Erythritol Tetranitrate

[LibertyOrDeath]

Interesting photos, Charles.

Oddly enough (and fortunately, I suppose), my initial product has been very white in each of my ETN dreams. It didn't look nearly as brown as the product in those pre-refinement photos. And this was from using Rooto straight out of the bottle.

Was KNO3 used for that ETN instead of NH4NO3 by any chance? Maybe there's a "potassium sulfate versus ammonium sulfate" issue here as brought up by Rbick in the thread, "Why KNO3 sucks for nitrations."

The DuPont studies using a Falling Hammer (USBoM format 2.5kg) test equivocated ETN in it's re-crystallized form with NG in impact sensitivity.
I can definitely see how the recrystallized form would be more sensitive than the powdery product I got from purifying with acetone. The cast form seems to be much more sensitive, too (maybe equivalent in sensitivity to the recrystallized form).

As stated earlier, I've found that ETN in powder form is quite hard to set off with a hammer. HOWEVER: I've noticed that if a small lump is placed on a piece of Al foil, melted, and the small "puddle" allowed to solidify, then hitting that solid "puddle" with a hammer can make it go off fairly easily.

This has safety implications for those who, like myself, are interested in experiments with castings. People shouldn't assume that their castings (or recrystallized product) are hard to set off by shock or friction because their powder is hard to set off!

@LiberyOrDeath
I like the idea of non-primary bridge wire ETN caps. To test it out I took a tiny pinch and confined it in aluminum foil. Then I put it on my blowtorch. After about 1/2 second the ETN detonated with a loud SNAP blowing apart the foil and putting out the torch.Bingo. That's exactly what I've been seeing.

Tomorrow I will try some 1-2 gram ETN charges with 40 gauge nichrome wire running through them. I'll post videos and report on success or failure.Excellent! Looks like you're going to beat me to it. :)

I suspect that success will be more likely if the ETN charge is cast with the bridgewire inside. But maybe a pressing will also work. Either way, I'm excited to hear of your results.

[Emil]

That's a nice video BTW Rbick.

I think this explosive has impressed and turned quite a few heads. Ok it's still reasonably sensitive, but the yields are pretty damn impressive, no nitric acid needed (for those who have problem a obtaining it), and a great performance.

I really like the idea of an ETN cap. I personally don't find the HMTD I have been synthesizing to be dangerously sensitive (doesn't mean I don't treat it extremely carefully), however, reading through the AP thread members seem to state that AP is highly unpredictable.
Getting rid of peroxides and replacing with ETN sounds good for everyone.

I've ordered a pound of Erythritol from overseas so will be exploring it soon for myself. I just hope the UK customs don't seize it, because I know it hasn't been given the green light for use in the UK yet.
O well we will have to see.

[Charles Owlen Picket]

@BERT - There should be NO password what-so-ever on that RAR. It's a simple collection of ETN photos that show methanol and ethanol re-crystallizations.
_________________________________________________


When re-crystallization is performed and the body of the material (the crystal itself) is well defined the sensitivity and power is at the level of the DuPont product. With no exaggeration what-so-ever, an amount no bigger than than a capital "O" will yield a report from impact similar to a .22 cartridge.

ETN, if re-crystallized from an alcohol, will produce either a platelet or a hexagonal. That is what you are looking for (according to several patents, etc) to achieve high brisance & a VoD of 7200-7800 (depending upon the mechanics of initiation).

Re-crystallizations are best not attempted from acetone as it is problematic. However, some experiments of mixed alcohol and acetone (80/20) have been attempted in the past when eurythritol was less pure than available today. The casting of ETN using a hot water bath has virtually no issues IF the product has a neutral ph. However, I would not attempt casting ETN if there is any hint of acid left over.

[Emil]

Well last night I decided it was time to try ETN for myself.
My Erythritol had arrived, I had a spare few hours, and everything was looking good.

I used the method which axt mentioned at the start of the thread:

100ml HS2O4 - One shot drain cleaner 91%.
60g KNO3
15g Erythritol

I started first by adding the KNO3 to the HS2O4, in an ice bath, and cooling.
Additions were over the course of about 15 minutes. Good stirring was maintained throughout. After this had been completed I let the mix chill while I prepared 15g of Erythritol. My KNO3/HS2O4 was now a peach colour (My Sulphuric acid was originally pink).

I added the 15g of Erythritol slowly in portions, over about 5-10 minutes, so the temperature would stay reasonable. The mix now, like stated earlier in this thread, was becoming harder to stir and turning into a syrupy solution. Stirring was continued after all additions had been made, and this lasted around 15 minutes.

The mix was now a pure peach colour and quite thick so I was unable to really say if their were any visible crystals.
I now poured this into a liter of ice water, and the colour of the water turned into a light green. Instantly I saw little crystals forming and floating around, some went to the bottom and some floated on top. But I thought to myself that it looked A LOT less that 20-25g.

At this point It was getting late and time for me to hit bed, so I took the water/ETN solution and placed it in my fridge for the night.

Today I woke up to filter it and again was looking at the container in confusion. The ETN had all floated to the bottom, but I was still questioning the yield. So I started filtering it and from there it was looking worse and worse. It looked like no more than a gram in total :(.

It's sat here now in front of me drying. It's a slightly off white/green colour, but there is a small amount. It didn't even to manage to half fill a tea spoon.

A couple of notes overall on the experiment:

-I Noticed that my HS2O4/KNO3 mix became peach colored and found it hard keeping some of the KNO3 crystals off the side of the beaker. Is this Normal, or does coloring not really affect experiments? Maybe Next time I'll go the AN route. Stirring was via a glass cocktail stick.

- I did NOT have a thermometer, but all was kept in an ice bath, and slow and thorough stirring maintained. NO signs at any time of high temperature.

I thought possibly that it could have been my Sulphuric. However, I pulled up the data sheet for one shot and it does not contain any buffers or inhibiters. Just Sulphuric acid and a dye. So this leads me to believe that it's suitable for use. Any one else ever used one shot??

Other than that the whole experiment has confused me somewhat. Expecting 25 grams of lovely white ETN, I’m sat here looking at few pea sized wet lumps of green product.

I was thinking maybe I should have used more Sulphuric acid. Because if you think about it I actually only had 91ml of it. The other 9 ml would have been the dye. Could it be possible the Erythritol didn't actually get nitrated properly because of the lack of acid??? Or maybe I didn't leave it to nitrate for long enough (Only about 15 minutes after all the Erythritol had been added)?

I've just tried detonating it and it failed. I just try to burn it and it didn't do much apart from melting into nothing. I'm pretty sure it wasn't even ETN

In the big picture I’m still reasonably new to explosives so any comments, tips or help would be great.

[Charles Owlen Picket]

I read carefully your procedure and have a few thoughts:

When you prepare the solid nitrate and H2SO4, allow for completion of that reaction: make sure that the solid nitrate is completely dissolved in the H2SO4 and you have a clear solution. It's fine if heat (up to 40 C) is generated from this procedure because _at that point_ you will start to cool it for nitration. This should be done with either a magnetic stirring device or real patience.

Nitration from mixed acids has some time-dependent issues. I have seen GREAT success with the above procedure with no more than two hours of nitration. IF you are not getting results at two hours; something is problematic.

Temperatures in nitrations is very significant and a very important issue overall. I firmly suggest you get a thermometer. However the temps you are looking for are no greater than 20 C during your additions HOWEVER.....ETN is VERY forgiving and run-a-ways are very infrequent. Efficiency is achieved by controlling variables!

I strongly suggest you look to the above two issues. However, if you suspect your sulfuric (I am unfamiliar with the brand, etc) - cook it down a bit at 300 C. That will give you stronger acid and IF you have some impurities you may be able to isolate them in that process via layers in a sep funnel.

Don't give up! Keep notes, get a thermometer and try the above two suggestions if you didn't have clear solution in the solid nitrate/acid and strong stirring/two hour nitration.

[Emil]

Thanks a lot for the advice Charles that's a lot of help.

I am going to get a thermometer very soon so then I can properly monitor my experiments

I Find it interesting what you said about the Solid nitrate and HS2O4 mix. I think this was almost definitely where my fault is. You see there were still bits of KNO3 undissolved when I started adding my Erythritol. Now I know that I must spend more time getting that first solution correct.

I still think my HS2O4/Nitrate mix is going to turn peach coloured though because of the dye. Shortly I'll be purchasing my distillation apparatus, so I will purify it before I use it.

I do have another brand of drain cleaner called Knock out. But I won't be using that in my experiments for the simple reason I read it contains inhibiters and buffers. Not only that but it's a thick brown/black solution. Looks heavily contaminated

[LibertyOrDeath]

Since we're talking about things that can go wrong, SWIM once ran into an issue with purity of ingredients when making ETN. He found that even though a certain brand of instant cold pack had nothing but ammonium nitrate and water listed on the ingredients, there most certainly was more than just AN in there.

The first indication that something was wrong came upon opening the cold pack. Rather than the AN crystals appearing somewhat translucent and colorless as with previous cold packs that led to success, they were snow-white and appeared much more dry.

When added to the H2SO4, the contaminated crystals turned the solution sort of purplish-brown. SWIM was displeased but figured he'd go ahead with the process anyway. The resulting yield was only about 12 g ETN for 15 g erythritol, and the ETN is tinted brown in spite of multiple attempts at purification. (Its properties do, however, seem to be the same as the ETN he made in the past.)

Anyway Emil, I concur with Charles: Don't give up! His advice is good, and if following it doesn't help, then you may want to reevaluate your ingredients (e.g., make sure your KNO3 is pure if you don't already know that it is).

As far as making sure you have ETN: SWIM has found that confining a small amount in Al foil and hitting it fairly hard with a hammer against another hammer (or an anvil, etc.) makes it go off much more easily than hitting it with a hammer against concrete. Apparently the concrete absorbs enough of the shock to prevent detonation. It's surprising that the difference is as great as it is: i.e., SWIM has to hit it with a hammer against concrete many times to set it off, but one or two solid hits with a hammer against another hammer will do it.

If you haven't seen them already, these YouTube videos will show you how your final product (after drying, of course) should behave. Be sure to wear ear AND eye protection, as detonating ETN confined in Al foil will often spray bits of Al confetti in your face.

http://www.youtube.com/watch?v=52lgHJlPfWQ
http://www.youtube.com/watch?v=zCv-rXk4XAM
http://www.youtube.com/watch?v=IcUfJxqOwbs

[Charles Owlen Picket]

As long as we on on this subject let me say that by the complete dissolving of the solid nitrate within the sulfuric acid you accomplish two things. You set up a true nitration acid which is adjusted for temp, but you can also determine the purity level or if adjustments are needed in the physical form of the solid nitrate.

What I mean here is that once I saw the use of NaNO3 become either a real problem or work well by the actual form of the nitrate. When the chemical was ground to a single micron sieve size it went into solution with ease....As a heavy crystal it floated around and caused problems.

IF you are not getting complete solution (total dissolving of the solid nitrate) then you will have problems! Because you don't have a complete mixed acid and you have solid nitrate impurities floating around mucking up your nitration! Your best friend here is a coffee grinder as it's a Hell of a lot faster than a mortar & pistol but both will work.....see, you're solving the problems! By noticing the "floating around" of specks of solid nitrate, you've determined that there were impurities at work during the nitration and so forth.

ETN should be up and nitrated within 2 hours because it's an easily nitrated polyol and a solid nitrate/sulfuric mix is a high nitric acid nitration. What's more there is nothing wrong with cooking your sulfuric acid for a bit. At very least you will concentrate it but you may also find a "layer" on it from impurities (buffering) that can very easily be removed.

Good quality ETN are very well defined crystals that look almost like raw sugar and can be detonated from as little as half a match-head in a fold of foil struck with a hammer against a metal anvil. The tiniest bit should bring a report like a .22 pistol close to the head (loud & sharp). As soon as you get successful at the synthesis you will begin to explore the re-crystallization variations which allow the production of a great many things: a sensitizer for plastiques, a dry explos w/ properties similar to NG, a base for caps, & even a good starting point for a EBW cap product.....Keep going, it's worth it.

[Emil]

Libertyordeath:

Ha, It's funny you mentioned cold packs as that is a very relevant issue for me today. I have just received my order of cold packs, which I ordered online, and was not happy to see "Contains Urea and water" on the packaging. I specifically ordered those cold packs because on their site it stated "Contains AN and water". I wasn't too pleased at all. Just shows you should never trust packaging. I know Urea is not useless, but I could of obtained a larger amount of that for much cheaper than the price I paid for the cold packs..

