no one else has tried it, then I certainly will at some point.

If the above doesn't work, then ETN still seems like a good candidate for use in a primary-free DDT detonator like the one described in the paper in this post:

http://www.roguesci.org/theforum/showpost.php?p=94912&postcount=23

Hinckleyforpresident (great handle, by the way :D):

One of the chemists here can correct me if I'm wrong, but the phenomenon you're seeing there might be what's referred to as "oiling out." Are you familiar with it? If not, there's a passage on it starting on p. 105 in a book called The Organic Chem Lab Survival Manual (2nd ed.) by Zubrick. Bugger recently put it (and an ungodly amount of other great stuff) on the Rapidshare thread:

http://www.roguesci.org/theforum/showpost.php?p=95622&postcount=719

This is only a guess, but I wonder if the reason it happened is that you used too much acetone and not enough water in your recrystallization. Dissolving your ETN in the minimum amount of acetone (or another solvent, as suggested by others) and then pouring it into a couple liters of water might prevent it.

On the other hand, your suggestion that this phenomenon could be used deliberately for casting-by-recrystallization is interesting. If you can replicate what happened, then at the very least it could be a useful property to know about. :)

Charles Owlen Picket

October 5th, 2007, 10:07 AM

@Hinckleyforpresident: This is not that unique at all....acetone is actually too good a solvent for ETN and is not used for re-crystallization for that reason. Try using ethanol or methanol and notice the difference..... You will be very pleased with the result. There are distinct reasons for this but for the sake of expediency -just give it a try and I think you will be quite impressed.

Rbick

October 5th, 2007, 04:52 PM

I would like to report a success with a ETN/NG charge. 8g of ETN was placed in a small dixie cup. I use them because they are wax coated. 2g of well washed NG was dripped into the cup. The contents were mixed and poured into a plastic bag. I was then able to mold the ETN/NG into a ball with the diameter of approx. 2.5cm. However, it could be molded into any shape and was very pliable and didn't come apart easily. The blasting cap was about .3g AP pressed into a straw and was initiated by fuse.

I have the video here (http://s164.photobucket.com/albums/u6/pudgedog69/?action=view&current=ETNNG2.flv), (it will also be available on my youtube page shortly) and the charge was quite powerful. The most impressive thing was the size. 2.5cm is very small, but the NG gelled the ETN so well that this small diameter was easily reached without using excessive force and risking detonation. I think I am most impressed with the size that I was able to compress 10g of high explosive into. This would be great for blowing heavy locks or for a strong booster charge in ANFO. Plus ETN and NG are some of the more powerful and easy to make explosives around. Having them together is a wonderful match :)

This explosive mixture is also very oxygen rich, and could be used to oxidize an added fuel, such as Aluminum.

To find the density, you take the volume formula of a sphere:

4/3 (pi) (r3) = 1.33 (3.14) (1.253)
This gives you 8.16 cm3
Now take the mass over the volume giving you 10g/8.16cm3 = 1.22 g/cm3

Thats a pretty good density for hardly having to press it. Obviously this isn't a precise mesurement, but it gives a ball park idea. The sphere wasn't perfect, but pretty even all the way around.

The down side was that the charge wepted NG. I had to keep it in a plastic bag to ensure none was lost. If I can find something that will help keep the NG absorbed, that would be most excellent :D