I do have KNO3 from two different suppliers. Both claim that it is of high purity, but obviously that doesn't mean it is.

Charles:

Thanks very much for the advice. you have definitely got me eager to try again by eliminating some of my possible and probable problems!

I am going to boil my HS2O4 and observe what happens, and also reduce the crystal size of my KNO3 (My trusty coffee grinder is on the way). :D

I may also try with AN as the nitrate as I have some lying around that I could put to use. However, I don't really want to go using my AN carelessly. It's hard enough to obtain here and it has plenty of other primary uses than a solid nitrate. Hopefully I'll be trying again this week when I get some spare time, and I will post the results.

At least this particular synthesis isn't too greedy of it's precursors. KNO3 is available by the kg's. Erythritol is nice and cheap, and I'm not to worried about how much HS2O4 I consume at this time, beings as I'm more interested in solidifying a definite usable source of it. (Beings as I have to take the drain opener route, and it's not by choice either).

[LibertyOrDeath]

Emil: Arrrghh, they sent you cold packs with urea instead of AN? Talk about "bait and switch"... :(

Not to abruptly change the subject from things that can go wrong, but here's something else that might interest people.

Cooper's Explosives Engineering (pp. 159-161) describes a simple way to theoretically estimate the VoD of an explosive to good accuracy. I did this calculation for ETN and got just over 8,000 m/sec, which is a little closer to that of other nitrated polyols such as MHN. Perhaps this is a slightly better estimate than 7,650 m/sec? I'm not exactly sure where the latter figure comes from; the first post in this thread says it was obtained by extrapolation, but I'm not aware of the details. In any case, it's good that the two estimates are close together.

Here's how the calculation taken from Cooper's book was done:

Basic formula: VoD = 1.01*(1+1.30d)*[N*(M^.5)*(-H)^.5]^.5

Parameters:

d = density of explosive in g/cm3
N = moles of gas released per gram of explosive detonated
M = grams of gas released per mole of gas released
H = heat of detonation = -1414 cal/g (Urbanski, Vol 2, p. 167)

The reaction when ETN is detonated:

C4H6N4O12 --> 4CO2 + 3H2O + 2N2 + .5O2

(Note: To use this method Cooper describes, certain rules pertaining to which products are assumed to be created have to be followed.)

1 mole of ETN weighs about 302 g and releases 4+3+2+.5 = 9.5 moles of gas. So N = 9.5/302 = 0.031457 mol/g.

M = 1/N in this case, since all of the atoms in the ETN end up in gas molecules. So M = 31.789 g/mol

Plugging these numbers into the formula gives 8 km/sec (Cooper uses mm/usec, but same difference...).

[Emil]

Nice to see that Liberty. Quite interesting. I'm not sure where that figure of 7,650m/s comes from, but I know that's what is stated on wikipedia.
However, ETN compared to MANY other explosives, is quite a new material.
A lot less covered than many others so it's quite possible the VOD is closer to 8,000.

On other news though I am very happy to say I had a successful experiment last night with ETN.

Following Charles's advice, I decided to look into what went wrong with my prior attempts. Luckily in this case, it was going to be one of two things. Either my HS2O4 or my solid nitrate. Not to my surprise, it was the solid nitrate that I was using before. (KNO3) It's quite possible it contains contaminants.

I was going to do two experiments in one, but in the end I decided to forget the KNO3 route, and try some AN instead.
To save on chems, in case of another failed attempt, I decided to scale the experiment down half. Therefore using;

50ml HS2O4
30g Ammonium nitrate
7g Erythritol.

I decided to grind up the AN into a nice powdery consistency, using my new coffee grinder. It worked so much better this time round. From the start I could tell things were running much smoother. The addition of the AN to the acid gave me a nice thin liquid where the AN was easily dissolving. (compared to before where I had a horrible thick slushy mixture where some KNO3 refused to dissolve).

The AN/acid mix this time around was so much more clear in colour also, just having a slight tint of yellow.

After completing it all, I ended up with a nice white powder floating around the ice water. After filtering and drying, my yield was still reasonably poor. This could of been down to a few things.
For starters the AN had been previously weighed out, but when coming to weigh my Erythritol, I realized that I had left my pocket scales somewhere else. So in other words I could of added a wrong amount of Erythritol. It was just a guess.

Another could be my HS2O4 containing impurities. I didn't get round to boiling it to purify it this time, but that is definitely on the list for the next time round.

Something that did concern me though with my finished product is that I could not detonate it. It burned with a blue tinted flame when set alight, but it did not what to detonate no matter how hard I struck it. I placed it in AL foil on a hammer and struck it with a hammer as hard as I could numerous times, but each time I got nothing. It could be possible my ETN was slightly damp still. Could this prevent detonation??

There are still a few things I want to adjust with future experiments. And I have to try again with a different source of KNO3 and see what results I get.

[totenkov]

I made another batch of ETN yesterday and I'm a bit unimpressed with the results. I used pure Erythritol (15 grams) from the health food store, sulphuric drain opener (100mls) and reagent grade KNO3(60grams). Mixed the nitrate with H2S04 and it gave me quite a thick mix which surprised me.

Added Erythritol over 20 minutes, then let it nitrate for another 20. Poured it into 2L of water and voila! Most of the ETN sunk to the bottom of the beaker were a bit floated to the top.

I filtered it out, bi-carbed it and let it dry.

Final yield ~ 9 grams

I hear about people getting 100% yields! I dunno what happened but now that I think about it I probably should have ruin it through acetone to get any unitrated Erythritol.

Its been drying for 27 hours and I haven't been able to initiate it with a hammer. Could it not be dry yet? It sure looks pretty dry.

NEW: Yep, I just didn't let it dry for long enough. I just did the hammer test and it let loose with a big bang. ETN is still a lot more sensative than I first expected it to be, still an excellent explosive in my opion though.

[Hinckleyforpresident]

I would like to report two great successes with ETN.

First, I made 120 grams yesterday from 75 grams erythritol using the ammonium nitrate method.

Second, I made use of ETN's positive oxygen balance by mixing it with nitromethane and nitroglycerin. The ratio I used was 58:32:10. It was sort of a slushy liquid, perhaps it would work well in a shaped charge.

Here is a link to a video of it: http://www.youtube.com/watch?v=HZpzB3q4ABc

[LibertyOrDeath]

Emil:

If I'm not mistaken, that Wikipedia entry on ETN was written by Rbick. He might have gotten the figure of 7,650 m/sec from the first post on this thread, but he can correct me if I'm wrong. I just wish I knew more about how that figure was obtained, since it only seems to be based on one person's estimate.

7,650 is not unreasonable, but I wanted to investigate ETN's VoD further because it seemed a little low compared to other nitrated polyols (e.g., MHN has a VoD of 8,260 m/sec at max density), and I couldn't find any definite figure for ETN in any of the books I've seen.

Regarding your hammer tests, damp ETN powder will definitely be harder to detonate that way. If you want to test a bit before it's completely dry, you might try confining a TINY amount in Al foil (say, the equivalent of one-tenth of a matchhead) and holding a flame to the foil for as long as it takes. This test might work even if the ETN is slightly damp.

It probably goes without saying, but wearing earplugs and goggles is a very good idea even when setting off such small amounts. I even like to keep my hands somewhat distant from the the foil (e.g., supporting the foil on a table and then holding the lit match with pliers) when doing this test.

totenkov:

I suspect you didn't nitrate it long enough to get a good yield. Letting it nitrate for an hour or two with some stirring should help. Also be careful about keeping it cool if you weren't doing that.

Hinckley:

Good job with that composition and with the scaled-up synth. 120 grams at once is pretty nice. I'd like to try that at some point.

Were the times involved in that nitration very different? I.e., can you give some idea of how long you took to add the nitrate to the H2SO4, how long you took to add the erythritol, and how long you let the stuff nitrate? Did you change any other steps in the synth? Thanks!

[Hinckleyforpresident]

Hinckley:

Good job with that composition and with the scaled-up synth. 120 grams at once is pretty nice. I'd like to try that at some point.

Were the times involved in that nitration very different? I.e., can you give some idea of how long you took to add the nitrate to the H2SO4, how long you took to add the erythritol, and how long you let the stuff nitrate? Did you change any other steps in the synth? Thanks!

Here is the procedure I followed (from azidechem x10):

-240 grams of ammonium nitrate is slowly added to 175 ml sulfuric acid while keeping the temp below 25 celsius.
-75 grams of erythritol is slowly added to the acid/nitrate mix while keeping the temp 10-15. This is stirred vigorously.
-While still keeping the temp between 10 and 15 degrees celsius, 330 ml sulfuric acid is added while stirring vigorously
-This is allowed to react for 30 minutes, then crashed into 4 liters of ice water and filtered

I got about 120 grams of ETN from this.

[Emil]

Liberty:

Yes, my ETN was still quite damp. I only decided to try detonate it about an hour after filtering. There was still a significant amount of moisture present though. I've used that entire small batch up in the end, but when I next synthesize some, I will try what you said.

Its handling qualities are so much better. My damp HMTD still detonated with a solid whack of a hammer. After my attempts to detonate ETN, I would feel a great deal safer handling it for use in caps over HMTD any day.

I think my problem is also the same as Totenkov. I haven't let my mixture nitrate for long enough, thus receiving a poor yield. But I have many plans for ETN yet, so further experiments are in the very near future

[Charles Owlen Picket]

When I was a kid we used to weigh common coins and thus have a method of weights to use via a balance {I remember that an American nickel was 5 grams}.

Re-crystallization is quite important with nitric esters made from solid polyols. For longevity and consistency, getting the acids away from nitric esters is vital (& safer!). Re-crystallization also provides a method of determining purity and the re-formed crystal will release it's energetic potential substantially better than the crude material.

This is particularly true with nitric esters such as MHN or PETN where the needle shape of the finished product allows for an accurate weighing of final yield vs the possibility of moisture or debris influencing weight. Crude nitrobenzenes are almost a waste unless re-crystallized. Tetryl actually has a tough time being initiated unless cleaned up.

ETN when re-crystallized is stable and will maintain itself for years. But it is substantially sensitive: much more so than PETN. Don't keep the stuff in a container that has a friction bearing surface (screw top, etc). One of the most interesting things you can add to your experiments is to look at the materials in a microscope. Record the structures and shapes when utilizing various synthesis & Re-crystallization techniques. Note that crystalline structure often has an influence on energetic material....

[totenkov]

Right now my ETN is dry stored in a glass test tube with a rubber stopper, normally I wouldn't store it like this but I want it dry because I plan to use it on the week end. I think it will be fine like this.

And yes it is more sensitive than PETN however it is still an excellent explosive and will be fine if you don't throw it around.

[LibertyOrDeath]

Hinckley: Thanks for the scaled-up procedure.

Folks, I just did a different calculation to estimate ETN's detonation velocity based on another method given in the book by Cooper mentioned above. That book was recently put on RapidShare, and the method is given on pp. 73-74. Unless someone asks me to do so, I won't repeat the details here, since anyone can download the book and see for himself how it was done.

This method is stated to be accurate to within + or - 2.4% for 95% of 80 explosives tested, and to within + or - 3.5% for 99% of those explosives. That's darned impressive accuracy. My result for ETN was a bit over 8.2 km/sec at theoretical maximum density.

So, unless I fucked up somewhere, we have two different methods of estimating explosive velocity that put ETN above 8 km/sec. At least one of these methods is highly accurate. And then we have other nitrated polyols such as MHN that are also comfortably above 8 km/sec. Thus, I think it's very probable that the initial estimate of 7,650 m/sec is somewhat too low.

[Hinckleyforpresident]

Today I discovered that ETN can be plasticized (to more of a solid than a gel) with nitroglycerin and nitromethane in a 67:25:8 ratio (ETN:NG:NM). It must be allowed to set though for about an hour or else it will be more gel like.

The end product has a wet clay texture. Perhaps by using more ETN in the ratio a solid moldable mass could be formed.

This product is very different in texture than the one described in my prior post, that stuff really was a gel, this is approaching plastique.

[Charles Owlen Picket]

Tenny Davis has written one of the best damn articles in print (pp307+) on the stabilization of nitric esters. The use of diphynelamine is common as is centralite. But what is little known is that urea is a fantastic stabilizer as well!

The use of diphenylamine will show a blue colour in the presence of acids and that is all to the better. But urea will accomplish the same stabilization when used as a wash (saturated solution) when used with ETN or other esters.

This is particularly important when ETN is discussed in the context of a plastic composition. The use of ETN is similar to that of PETN as their relative sensitivities are similar; as are their needs in plastics for long term storage and stability.

[Alexires]

Hinckley - Have you tried leaving your mixture around to see if it bleeds NG?

Also, what is its sensitivity like (shudders at moulding a NG/ETN mix with hands)?

[Hinckleyforpresident]

Alexires-
I left some around for about 4 hours. It didn't sweat very much NG out, just a thin layer on the surface. Still though, I wouldn't recommend leaving it around for any extended period of time.

I haven't tested its sensitivity extensively, however the small amount that I have done shows it to be slightly less sensitive than ETN.

The 58:32:10 ratio works a whole lot better. It's not a plastique, but it's damn powerful and of roughly equal sensitivity.

[totenkov]

Guys I just need to warn you all.

Be careful adding your Erythritol when making ETN. I had made it many times and went ahead and added all the erythritol in large portions. Trying to make a very large batch of ETN. I came around the side of the house just 10 minutes ago and it was fuming and bubbling like crazy letting off giant clouds of N02. Scared me so bad. Now all I can smell is NO2 and my entire lab smells like it. Just because its hard to get a run away doesnt mean it can't happen.

I poured a ton of water on it and then went away, and then came back and it started spewing NO2 again. Be Careful out there!!

[Barnacles]

ummm, What on earth possessed you to leave a large up-scale reaction of dangerous compounds alone for 10 min? The larger the production the more can go wrong. And then you left again? nice. Generally when things go wrong, you dont just pour water and leave it to its means... People actually have to be present to control a reaction.

No offense but this is hardly a warning, it should read as, " I thought it was a good idea to leave a large reaction of dangerous compounds alone and something went wrong (no kidding).

Also you sound very young...

+++++++++++

Don't quote whole posts - The_Duke

[Charles Owlen Picket]

There are specific reasons for "up-scaled" reactions (specifically nitric esters) beginning a run-a-way and this can be controlled.
Frequently what occurs in mixed acid nitrations are both hot spots and layer temp fluctuations. Most people know that hot spots can be controlled by utilizing a magnetic stir bar or some elbow grease to continually move the nitrated material to new "zones" within the acid. When using a solid polyol (either mannitol, erythritol, whatever) attempt to screen or stir it so that the material defines itself as individual crystals. Lumps will "hot-spot" with ease.
Not making sure that the nitrated material is of a fine consistency and added in small portions (SLOWLY) is perhaps the biggest single thing that sets off run-a-ways. This (run-a-ways) can occur even with pentaerythritol which is generally an easy nitration if the material is added too quickly and lumpy. The greater the volume/weight of the material to nitrate, the faster the temp can jump due to a variety of factors in the midst of the nitration. Check out old pictures of industrial-level equipment in large scale nitrations. They have just a great emphasis on the automated addition mechanism as temp control; if not more.

The temperature issue is much more complex. If there was some effective way to control temp the majority of the run-a-way problems are dealt with. There was a list of coolants to maintain a specific temp but in general (& from memory) it goes something like this:
WATER, ICE, ICE / SALT, ETHYLENE GLYCOL / ICE, ACETONE / DRY-ICE (There are, of course, a great deal more and varied schemes here: I just can't remember them)
Until when you get to acetone/dry-ice you are talking about serious below zero temps that will inhibit all but the most intense reactions, etc. Remembering that if you get them too cold they won't bond.... What would be very "cool" would be a portable refrigerant tube mechanism to simply place in the coolant instead of ice!

[totenkov]

Well SHADOW3910 :rolleyes: After 10-15 minutes when the solution is at 2 degrees I always leave the reaction and come back to check on it to make sure it stays at an acceptable level. I have been doing so for as long as I can remember without incident.

Maybe you misinterpreted my post. I have made much larger batches than this with the exact same chems at the same concentrations with the same cooling. I think I got the runaway because off the eryrthritol being added to fast and my nitrate solution was near solid. In future I'm going to take more time with the synth, I was in a hurry, this is when mistakes happen, not because you are young. :rolleyes:

[LibertyOrDeath]

totenkov: Just for the sake of curiosity, how large (quantities of reactants) was the reaction that ran away on you? Thanks.

[totenkov]

300mL - H2S04
170g - KNO3
65g - Erythritol.


All in a 600mL beaker in a salt ice bath.

[Shadowmartyr]

I've been scavenging the bowels of the net for any kind of Erythritol synthesis information. I know it can be bought easily online but that is not an option for me right now, unfortunately. If anyone has any information on its synthesis please post.


Thanks

[Charles Owlen Picket]

Although pentaerythritol has a butt-easy synthesis Erythritol does not. It is a solid alcohol sugar that originally came from a certain lichen species & in some red algae - Apparently there is a complexity in that it does not occur year-round nor in all red algae....sorry. Considering how easy it is to buy; I just can't see working to synthesis it. Same issue with other solid alcohols....I would imagine that mannitol would be a pretty involved lab for a home chemist and why bother? It's availability is such that purchase is sure and simple; allowing concentration on the energetic [use of same].

[totenkov]

I have never seen mannitol anywere. Do you make it or where can it be obtained? I also did a quick serach to find that Mega says its unstable and other sourses say its a somewhat stable secondary. Is someone able to clear this up?

[Bert]

There is plenty of information on Mannitol hexanitrate (MHN) here- It has been used commercially as a base charge in caps. It has also removed several fingers from one of the more senior people here. Look harder.

[Up1]

2 days ago, I thougt of making som ETN, and I hade read whole this thread, and looking for all tips an prosedures that people have had an sucsesfull result with.
I had had the choise of going with Axt's KNO3 method, or go with NH4NO3 instead. My experiences with the Cold-pack AN, has shown to get a little bit thick, caused some wax or something. It get a little bit white to.
My experiences with my fertilizer KNO3 is that the mixture with H2SO4 gets a little bit thick to, but I solve that by heating it a little and continue.
I have had much bether yeld with NC when using KNO3 instead of NH4NO3.
So I choosed to go on with KNO3, cause I have read some people here have get low yeld with AN, and most of the people using KNO3 have had good yelds.

I weighted out 15 grams of Erythritol, and grinded it in my cofeegrinder.
Then I weighted out 60 grams of KNO3, and grinded it to.
I measured 100 ml of High quality lab H2SO4, wich costed me about 62 Euros over 1 year ago.

I started with cooling my H2SO4 in an ice bath until it was about -5 degrees C. Then I started adding KNO3. One topped tee-spoon at the time, and stirred rapidly for about 30-60 seconds for each time.
The temperature never raised above 10 degrees C, and I used about 10 minutes adding All the KNO3. It got very thick, and I stirred some more. It was some lumps of KNO3 that didn't had dissolved in the H2SO4.
Then I went to the stove, and put it on maximum in about 20 seconds, then turned it of, and put my beaker on it and stirred rapidly and watched the temperature. Suddenly it just solidify'ed almost totally. I got problems stirring it. I took it of the stove and checked the temperature, and it was about 10-15 degrees. For some reason I cooled it for some seconds, and stirred.
After 10 minutes of stirring, the mixture got normaly thick again, and I went to the stove. I thought that the reason it solidify'ed was caused by to fast warming. Then I did like I always do, and turned it on the lowest level, witch gives about 50 degrees C, and yes, I have checked it.
Then it all went well, and after about 5 minutes of stirring on the stove, it was gotten thiner, and the rest of the KNO3 lumps where gone.
I had it one the stove until it was at 30 degrees C.

Then I went to my "lab" and added 1 tee-spoon of erythritol and stirred rapidly. I stirred it about 30-60 seconds each time I added erythritol.
When I saw the temperature getting near 35 degrees C, I put it in the Ice-bath so it got back to 30. After all the erythritol was added, I had a thick mix, and I kept stirring. The temperature kept itself on about 30-35 degrees C, and didn't rise. After some minutes, some white crystals forming in the acid mixture. I kept stirring continuously for about 10 minutes, and then I just stirred for about 20-30 seconds about every 2 minutes.
I let it react for 30 minutes, and in the end the temperature started dropping. That may be because all the Erythritol that possibly could react with the acid had reacted completely or something.

Then I took a large spoon, and diged out all the acid/nitrate/erythritol mixture, and put it into about 2 liters of cold water. I stirred in the beaker some minutes an let it all stand there, so all the lumps dissolved, and all I had was fine white powder and liquid.
I filtrated the liquid and got allot of white clear powder. I washed it in 1 liter of 10% Sodium bicarbonate solution, in about 30-45 minutes, and then in 1 liter of hot water. Then I filtrated it and dried it. When most of it was dry it started smelling very weakly of acid or something, might be a essence of NO2.
So then I washed it again, the day after, in a 5% bicarbonate solution for about 30 minutes, and then filtered it, and poured about 0,5 liter of water through the filter. I dried it, and I got about 26,6 grams of ETN, which is about 71,67% yield. I didn't want to recrystallize it with ethanol, because the crystals where to small for my filters, at first, but time solved that(I tested with a small lump).
But I didn't want the stress and the smell, so I didn't do it.

When it all where sat for drying, I weighted 1 grams of ETN/water and sat it for drying 10 cm under a lamp on a coffee filter. I didn't thought I was near 61 degrees, but it melted. When it all where cooled down, I had left 0,3 grams of
powder and high dens lumps caused by the melting, and a 5 cm diameter piece of coffee filter impregnated with 0,3 grams of ETN.
I took a piece of plastic foil, about 5 cm diameter, and a similar piece of aluminum foil. I took 0,2 grams of HMTD in the middle of the plastic foil, and put a bridgewire igniter in the middle of it, and wrapped up the foil around the wires. Then i took the Al-foil and wrapped it around the plastic, and pressed it so it was dense. Then i had the 0,3 grams of powder ETN, in the middle of the filter with ETN, an put the HMTD detonator in the middle, and wrapped up the paper around it, and presses the paper like a ball. I took an Al-foil piece of about 7,5 cm diameter, and wrapped it around and pressed it to make it dens.
Then I taped it to a piece of wood, 30 cm long and about 4 cm wide, and put it in a pile of snow. Then I put some more snow on top. Then I detonated it with a 9 V battery, and it vent BOOM. It was a hard boom in the ground, cause the snow prevented it from making allot of sound, cause my neighbors shouldn't know. When it exploded the whole snowpile blinked white. First I didn't understand why, because ETN dosent make a lot of visual effects, but then I understood that the ETN had oxidized some Al-foil. Then I brushed the pile of snow away, and found 3 pieces. 2 that where about 10 cm, and one nearly broken in the middle 10 cm piece. I have some pictures of the wood, so I'm gonna see if I can upload it here somehow.
That test clearly showed it is allot of power in ETN.

Right now before I wrote all this, I was trying to plasticize som ETN.
I started with 0,9g of ETN, and then added 0,1g Chainsaw Oil.
Then i stirred it and tried to press together lumps with a stick, but it was just loose. Then I added 0,1g Oil more, and mixed it some more, but it was hard with the stick, so I used my fingers, and pressed it all together.
I pressed it and made a ball of it, and the consistence is nice, and very mold-able. After some cuddling and molding I weighted it, and it is 1,0 gram.
It's some oil left in the beaker I mixed it, and some got on my fingers, So I guess 10-15% Chainsaw oil works very nice. One day when I have more ETN I will scale up the test and see more accurate.
I'm gonna extract some PiB from "Grey tack" and plasticize it with PiB and the chainsaw oil, to see what we get.

This got a little long, but whatever. Glad to share my experiences!

[Shadowmartyr]

So I was following AXT's synth with the ammonium nitrate, I added a teaspoon of AN to the Sulfuric acid in a glass container. Instantly a white cloud shot out of the glass and went in my face. I was wearing a shield but no breathing protection. I'm afraid I inhaled a bit of this on accident.

I now have a bad headache. What was this gas? It wasn't NO2 was it? Kind of scared me a bit..I went ahead and dumped the chemicals.

[ex1ge]

HNO3 Vapour I beleive.

[Masonjar Chemist]

It was most likely nitric acid vapor. I have had experience with the headache you are referring to and can tell you that you can expect it to linger for about 5 hours after the inhalation. Nitric oxide (NO2) is a red/brown gas so it is unlikely that this is what you breathed. For future reference you may want you chill the sulfuric acid prior to the addition of your nitrate to minimize you loss of nitric acid in vapors.

[BlackFalcoN]

The vapour you inhaled is also mentioned in this thread:
http://www.roguesci.org/theforum/showthread.php?t=2461

Most likely the vapour was nitric acid or possibly gasious ammonia.

Both nasty things to breathe I'm sure, but nowhere as bad as inhaling NO2 (which will cause pulmonary oedema which eventually can be fatal due to fluids building up in your lungs and decreased oxygen absorption)

But since NO2 is reddish-brown, and the vapor you observed was more whitish, I don't think you should fear for your life.

( don't hesitate to consult medical help though if this gets worse; a nitric acid synthesis is nowhere as illegal/suspicious as for example a VX gas synthesis and certainly not worth getting killed/maimed over ;) )


Symptoms of pulmonary edema include difficulty breathing, coughing up blood, excessive sweating, anxiety and pale skin. A classical sign of pulmonary edema is the production of pink frothy sputum. If left untreated, it can lead to coma and even death, generally due to its main complication of hypoxia.

If pulmonary edema has been developing gradually, symptoms of fluid overload may be elicited. These include nocturia (frequent urination at night), ankle edema (swelling of the legs, generally of the "pitting" variety, where the skin is slow to return to normal when pressed upon), orthopnea (inability to lie down flat due to breathlessness) and paroxysmal nocturnal dyspnea (episodes of severe sudden breathlessness at night).

[rangegal]

Oh yes, your first nitric vapor. I remember how scared I was when I saw all those fumes coming out of my reaction vessel. I knew there was supposed to be some "fuming" but at the time I didn't really know what that meant.

You still need to be careful though, I do my synth's outside under a lean to, sometimes with a fan blowing in front of the vessel if its not windy. BUT lately my asthma has been recurring pretty bad. I've had to use my inhaler for the first time in a year, and I think its from stray HNO3 fumes lingering under the roof of my lean to.

A (miniature) fume hood, or a strong extraction fan would work great. You can make a mini fume hood by hanging an inverted funnel over your reaction vessel, and hooking it up to a fan with some tubing.

[Shadowmartyr]

Thanks for all the help guys. Headache is gone but my nose is still a bit numb so you would say to smells and such. I learned my lesson.

I also noticed when I followed the synth and crashed the nitration into a liter of water the container turned very warm to the touch...

[Hinckleyforpresident]

Thanks for all the help guys. Headache is gone but my nose is still a bit numb so you would say to smells and such. I learned my lesson.

I also noticed when I followed the synth and crashed the nitration into a liter of water the container turned very warm to the touch...

Sulphuric acid + water gets hot, this is very well known :rolleyes:, that's why you should add sulphuric to water slowly. Diluting it more will help cool it.

Also, your nose is numb from the fumes :eek:? Good god man! Stand downwind at very least. HNO3 fumes are not kind to the lungs (although better than NOx's). Some sort of safety measures should be taken, otherwise you're sort of asking to die of pneumonia.

[Rbick]

I also noticed when I followed the synth and crashed the nitration into a liter of water the container turned very warm to the touch... This is the exothermic reaction that occurs when sulfuric acid comes into contact with water. Don't worry, its normal :)

For future reference, when making your nitrating mixture with AN and Sulfuric Acid, try and keep the temperature as low as possible, even before beginning to add the material to be nitrated. The reason for this was discussed here (http://www.roguesci.org/theforum/attachment.php?attachmentid=992&d=1190786433) on the FTP. It is an interesting article, and I urge everyone who uses AN in nitrations to read it.

But basically, through experimental observation, it was seen that copious amounts of nitric acid were lost during the creation of the nitarting mixture when using AN. This will obviously lower the yield of your end product. In the experiments, quickly heated AN/Sulfuric Acid mixtures gave of 85% of its Nitrogen in the form of NO2 fumes! This greatly decreased the amount of nitric acid formed, thus lowering any nitrating potential. As the mixture was heated more slowly and allowed to stand, the amount of NO2 was greatly reduced, resulting in more Nitric Acid. When reading, also pay attention to the mentioned volumes and masses used, since these too play a part in the amount of Nitric Acid produced. From what I understand, they weren't trying to solve the problem of nitrating and creating explosives in this article, but from my own experiments, the information mentioned above makes sense.

I was able to confirm this with my own experiments using AN + Sulfuric to nitrate erythritol. I had begun to wonder why my yields had been so unsatisfactory until I read that article. Usually I let my mixture get to around 40*C - 50*C, which gave me horrible yields. Since then, I have kept the temperature at approx. 30*C and have been very picky about the masses used, which has increased my yields substancially.

Oh and also, perform your nitrations in well ventilated areas and/or with a gas mask. I use my "borrowed" M-40 mask from the Army :D It helps me sleep easier knowing I won't have respiratory problems later in life.

[rangegal]

It also helps to crash the nitration mix into water with ice or snow in it. Thats what I've been doing ever since my first guncotton synth when the jar got so hot it burnt my hand!:eek:

Headache is gone but my nose is still a bit numb so you would say to smells and such.

Hinckleyforpresident: I believe by "numb so you would say to smells" he means he is unable to detect smells, not that he can't feel anything in his nose.

[Emil]

When I tried my first ETN experiment, it was my first time dealing with a
HS2O4/Nitrate mix. I attempted my synthesis in my room, which was a pretty stupid thing to do. But of course, being new to everything I didn't know how much/if it was going to release any fumes.

Nevertheless, after about 5 minutes I decided it would be best to dump it all. The HNO3 fumes are released for the whole duration of the experiment, so outside with decent ventilation, or a fume hood is your only option if you cherish your lungs.

[Shadowmartyr]

Well, despite my problems the first time I gave it another go (outside :)) and got it right this time; here is the synthesis I followed. This synth was given on the Amateur pyrotechnics forum (now pretty much dead).


48g AN (Cold-pack grade)
100 ml 94-96% H2SO4 (Liquid Fire drain opener)
15g erythritol

The temperature outside was around freezing, so I left the H2SO4 sit outside to chill in a glass jar for 30mins (this is important as many have said above, if not cold outside chill in a freezer).

I added the AN in 3 big even amounts and stirred rapidly and continued to stir over about 10 minutes off an on. After the AN dissolved I let it sit for 10 minutes to cool and stirred occasionally.

Since it was already cold outside I didn't bother with an ice-salt bath but I recommend doing this if it's not cold where you live, since the jar will heat up from the nitration.

I added the Erythritol in about 10 even amounts over about 15 minutes while stirring rapidly when adding it and every minute in between off and on. After all the Erythritol was added, I stirred rapidly for about 2 or 3 minutes, then left it for 30 minutes to cool, stirring about every 3 minutes for 1 minute (this is important, I've heard of people leaving it to sit unattended and they come back and its fuming NOx gases).

After I had let it sit and stirred it I now proceeded to crash the nitration into a glass with a liter of cold water. It's important to stir the cold water rapidly with a glass stirring rod while slowly dumping the nitration in it. After the nitration was added almost instantly a brownish precipitate formed on top and in the bottom of the jar.

Some people recommend putting 3-4 ice cubes in the cold water before adding the nitration to further keep it cool since the acid will heat up when it comes in contact with the water.

After all the nitration was added I slowly stirred on and off for 5 minutes.

Then the ETN was then filtered by using a shirt over a pneumatic trough. After this the precipitate was washed off (still on the shirt over the trough) with 2 liters of baking soda solution (4 tablespoons baking soda per liter of water) to get rid of any remaining acid. The ETN was then washed with 2 liters of cold water to get rid of anything else.

After that I scraped it onto some newspaper and let the crystals dry. The crystals were then stored in an airtight glass jar (I heard the ETN produces NO2 fumes).

The final yield was around 20 grams after neutralizing/washing. I never did recrystallize it though but this can be done.


Just wanted to share my experience.

[Enkidu]

Unless you're using it immediately, you need to recrystallize and neutralize again ASAP.

[rangegal]

Are you going to test it?

If it works then this stuff sounds easy as hell. You didn't even monitor the temperature and you got it right! With some explosive synth's precise control of the temperature is very important, even in freezing weather!

Obviously some temperature control is still crucial with ETN, but not nearly as much as something like NG. Perhaps this is why some people felt it was safe to leave the reaction for a while, they took ETN's ease and simplicity for granted.

Of course, that theory is only plausible if your stuff works.

If it does I still recommend you use a thermometer though, as it is better to notice a runaway coming on the thermometer than by toxic red fumes coming out of your reaction.

This sort of worries me though, an easy and VERY powerful explosive is a double edged blade. If the feds catch up to it and figure its to easy for people to make, they're going to start watching/regulating erythritol, if they haven't already.

[Shadowmartyr]

Well, it was really cold outside and I gave it plenty of time to cool between reactions. And also the final product was a powdered kind of substance I'll probably mix with some type of oil to make a "plastic".

I'll be testing it today and I'll post the results.

[Shadowmartyr]

Unless you're using it immediately, you need to recrystallize and neutralize again ASAP.

How often should this be done? Nobody mentioned on storing it properly and the techniques involved.

[totenkov]

I don't know exactly what he means, if stored in an airtight environment away form impurities you shouldn't need to do this. ETN, like any explosive needs to be well neutralized before it safe for storage. Use some kind of indicator if you have it (litmus) because a too basic solution is just as bad as a to acetic one.

Recrystallizing refers to a method of getting rid of impurities, by dissolving the ETN into a solvent and filtering out impurities and then precipitating out the ETN and filtering out the new 'clean' product. Search before asking simple questions again.

Once neutralized ETN can be stored under water if you are paranoid or dry in a test tube. I have an old sample 3+ years in a test tube and it showed no sign of decomposition (it was stored dry). It was in a drawer at my lab bench and it had rolled to the back and I had forgotten about it. It was about 10-12 grams and detonated like fresh product.

[Enkidu]

How often should this be done? Nobody mentioned on storing it properly and the techniques involved.

Please UTFSE about recrystallization, storing, and stabilization of nitric esters.

You never properly neutralized it. Acid is still trapt within your crystals, which will cause decomposition.

You should only have to neutralize once.

[Charles Owlen Picket]

Without doubt; there is ErTN that has been stored after re-crystallization in a neutral condition for years and is as fresh and strong as the day it was born... And as a matter of fact I had written several pages myself on re-crystallization techniques and crystalline formats from differing solvents.

[Shadowmartyr]

Please UTFSE about recrystallization, storing, and stabilization of nitric esters.

You never properly neutralized it. Acid is still trapt within your crystals, which will cause decomposition.

You should only have to neutralize once.

Calm down man...

I used it a day after I made it, not an emergency or anything. I don't think I will be making it anymore anyways...I wasn't particularly impressed with the results of the detonation. I had 40g ETN in a plastic film cup with a 3g AP detonator. It was a full detonation but failed to do considerable damage to the tree I had it next to.

[Emil]

That's not ETN's fault. It's a good explosive with a high VOD. Just because it didn't do much damage to the tree you had it near, doesn't mean it's a poor explosive. Ever thought maybe that the plastic cup you used was a crap container to house an explosive in?? Try something stronger.

And theres no point in comparing its performance if your just going to randomly place it near an object your aiming to damage. If there if nothing to aid the direction of your impact then it probably won't be very effective. Im sure you are aware of what a shaped charge is???

[Up1]

Calm down man...

I used it a day after I made it, not an emergency or anything. I don't think I will be making it anymore anyways...I wasn't particularly impressed with the results of the detonation. I had 40g ETN in a plastic film cup with a 3g AP detonator. It was a full detonation but failed to do considerable damage to the tree I had it next to.

If you want to test out the power of ETN, you should make a lead block and test it once more. One three can be stronger than another.
If you have casted the ETN the brisans should be relative high, and ETN alone has alot of energy, so if you fuel it with aluminium it should get a clearly a little more power.
6439 Kj/kg alone, and still more oxygen to use.
C4H6N4O12 ---> 4CO2 + 3H2O + 2N2 + .5O2
3 mol ETN and 2 mol Al is oxygen balanced.
3C4H6N4O12 + 2 Al ---> Al2O3 + 12CO2 + 9H2O + 6N2
Thats just 5,61% Al, but it will help, and the brisans will not be far away from the maximum. The energy will be about 8029 Kj/kg.

[Rbick]

I recall making a 12g ETN charge back in the summer. It blew a substancially thick (about 3 in) tree clean in half, and it wasn't even a shaped charge. It was a live tree and very tough indeed. Your problem is probably due to your density. Density plays a HUGE role in the power of a charge. 1.6 g/cm3 is about where you want it to be for ETN. This means your 40g of ETN would fit within a 25cm3 space for maximum performance. :eek:. That is pretty darn small.

The difference between 1g/cm3 and 1.6 would lower the VoD and overall power by and extremely large amount. So when making your charge, if you have the means to do so, ensure you have reached a desireable density. Without proper equipment and saftey measures, this can be very dangerous, so do your research.

[Charles Owlen Picket]

I recall making a 12g ETN charge back in the summer....
From what I could find ETN get's awfully close to equivalent VoD of PETN (perhaps 94.85xxx% of it's total). Generally the same as PEN. However that figure can be altered (and the number did differ) when looking at research done in casts/melts of several experimenters. PETN doesn't like to melt :-)
I've seen a gram compressed within an Al cap body taped to a steel trash container and blow a fist size hole in it. - - Anyone who is not impressed with ETN either didn't make ETN correctly or is too jaded from working with CL50 in high altitude dets at Los Alamos.

[Rbick]

Well of course Charles, who here HASN'T worked with CL50? I heard mixing vasoline and potassium chlorate is more powerful anyway. :rolleyes:

I commonly use ETN as a booster in AN based charges or PLX compositions. Usually in small amounts, .5-2g, achieving detonations that primaries would never be able to. This saves a lot of material, and minimizes the need for use of unstable primaries. The largest charge of ETN I have ever used was 20g. Has anyone here ever used ETN in substancial amounts? Say 50g and above? (and of course remembered to press to a reasonable density :p).

I'm curious as to how a synthesis of that much ETN would work out. Such as the time needed and temperature control.

[Emil]

Yes, I think either earlier in this post, or in the other ETN thread (plasticized ETN etc), one of the members made around 150g in one synthesis. (I think it was Hinckleyforpresident).
They have also written down the procedure they used. Worked quite well for them I think. I guess it just takes a little more caution when adding your Erythritol to avoid a nasty run away reaction.

On my previous couple of ETN experiments, I had no problem what so ever with temperature. Nice slow additions, ice bath at hand. The solution never exceeded 10 Celsius throughout. I remember reading one of the members’ posts about adding the Erythritol in one portion.... and it turned out to be a bad idea. Maybe if your working with a larger amount of acid, you can also get away with adding more Erythritol at once (raising the ratios appropriately from a smaller experiment)

[Charles Owlen Picket]

I think you can scale it up to about +100gr (w/ solid nitrate mixed acids) and then you need to make some decisions. I don't think you can work with pounds levels as the cooling becomes too tough to control without much more sophisticated lab equipment. At the several ounce level you better have a pretty big stir bar as well. The material gets so thick; it's like stirring cold honey.

< My chlorate and vasoline plastique wouldn't form around the dial of the safe I was breaking into for the CIA.>

[Emil]

Charles.... Come on... what were you doing trying to use a Vaseline and chlorate plastique?... You should of been thinking along the lines of a shaped charge consisting of baking soda and vinegar. The VOD is SO much higher. :rolleyes:

That is a very good point though. Cooling and stirring becomes an issue to take into mind when scaling up experiments. I find the AN/HS2O4 is lovely and thin until you start getting half way through your addition of Erythritol, then it becomes more of a sludge than a mix. The KNO3 route is sludge from the start which becomes near impossible to stir by the end.

I recently bought a hotplate/magnetic stirrer and was tempted to use it for an ETN synth I did last night, however I was a bit paranoid on using it for the simple reason I wasn't sure if it was safe to have a PTFE bar whizzing around on the bottom of the vessel. After ETN starts forming I didn't want there to be a risk of the friction from the magnetic bar initiating any lose crystals. What are your guys views on this??? Safe to use or did I do the right thing???

I was recently thinking about a new idea involving cooling, which would probably be suited for cooling on a larger level. It would be relatively cheap and easy to set up. You know the pipe freezing kits that plumbers use? Well there are plenty of different types varying from different fittings to different sizes. But I was thinking about housing the beaker in a jacket (similar to what the copper pipes are surrounded with), and then you literally just apply the spray (Again different types but main one being CO2) inside the jacket.

This is able to easily freeze water, so given that fact, you should be able to keep any solution extremely cool. I'm going to look into it anyway.

[Charles Owlen Picket]

It's perfectly SAFE! Just to put your mind at ease I have a collection of stir bars and have used them with quite friction sensitive materials with no problems. The issue is that if you look closely at the stir bar in motion a very small portion is actually making a pivot on the glass; the rest is whirling through the material. It's pretty damn safe. I even have a "heavy mother" for exactly this purpose (stirring honey) and it was more $ than the damn machine!

One issue is that the hotplate potion can "wear out" in time. If yours ever does - Take it apart and look at how they use a thin hotplate material for it. mine was made in the USA but was not meant to last (IMO).

[Emil]

Excellent, that has made me happier now knowing I can use it next time. It saves a lot of hassle. It's not so bad using AN because you can stir with the thermometer without damaging it. But stirring is never usually the issue anyway, it's more stirring while avoiding the HNO3 vapors that keep rising off. Ill use a fan next time to direct the fumes straight out the shed door. It's too cold to be doing experiments stood outside lol.

I’m not exactly sure where my one was made, to tell the truth I bought it second hand anyway. It seems reasonably good. If it ever did go wrong though, I would possibly be tempted to get a Bunsen burner that is fed from an LPG container. Hotplates are not the cheapest things on the market.

After a few dismal attempts at ETN, I had a nice successful one last night.
My problem beforehand was that I was not leaving the Erythritol to nitrate for long enough after being added. This time I left it 30 minutes with stirring every 2 to 3 minutes. After neutralizing and filtering, I have 2 large coffee filters filled with ETN drying as we speak :)

I plan to test it soon, thinking that maybe a nice shaped charge may suite the bill.

[Rbick]

Please post your lab notes (either here or PM me). I'm curious to see your quantities, temps, times, ect. I find it useful to compare what others have done. A big part of scince is the free exchange of information :)

[Emil]

Of course. Well I start with my precursors.

HS2O4 110ml

I use 110 opposed to 100 as my Sulphuric acid is of 91%, and also make sure it is cooled in the fridge before use. It is the Drain cleaner brand "One shot". Soon I'm looking into purifying it further, as it only contains a dye (no buffers, inhibiters)

Ammonium Nitrate 60g

I have 2 different types of AN. Nice pure semi clear/white crystals (which you don't see so much of anymore. And the classic "fertilizer grade" which are the little white waxy prills. I use the fertilizer grade for most nitrations, and don't bother to purify it, just grind it up using a electric coffee grinder.

Erythritol 15g

The Erythritol I have at the mo' is granular, so again I grind it up via the coffee grinder, this way all my chemicals are a nice fine powder.

I start by adding my AN to my chilled HS2O4. I do this over the course of about 20 minutes to assure that the temp is easier to control (after all no rush:)). With nice constant stirring, I keep this mixture in the region of 10-15 Celsius via an ordinary ice bath. After all the AN is added, I leave the solution for around 10 minutes to cool to 10 Celsius and settle down. (Stirring every couple of minutes).

Now I begin adding the Erythritol. For some reason I don't find temperature such an issue with this part of the experiment, as it seems to remain around 10c throughout. (This doesn't mean that I am tempted to do it faster next time, as I've heard about the runaways) Addition of Erythritol is done over the period of about 10 - 15 minutes with nice constant stirring the whole way. Half a tea spoon at a time never seems to cause me any concerns with temp.

Now I leave the mixture for 30 minutes with stirring every 2 or 3 minutes. The beaker still remains in the ice bath all the way through this period. I've learnt from my previous mistakes of thinking 10 minutes of nitration time is long enough, and being punished with little or no yield. The mix, now like a thick creamy honey liquid, is crashed into a liter of fridge chilled water and stirred for a minute or 2.

After I've prepared my solution of Sodium Bicarbonate and water (Usually a 4%), the ETN/water solution is placed straight into this with good stirring. I let the ETN sit in this for around 5 minutes.
Filtering is a reasonably nice job with ETN, large coffee filters are used and the ETN doesn't seem to clog up the filter like other things can do. After collecting the coffee filters, a quick wash through tap water and it's ready to dry.

I'm thinking maybe I should work a bit more on my neutralizing stage. Some people say a soda/water wash is a smart thing to repeat maybe twice or even 3 times. What do you reckon? I haven't tried recrystalizing my ETN yet, because I plan to use it soon.

I'd appreciate your feedback and your lab notes also. Pm or post here. :)

[Rbick]

My lab results for ETN are posted some pages back in this thread. Multiple experiments using the same method and quantities have been done, so I see it pointless to repost them. They had excellent yields, so I didn't see a need to tweak them too much. One thing I did change was the time in which I added my AN, which I discussed earlier in this thread on page 29.

I also changed the way in which I purify my ETN as well. Usually I recrystalize after my first wash with bi carb. Then I do one more rinsing with bi carb/water solution and let it dry. I have had about 75g ETN in storage for approx. 4 months and hasn't decomposed what-so-ever and still performs well. It is kept in a sealed tuperware container with no exposure to light.

One mistake I found previously was when I tried to quicken the speed of drying my ETN. I placed a heat lamp over it, not directly, but enough to warm it considerably. Checking my thermometer, it only rose to about 26*C, not nearly enough to melt the ETN, nor cause an explosion. Upon checking my ETN only 2 hours later, I found over half of my ETN had disappeared! It had been decomposed by the direct heat and light :o So instead of a 20g yield I ended up with 8g... From this I learned its best to leave in a window to dry or just in the open air with a dessicant suspended below or above it.

[ex1ge]

I have also experienced what I believe to be the same problem as you, Rbick, the wet ETN was placed on a desk near a fan heater under halogen lighting, from a nitration of 8g of Erythritol only ~9g of dry product was retrieved.

[Charles Owlen Picket]

You can scale up with success the 110 / 60 / 15 by 3x with basically no heat problems to 330,180,45gr Erythritol and at this point you are getting a yield! Those are the figures I work with quite a bit. My typical re-crystallization is via methanol for more granular material. Ethanol continues to give thin platelets than although they pack well, they do not pour. However I do NOT use acetone. It's too effectual a solvent and the material is poorly formed from it.

[Emil]

Excellent, I'm quite tempted to give that a try next time. After going through the long filtering/neutralizing/drying section, it is nice to come out with a considerable amount of product for your troubles.

Yes I think I shall look into re-crystallization soon as that could play quite an important part of keeping my ETN pure and in good shape for any period of time. I haven't done a final weigh in of my ETN yet, but earlier I did a quick check and it weighed in at 35g! It was basically dry when I did this, only a tiny amount of moisture left, so I'm hoping final yield to be near or on the 30g mark. This would still be really high. I'll post results later.

I took your advice also Rbick, about drying the ETN. As I read your text I was just thinking of placing it under a lamp haha, I think you may have just saved my yield. I left it by a window for an hour or 2, and then just let it dry in the open air over night. It's not the quickest at drying, but I am nearly there now

[tijo77]

After some tests :

18 mL HNO3
33 mL H2SO4
12 g Erythritol

- Mix the acids (65/35 ratio)
- Acids are precooled (-15 to -5°C)
- Once mixed they are colled again (-15 to -5°C)
- I observed that the reaction between HNO3/H2SO4 can take a while to finish.

- Erythritol is then added in portions and the temperature is allowed to rise and is kept between 10 and 20°C.
- I Wait 30 minutes after last addition with occasional stirring.

- Added to cold water with stirring (the temp. rises)
- Cooled down
- Filtered/Neutralized

Quick drying method

- The very wet powder (I don't press it in the filters to avoid waste of time) is (more like a cream mixture) warmed to about 80 celcius degrees in a water bath (to avoid over-warming) so the ETN (now liquid) seperates and falls to the bottom.
- This is allowed to cool down.
- The water is throwed away and the solid cake of etn is dryded with towel.

- I suggest to incline the beaker to about 45° to make the cake easier to remove from the bottom. Also, melt the etn completly and don't move it after to make it completly free from water.

Casting and comments

- The dry cake of etn that took the shape of the beaker can be immediatly broken in smaller parts and casted the same way as above for sticks manufacturing.
- I let a hole in the center for the detonator.
- Yield is about 50-55% that way and it can be increased to 70-75% by adding 3 times more acids. But I keep the above mentioned method because it would be 2 or 3 times more expensive that way (3 times more acid for 1/5 more product is not worth it). Actually it costs me about 0.053$/g so about 8$ for a casted stick of 150g etn.
- With water, liquid etn looks as NG with water : it is milky. Free of water it is clear as water.
- Sometimes I got NO2 fumes when casting etn. I believe there was acid remaining (no fumes = good filtration). Could there be a possible decomposition ? (I never get over 90°C).

- ETN has shown pretty good chemical stability and GREAT sensivity properties. This is by far my favorite explosive.

- I use AP to detonate it, which means that I need to manufacture detonators short time before use for security and mainly because old Dimeric AP as sometime not been enough to detonate a stick of etn. (Ending in a loss of etn).

- I observed, with the above method, that when pressed hard to evacuate maximum water from ETN after filtration there is a big 50% of water remaining.

- Over all, ETN has an incredible and affraiding power of destruction...


I would really appreciate comments

[totenkov]

I applaud your work. This is a very good post, I have yet too see a good synth using HNO3. I have not tried your method but the synth looks sound.

Good work.

[Masonjar Chemist]

I agree, excellent post tijo77 :). I was just curious about this statement though.

I need to manufacture detonators short time before use for security and mainly because old Dimeric AP as sometime not been enough to detonate a stick of etn.


I am fairly certain that trimeric AP will not degrade to lower cyclic versions over time under normal conditions, so “older stuff” shouldn’t be any less potent than freshly synthesized AP. My apologies if I misunderstood what you were trying to say.

[Enkidu]

- Filtered/Neutralized

- Sometimes I got NO2 fumes when casting etn. I believe there was acid remaining (no fumes = good filtration). Could there be a possible decomposition ? (I never get over 90°C).

I would really appreciate comments

What neutralization techniques did you use? If you just wash the crystals with sodium bicarbonate soln, you don't neutralized the acid trapped within the crystals. However, if you dissolve the ETN in a solvent of your choosing, and then add a little bit of bicarbonate, you will get a much more complete neutralization.

[Charles Owlen Picket]

What method of ID are you using to ascertain that they are indeed, NO2 fumes? If you are seeing "red" fumes, etc - then I suppose there is no real need to go any further but if it just smells like the NO you are familiar with, there could be a few reasons (all workable). I have yet to cast materials that did not give some odor.

[tijo77]

Thank you for your participation.

I know this thread does not concern AP, but I read more than one time that Trimeric AP decomposes to the Dimeric form over time. However, this doesn't mean you are not right Masonjar Chemist. I you are, I think that the only remaining danger, if there is, with old ap would be its sublimation/recrystallization in larger crystals; phenomenon I observed on all my old batches, even the sealed ones (I often make bags you can throw, so they explode when it falls on a hard surface).

For the fumes I mentioned, they were yellow/brown and carrying an HNO3 smell. Also, the two times it happened (with quick filtrated batches) the ETN didn't stop to fume during solidification and had an oily layer on it once solid accompanied with HNO3 smell again.

That said, I generally get 15g to 17g of clean ETN using my method (to mention the yield). Theoretical is about 30g from my calculus.

[Positron]

Hi All,

What would you recommend as an initiator for ETN in a detonator? More specifically, what can you tell me about ETN's compatibility (degree of stability) with the following primaries: AP, HTMD, and MEKP?

Thanks...

EDIT: Added the following:

Because I am unfamiliar with ETN and it's properties, I am trying to err on the safe side. That's why I'd like your opinions. Anyhow, my ponderings:

Would it be necessary to completely isolate the primary's (with carefully selected types of plastic, for the MEKP) from the ETN? What would happen if the aforementioned primary's were intimately mixed with the ETN? Would any dangerously shock-sensitive compounds be formed over time? Would the ETN or the primary decompose over time, at the interface between the two chemicals?

[Charles Owlen Picket]

Hi All,What would you recommend as an initiator for ETN in a detonator?

Please see thread entitled "ETN: Thinking Outside the Box". It begins to address this issue.

[Positron]

Hi All,

We did another simple initiation test of ETN today. Like the other, this experiment was designed to be proof-of-concept only, with very little data other than the fact that it worked. I believe that this is a good starting point for further plate-dent and lead-block testing, with the use of:

1). Double-Salt primaries
2). 7:3 KCLO4/Al flash Powder
3). EBW's

...for initiation.

-------------------------------------------------

INTRODUCTION:

A ~1 gram sample of ETN was compressed into a .30 caliber rifle cartridge, and detonated by use of an exploding bridge-wire detonator.

ETN SYNTHESIS:

The ETN itself was prepared via the NH4NO3 and H2SO4 method. The ETN precipitate was washed several times with distilled water, and then washed 3 times in a strong NaHCO3 solution, then with another wash of water. After thorough drying, it was used in this raw (non-recrystallized) form.

PREPARATION OF BRIDGE-WIRE:

A 1/16" piece of #XX bare copper wire (I need to measure this...probably #36 gauge) was soldered between the ends of two pre-stripped PVC-insulated wires. Care was taken to not get any of the Sn/Pb solder on the bare copper bridge-wire itself (this would significantly reduce its electrical resistance, with the possibility of a consequent low-energy discharge).

The bridge-wire was pushed 1/8" into the back of an empty .30 caliber rifle cartridge, through a 1/8" hole drilled into the end. The wires were then J.B. Welded (using J.B. Kwik) into place for strain-relief.

LOADING:

14.1gr (.913 grams) of ETN was packed into the cartridge. The loading pressure was an arbitrary 16PSI, developed with a 0.3" diameter wooden dowel rod and a 5lb. weight set on top of the dowel for a consistent loading pressure. The ~1gram amount of ETN was pressed into the cartridge in ~200mg increments.

FINISHING:

A brass plug was turned down to .305" in diameter, and press-fit and J.B. Welded (J.B. Kwik) into the remaining 1/4" of empty space in the end of the cartridge.

SPECIFICATIONS:

Total weight with ~6" of lead-wire: 101.4gr
Body of detonator: .30 carbine rifle cartridge
Total mass of ETN: 14.1gr

ELECTRICAL DETONATION:

The detonator was placed in the middle of a large coffee can and surrounded by sand. An 80uF capacitor was then charged to a measured 600V, and discharged into the bridge-wire of the detonator via a total of 5 feet of #22 twisted-pair wire (10 feet total wire length). The resulting high-energy electrical discharge initiated the ETN to detonation.

ANALYSIS:

93% of the total detonator weight of 101.4gr was recovered. The brass was stripped into several elongated lengths, averaging approximately 1/8" x 1.0" each. The .305" diameter "plug" and the cartridge "head" (heavier brass that supports the primer) were recovered intact, and very cleanly stripped of any brass that would normally form the body of the cartridge.

All of the brass "strips" had a deeply sand-blasted finish.

Completed Cap:
http://www.choiceelectrophysics.com/forumfiles/EWF/14.1gr ETN DET.jpg

Remains:
http://www.choiceelectrophysics.com/forumfiles/EWF/14.1gr ETN DET Pieces.jpg

Wiring Diagram:
http://www.choiceelectrophysics.com/forumfiles/EWF/Wiring Diagram.jpg

The Bridge-Wire:
http://www.choiceelectrophysics.com/forumfiles/EWF/EBWwquarter.jpg

Explosion of the EBW Element:
http://www.choiceelectrophysics.com/forumfiles/EWF/EBW Explosion.jpg

Sound Dampener:
http://www.choiceelectrophysics.com/forumfiles/EWF/sounddampener.jpg

[Charles Owlen Picket]

Gives rise to some unique questions and nice work there! Could you give some detail on the voltage and current? It's source and the specs? - You had 600v @ what level of current & from what source? That's a pretty nice little presentation there: Good stuff!

[Bert]

Please describe the switching circuit.

A very minor point- That's a .30 carbine case. M1 Garand is a .30 '06 weapon (7.62x63mm); except for a some US navy ones which were .308 (7.62x51mm NATO).

[Positron]

Charles Owlen Picket: Thanks, and I do wish that I had voltage and current waveforms throughout the pulse, but I don't. I desperately need a digital storage scope! The only definitive electrical data that I have is that the capacitance was 80uF (160uF/2 as they're in series...) and the voltage was 600V (measured with a meter at the time of switch-on). Total electrical energy = (.5 * C* V^2) = 14.4J. (Remember that only a small percentage of this energy actually makes it to the ETN molecules).

Bert, thanks for clearing up the cartridge type. Indeed, it's a .30 carbine round.

The switching circuit was very complicated: touching two wires together ; )

For those that don't know, When two wires are touched together OR switch contacts close, the metal will mechanically "bounce" a tiny bit as it touches. This "bounce" can cause small air-gaps to occur just as the electric current begins to flow. The end result is possible unreliable explosion of the Bridge-Wire, caused by high resistances at the wrong time.

An infinitely better (probably the best) way to switch high currents is to use a MOSFET or IGBT transistor. Doing this completely eliminates such things as contact bounce, arcing, and metal corrosion from the picture.

Touching wires can work (it did in this case), but it requires statistical (very many tests) testing before it can achieve the Nirvana of being 100% reliable.

There are other options, but everything is a tradeoff.

[Man Down Under]

There's no bounce with a mercury switch.

[Positron]

I'm not so sure about that...

With the high currents normally used in EBW detonators, the mercury could conceivably be blown around with the quickly varying magnetic field surrounding the current path through the mercury. Although a different phenomenon than contact-bounce, it will likely cause similar problems. Sounds crazy, but I do believe that this would be the case.

I've never seen a mercury switch used in a high-current application, unless used in an ignitron under tightly-controlled conditions (vacuum & external magnetic-field shaping).

[Man Down Under]

Turbulent eddy currents may push away the mercury in contact with any one part of the switch, but that would push mercury up against another part of it, wouldn't it?

I'm just having a hard time thinking of a couple of photo-caps as being 'high current', as if they were an EDM machine.

If it's that big of a problem, make a stab switch.
http://www.wipo.int/pctdb/en/wo.jsp?wo=2001056049&IA=WO2001056049&DISPLAY=DESC

A "stab switch" utilises a piston means (usually in form of a pointed rod i. e. a nail) capable of penetrating two conductive elements. The conductive elements are held in open circuit, usually by an insulating material, and the action of the piston or rod penetrating both conductive surfaces and insulating material rapidly completes the circuit.

[Bert]

My gut reaction is that this is an electrically initiated DDT. ETN when confined is an easy cook off. Try it again with a commercial ematch or equivalent at low voltage and see what happens.

BTW, as long as you're essentially using a "sand bomb" for your testing, why not pre-screen the sand for particle size, then re-screen it after the test to show how much sand you've crushed? That data over a series of tests would be more interesting to me than pictures of the capsule fragments. If you have access to a sand blasting supplier, you can even buy pre-screened sand in various size ranges and of a consistent mineral make up.

[Positron]

Bert, Hmm, yep it's a possibility.

I wanted to try it with NiChrome to test it for cook-off...but, copper is easier to get ahold of for most people. And, it's easier to solder copper. (though NiChrome can apparently be soldered using ZnCl flux...)

Sand-crush is high on my list of things to do. That and trauzl tests.

Man Down Under, I have witnessed that when truly huge currents flow in copper braid, the braid is physically smashed and compressed inwards. This definitely lines up with what you said...BUT, I don't think that the forces would be as symmetrical in a little blob of Mercury.

[HotTime]

Although purification of ETN has been discussed in previous posts, there has always been limited detail for my satisifacton (unless I missed something) and therfore I ran some experiments of my own and wanted to post my results for comments or suggestions.

I purified three different samples all in ethanol (denatured alcohol). In the first process 30g of raw ETN were dissolved in 600cc of ethanol after first heating to 60 degrees C. After addition, the temperature was raised to 70 degrees C (above the ETN melting point). Two tsps of NaHCO3 were then added with rapid stirring. As NaHCO3 is not soluble in alcohol, this creates a suspension only with rapid stirring. The solution changed to a light yellow-brown color (presumably from the reaction of the NaHCO3 with any residual acid?). The solution was evaporated down to about 500cc and then filtered while still hot. The filtrate was cooled in an ice bath down to 10 degrees C and slowly poured into 500cc of rapdily stirred iced water (distilled water). The resulting precipitate was filtered out, rinsed with 500cc of distilled water and dried (it dried relatively quickly - less than 24 hours at room temperature). The result was 25g of pure white fluffy powder which was pH neutral.

In the second process, 65g was dissolved in 600 cc of ethanol heated to no more than 61 degrees C. Two tsps of NaHCO3 were then rapidly stirred in and the solution evaporated down to a final 500cc. Again, the solution turned to a light yellow-brown color. The solution was filtered hot and then cooled down to 10 degrees C. in an ice bath. This, unfortunately, resulted in a few crystals falling out of solution before dumping in ice water and these appeared to be larger crystals. This solution was then slowly poured in 500cc of rapidly stirred iced water. The resulting prcipitate was filtered out and rinsed as before. This was then dried, but the character of the crystals was decidely different than with the first process and took longer to dry. I have yet to properly examine the crystals microscopically. The final result was a pure white powder that measured 51g and tested pH neutral.

The third process involved dissolving 30g in 350 cc of ethanol after first heating to 60 degrees C and then elevating the temperature to 70 degrees C. This time 3 tsps of NaHCO3 was added to the solution with rapid stirring with a similiar change in color as with process #1 and #2. Evaporated down to 300cc, the solution was filtered hot, cooled to 10 degrees C and slowly poured into 600cc of iced H2O. The precipitate was filtered and washed as before. The appearance and characteristics of the crystals was similiar to the first process. It dried more quickly than process two and resulted in 25g of fluffy pure white powder which tested pH neutral.

Conclusions: I have concluded from this experience that one should dissolve 10g per at least 100cc of ethanol to avoid recrystalization beginning before the ice water "dump" and it is probably wiser to cool the filtrate down to only about 15 degrees C instead of 10 degress?
Heating the ethanol above the melting point of ETN (70 degrees C) appears to distinctly change the character of the final product.
The volume of iced water should at least equal the volume of the ethanol/ETN filtrate to be poured into it.
Although the NaHCO3 does not dissolve in the ethanol it appears to be effective in neutralizing any residual acidity and it does not appear to require much (I will be testing each sample for acidity in the months to come to see if any shows up).
It seems that a 15% to 20% loss of mass from the original raw product can be expected?

Any comments, suggestions or criticisms of these conclusions?

[-=HeX=-]

I have just returned from firing two ETN based 300 gram charges.

Confinement was 40 mm schedule 40 PVC pipe. Detonator was my standard 5 gram acetone peroxide cap.

Charge 1 was straight ETN at a density of 1.7 g/cm2. It was placed on a 1 foot diametre ash tree and taped on. It made a huge blast and blew the tree trunk to fuckdom and felled the tree.

The other charge was 60% ETN 40% HDN. Density of 1.7 g/cm2. That charge was placed on an identical tree in the same manner and dealt the same if not more damage to the tree.

No pics cos I was away from any phone or camera cos of my fear of static near caps.

[Emil]

Sounds good. However I can't help to notice your detonator you are using.
5 grams of primary is too excessive for ETN. You have to remember that ETN has a reasonably high sensitivity on the scale of HE's. There's really no need to put yourself at a high risk with 5 grams of AP, when 1 would be plenty enough.

The difference between 1 gram and 5 grams of primary accidentaly going off is vast. Especially with something crappy and unpredictable like AP, the chance of an accidental initiation is all the more realistic.

This is something you see alot, and mainly comes down to the issue of safety.

I would like to try a big charge of ETN sometime, it really is a great explosive.

[Deceitful_Frank]

I have just returned from firing two ETN based 300 gram charges.

Confinement was 40 mm schedule 40 PVC pipe. Detonator was my standard 5 gram acetone peroxide cap.

Charge 1 was straight ETN at a density of 1.7 g/cm2. It was placed on a 1 foot diametre ash tree and taped on. It made a huge blast and blew the tree trunk to fuckdom and felled the tree.


BS erm... BS!

Straight ETN at a density of 1.7g/cm... I take it you meant CUBED?
So you are pressing your straight ETN charges inside a black hole? With 3000psi I can barely get pure ETN to around 1.4g/cm3 which would be the equivalent of pressing with a force of over 4700 pounds in that schedule 40 tube!

Oh and your 300 gram charge felling a foot wide ash when taped to the outside. The blaster's training manual gives 3.6 pounds of TNT and thats for regular live wood so I'm gonna say IMPOSSIBLE.

[totenkov]

No pics cos I was away from any phone or camera cos of my fear of static near caps.

no pics cause it didn't happen :)

[-=HeX=-]

Deceitful_Frank: this is not bullshit. Yes I meant cubed but my formatting was fucked up due to using my 3G cell phone to format the post. I apologise for the confusion.

It was pressed using my fathers hydraulic ram thing which is rediculously powerful and can easily exert 5000psi. Its an intustrial thing which he uses for his work. It was at least that density and ETN IS WAY MORE POWERFUL THAN TNT!

Also, a military EOD I happen to know personally says that most training manuals way overdo the charge weight and you can get by with way less, 1/2 less in fact.

I respect your input but I have no reason to bullshit anybody here as bs costs lives. Any more
'input' frank?

Emil: I know exactly how shitty AP is, but due to lack of anything better at the moment, but I see your point. I guess I am just set in my ways for now.

[-=HeX=-]

Alright fellows. Looks like I have a lot of grovelling, apologizing and explaining to do. I would have edited my post but my phone won't let me.

I normally check out every variable when blowing stuff up but this time I made a bad mistake, I forgot to check the condition of the wood.

It was dead. Face wood is fairly common around here and the winter must have killed it off. So frank, I apologise for my mistake. The tree was felled because it was dead. In fact, half the bloody forest of trees are dead due to a bad winter which hardwood cannot survive (I study woodwork and we learn a lot about trees). And we all know exactly how weak and brittle dead wood is!

Totenkov: my only camera that I own is on my cell phone and like I have said, its a SOP to keep phones and other electrical kit away from detonators! I like having all my fingers and other appendages attached! I will obtain a digital camera as soon as possible. That is, depending on my currently limited funds. Once again, I apologise.

[NameWithheld]

My word probably doesn't carry any weight around here, but I would just like to defend HeX for a moment to point out that its perfectly realistic for 300g of high density ETN to take down a decently sized tree, assuming deadwood. And as HeX points out, deciding someone's claim is a lie based upon a manual's statistics is fairly unreliable... manuals are generic guidelines and always use significantly more than is truly necessary. I've taken down live trees (diameter approx. .5m) with less than 200g ETN when placed correctly.

That said, I've never even tried reaching a density as high as 1.7 (for powdered ETN). I'd personally be worried about it going off just from the pressure, but perhaps I'm just paranoid from working with too much HMTD...

[Rbick]

I was quite surprised when i saw 1.7 g/cm3. From every source I have seen, they say max VoD for ETN is 1.6 for best performance. Anything past that I'm assuming would dead press it, decreasing its power or disallowing it to detonate at all. I have never used a hydrolic press before, so I can't say much in the way of how realistic reaching 1.7 would be. Its not so much a question of if, but why. As Namewithheld said, I'd be in fear of it detonating.

As for the amount, after using ETN on several occasions, 300g taking down a dead tree seems reasonable. Considering the R.E. factor of ETN, extrapolated from that of PETN, is probably around 1.6. This means 300g of ETN is "equal" to 480g of TNT, 453g being 1 pound. Or if it was shaped, well the answer there is obvious. And my signature was actually taken from military explosives manuals, with the p in the equations being the amount of explosive to use. It was jokingly said that p=plenty because so much excess explosive was used.

[thelasttrueone]

I did a synthesis as per the specifications at the beginning of the thread, but with all reactants doubled and using 96 grams of NH4NO3 instead of 120 grams of KNO3. After the last addition I waited 30 minutes. The mix had cooled to around 5 degrees Celsius and I crashed it into cold distilled water. After this (in a regrettable fit of laziness) I went straight to filtration. I began filtering the first bit of the now quite warm mixture. When this was in the filter it started to have a runaway reaction! Obviously I crashed this out of the filter into my waiting "safety water". After this scare I neutralized the rest of the mix and filtered it without incident. The point of this is that there were obviously unreacted acids and erythritol even after waiting 30 minutes. Due to this I have always waited around 2 hours with my nitrating mix in my ice bath in subsequent nitrations, I have seen no reduction of yields. I was wondering if there are any thoughts on whether 1) why this happened or 2) if leaving a nitrating mix for too long has any negative effects. For reference my AN is from cold packs crushed in a mortar and pestle, My sulfuric acid is boiled down drain cleaner and my erythritol is crushed sugar substitute.

I also have a video of my a detonation of a 55g charge of ETN (this and 1 other nitration worth) but I am reluctant to post it should I?

[Hinckleyforpresident]

@thelast

Could you give us some info on how much water you crashed into along with details of the runaway? You sure you're not mistaking normal heating to be a runaway?

[-=HeX=-]

Its a possibility that some remaining acid reacted exothermically with the water. But acid to water is what you ought to so I cant see that being a possibility. Was the water warm or freezing?

I see no reason why you should not post the video. In fact, I encourage you to post it, I have to go without my fix until the summer. Actually, would you mind if I used it in a forum video a bit like THErAPIST did?

[Rbick]

thelasttrueone:

If you're not having problems with 2 hours, then go for it. I did have one experience where I left my nitrating mix for 3 1/2 - 4 hours. My buddy had come by and made me go to the bar with him for a while. When I returned, the mixture was totally dissolved and only a clear liquid with some brown crap in it remained.

The fact of the matter is: Sulfuric acid will dehydrate erythritol and ETN, taking its H and O and turning it into water. This will happened much faster if it is not kept below 20*C. So where 2 hours at 10*C might be ok, 2 hours at 25*C might not be. I personally keep it at 1 hour max and max temp. at 15*C just to make sure the Sulfuric doesn't start attacking my product.

[totenkov]

30 minutes is not enough for a complete reaction were anything over 1:15 will cause decomp. I usually leave my ETN reacting for about one full hour. Relax, it is perfectly normal for large amount of heat to accumulate during the water down.

[Charles Owlen Picket]

QUOTE:
".... After this scare I neutralized the rest of the....."

Do you understand what a "run-a-way" reaction is within the dynamics of a nitration?

QUOTE:
I also have a video of my a detonation of a 55g charge of ETN (this and 1 other nitration worth) but I am reluctant to post it should I?

If this is a rhetorical question then most people would answer from a standpoint of their own entertainment or amusement. If this is a question of whether you should from a standpoint of a legal or self-preservatory position then the answer is obvious.

[thelasttrueone]

Yes I understand what a runaway is, to clarify exactly what I saw and what was produced let me go into more detail. The funnel has about, say 150mL of the solution in it. It is sitting there, filtering slowly and bubbling. I didn't think this was all that strange until the bubbles started to have a brownish color. They picked up in their size and frequency until the entire mix was frothing like boiling water. I felt the side of the funnel, it was very warm. There was lots of NOx gas being produced and it was stinging my eyes and throat. I crashed it into 500 mL of water in a mason jar. The product I retrieved after this was very interesting. Strange crystalline structures of ETN had formed due to the heat and the bubbling. I believe that all those signs point to a runaway yes?

The water for the initial crash was another 500 mL and it was cold around 10 C from being in the freezer. I used 500 mL for my water crashes/neutralization because mason jars only go up to 800 mL and that was my only glassware at that time.

Hex I will send you the video if you pm me your email address.

[Charles Owlen Picket]

In your dialog you described placing the nitrating material into cold water and after which you saw bubbling brown gaseous material. That is, frankly, odd. Generally speaking the amount of water would dissipate the nitrating acids to the point of solvency where no NOx could be generated thereof. I suppose it's not impossible because it happened....but it's odd none - the less.

A run-a-way is a colloquialism [an expression] in some chemistry circles used to describe a reaction which speeds up to a point of lack of control, high exothermic generation: ruining the underlying reaction (note however it does not have to be exothermic in all cases). The casual factors involved in a nitration (which is what we are speaking of) are actually multi fold. Too rapid an addition of the material to be nitrated & lack of stable temp control being the most common. The lack of movement (stirring) can also create "hot spots" as the exothermic dynamics of nitration are always in play. On the flip side; too vigorous a stirring can also ruin the reaction by exposing too much of the material to acid too quickly for the cooling system to catch up.

Nitrations are the big Birtha of common chemical reactions as they are not easily organized & they are acted upon by so many extenuating circumstances. They are actually more of an art than a quantified reaction, many say. With each material, there are complex elements that interact with the (nitration) process. Polyols (solid alcohols) have a set or group of rules but those change when the question of "line crossers" is raised. When the process of nitration is learned many people look to the later half of the 19th century for techniques. It had been very rewarding for me, frankly to do so.
The lowing of the acid concentration will lower chances of exothermic activity in any reaction. So when the acids are dumped into water the process should cease as the acids are now too dilute, etc, etc.

[thelasttrueone]

This is my theory, as strange as it may seem. Adding the acid mix to water caused heat. I then added this to the funnel causing some water to filter out leaving enough acid and other reactants + heat to cause a runaway. I wish I had either kept some of those crystals or taken pictures, they looked like some kind of modern art.

I was reluctant to post this but I realized that I had proven a few things. Let your nitration go for more than the 15 minutes suggested in the beginning of the thread, Diluting your acids is no guarantee of safety and that ETN can and will run away given proper conditions. I will continue to study ETN and I will document more thoroughly with pictures and observations written on the spot. By the way, I think I will be doing a test tube sized nitration that I will purposely make runaway. Is there any chance of detonation? I understand the gases produced are dangerous so I will have my mask on this time.

[Charles Owlen Picket]

Oh shit, I've seen PETN nitrations in a run-a-way reaction. Most ANY nitric ester can do so given certain modalities: especially speed of exposure to nitrating acids. Heat's a killer!

Can run-a-way explode? [We know that NG pops all the fucking time,] but could a solid polyol? Yes, in fact the SMALLER the run-a-way the more likely the pop with a solid! Due to heating of the entire mass in unison with no cooling portion of the mass. it's easier to heat up a small mass than a larger one. And the critical level of heat prior to explosion would be easier/faster with a smaller mass.

I wish I had some old links but that's on another machine.....There is (was) a plant in Malaysia that popped and it was a PETN plant! Idiots at the helm fostered jackass policies & procedures. Looking to PETN for what ETN could do is not far fetched as the later is more sensitive but both nitrations are close in ratio & proportion.

I would not play with attempts at control of a run-a-way to examine the dynamics of the explosion....principally because you would have a great deal of difficulty controlling the time of the final approach (& the runway's on fire!).... a little joke there.

[Hinckleyforpresident]

@thelasttrueone

Did you not stir the nitration mix into the water to help cool it down :rolleyes:? Localized heating is normal when dumping sulfuric acid into water, and it will remain hot unless it gets mixed well. This is especially true with gel like reactions such as ETN where the reaction mixture will simply settle at the bottom as a blob while getting hotter and hotter.

My only runaway nitric ester reaction was with PETN, and rapidly stirring it and dunking the beaker into an ice bath cooled it down sufficiently.

[thelasttrueone]

Yea I didn't really stir, I think I may have swirled but I can't remember. My stirring rod (I only have one) was already clean and I was being lazy. I have revised my methods since then so don't worry.

[Lewis]

I have had good success with ETN synthesis in the past, but I've recently ran into some troubles. I've started using Ca(NO3)2 in stead of the ammonium salt, due to cost issues.

While the reaction goes along just fine, I can't effectively separate the ETN from the also insoluble CaSO4 once the reaction has completed. It's a huge pain in the ass, and for my own reasons I don't want to simply recrystallize the ETN from the mixture.

It would be much better for me to have a solvent with which to remove the sulfate, before filtering and collecting ETN.

On my first nitration with Ca(NO3)2, I simply dumped the nitration bath into cold water, as usual, swirled it to achieve maximum suspension of ETN crystals, and quickly decanted all liquids into another container (leaving behind mostly CaSO4, which is heavy and stayed piled at the bottom).

I was considering the possibility of removing the solids from the nitrate/acid mixture once the nitrate had dissolved, but no practical way of doing that came to my mind.

Any ideas as to how to streamline this process?

[-=HeX=-]

Lewis: how about simply filtering the nitration mix through a cake of 3 filter papers? KISS! Also, keep the sulphate for castable plaster incendiaries. Then, after filtration, continue the reaction with the filtrate.

Why do you not want to simply dissolve the ETN in acetone and recrystallise?

[Emil]

Well if your having issues with your nitrate, then remove your problems with it before you start.

If you were to purify your calcium nitrate, and remove all useless solids, then you wouldn't have anything to interfere with your reaction later on.

I had the same problem with Sodium nitrate that I buy in fertilizer form.
I tried my luck with it in its current state, which is quite contaminated,and my reaction was a complete mess up. The Nitrate was hardly even dissolving in the H2SO4, it pretty much just conjealed together and solidified into big lumps.

I purified it using the classic hot water route.
Dissolve as much of your nitrate as you can in hot/boiling water, filter of insoluble contaminents, cool and filter. Continue to boil down your filtered water until you no longer collect any crystals upon cooling.

This route does have its small loses in final product, but it is small and the results are worth it. From a white prill, I was rewarded with a crystal clear set of crystals. The good thing about this is that it is a very clean experiment to do with no horrible chemicals involved, and you can do the batches as big as you like (a Kilo of nitrate at a time).

[-=HeX=-]

Emil: I believe it is not the useless solids bothering his reaction but the calcium sulphate formed in the reaction Ca(NO3)2 + H2SO4 => 2HNO3 + CaSO4 As calcium sulphate is insoluble and coprecipitates with the ETN. He still should keep the calcium sulphate, waste not want not!

I wonder if this concept is good: make a collidon with methyl nitrate and NC, and use it to plasticise ETN. It should be a redicoulously powerful moldable explosive, albeit gives headaches. What do you all think?

[Emil]

The idea sounds good, however as far as plastic explosives go we have seen problems with these type of mixes before.

A perfect plastic would be a material like just mentioned, all 2 or 3 materials are energetics, and contribute to the power and performance of the final composition. Theres no inert materials which dull down the power, as with the likes of most plastic explosives.

But the mix is almost too good to be true and that's what I think it is. It would have power and brisance higher than c4, and would still be moldable.

The real problem is though its properties. I think we have found out before that most mixes which consist of a solid explosive mixed with a liquid explosive seem to lack the key factors that make a succesful plastique. The main fault we see with them are that they "weep" over time and don't really bind as they should. This does create problems over time, with storage especially.

If you were planning on using the explosive soon after mixing then this would probably be excellent. Another great point would be that you wouldn't have to worry about ratios, dulling down the explosive to the point that it won't shoot is not an option beings as you are using a liquid explosive as the plasticiser. This allows you to get a perfect mixture and saves worry of it being to dry.

This is only most of the cases I read, however I could be wrong and maybe there is some fully energetic plastic that someone has stumbled across which stores great aswell???

[Lewis]

Lewis: how about simply filtering the nitration mix through a cake of 3 filter papers? KISS!

Too simple.

Last I checked, sulfuric acid makes short work of paper.

[-=HeX=-]

Emil: it should not weep. The myrol and NC form a collidon or gel iirc. Then the ETN is added which thickens the gel to the right consistancy. The only problem is that myrol is volatile and evaporates. I feel another experiment being planned...

Lewis: I dont think it would eat a glass wool filter too well... :) try using fine glass wool as a filter. We used it as a filter in chemistry. It is inert and seems to work.

[Lewis]

Well, I went ahead with the synthesis. It was unremarkable in itself, but after that, things got hairy. I poured a thin stream from the nitration bath to a larger (and colder) water bath than normal. The result is extremely fine crystals of ETN and the sulfate. They are so fine that they pass through my usual cloth filters like they weren't there. I'm not sure what to do now.

I'll have to look into those glass wool filters for my next batch. Any idea as to where to look for them?

[-=HeX=-]

Glass wool is used in woodwork for lightly sanding softwood or varnish. I also found it as a line of scouring pad in the kitchen. Try a woodwork shop:)

Why do you not just dissolve the ETN in acetone and recrystallize? It would be the simplest way.

What ratios or amounts do you use? I use 238 grams of ammonium nitrate, 500ml of sulphuric acid (95%) and 75 grams of erythritol. Yield is around 105 grams these days after washing. They sometimes are 140 grams. What time do you let it nitrate for? What kind of yields do you get?

I have done a lot of testing on ETNs toxicity bye found it to be a good vasodialator and it gave less of a headache than nitroglycerine. Dont ask why I ingested it. I took 500 milligrams. It got me out of trouble. Any one else tried this? It was very very well washed and recrystallized from alcohol and acetone.

[Ethyl]

Dont ask why I ingested it. I took 500 milligrams. It got me out of trouble.


Out of trouble eh?:) Did you eat your detonator?:D:D

[Rbick]

Dont ask why I ingested it. I took 500 milligrams. It got me out of trouble. Any one else tried this? It was very very well washed and recrystallized from alcohol and acetone.

You're crazy man! I'm not particular on ingesting energetics. It is well known that PETN is used as a vasodilator in modern medicine, and since it is similar to ETN, I place my confidence in this fact.

ETN, like sugar, we'll say glucose for example, with formula C6H12O6, will be metabolized and used in cells for energy, resulting in CO2 and H2O biproducts which are passed through the urine and in exhalation. Erythritol is in itself a replacement for table sugar and is a polyol. It is a simple sugar and easily digested by the body. ETN obviously contains nitrate groups, unlike regular sugar, which will be released into the blood vessels and produce a dilatory effect. So from these facts we can extrapolate the effects of ingesting it, rendering the need to ingest it useless :p

Thanks for the information on the glass wool though. I will be finding some for the use of filtration. Having filters break is really is a pain in the ass.

[Lewis]

What ratios or amounts do you use? What time do you let it nitrate for? What kind of yields do you get?

I've been at ETN for a while now. I've changed all sorts of variables, but I'll try to get the basics together...

I've used equimolar amounts of KNO3, NH4NO3, and Ca(NO3)2 for reactions, ammonium nitrate giving me the best results, next would be calcium nitrate, and last, the potassium salt.

I've stuck pretty close to the original procedure in this thread.

I also tried one involving the use of minimal acid before the erythritol is added, and then putting the rest in after. (I think it was Mr. Cool's site?)

I generally use a little more acid than necessary, because no one likes stirring thick slop for long periods of time. I keep the temperature between 12 and 17 degrees C, and add the erythritol as fast as possible while still staying in that range. After the erythritol is added, I leave it for anywhere between 10-30 minutes.

Honestly, everything has always worked out totally fine as far as the nitration goes. I've never even come close to a run away, and the only failed attempts I've had were early on with KNO3. My issues arise with what happens afterward.

I've never been one for grunt work, and the whole process of washing/filtering/neutralization/recrystalization/drying has always been a pain in the ass to me.

If this CaSO4 issue is straightened out (and it should be quite easily), I encourage everyone to switch to Ca(NO3)2, unless their ammonium nitrate is very, very cheap. Calcium nitrate is perhaps the cheapest nitrate out there, and the agro crap I've picked up is way more pure than the other nitrates I've got from the same place.

[-=HeX=-]

I personally use ammonium nitrate due to its wide and cheap availability here, despite our domestic terrorist groups and spate of criminal pipe bombings. I have found the sulphuric acid the worst pain in the arse to find but found a source. I use more nitrating mix than is nesecarry to avoid partial nitrations but it helps with stirring.

In my last batch I used the following ratios:
NH4NO3: 238 GRAMS
H2SO4: 500 ML
Erythritol: 70 grams
Yield was 92 grams.

I think the yield was a tad low... Any ideas? Still, I am not complaining.

[Emil]

Hex:

It's always possible that it wouldn't weep, however my point is simply that you don't really see any "fully" energetic plastic explosives in use. I'm sure we would all agree that the military is pretty effecient in using the best materials/weapons available, and C4 has been the choice for a long while. I'm sure they've experimented with most of the things me or you would have, and the reason they haven't used any all energetic plastics pretty much speaks for its self.

However give it a good try and let us know how it goes! You may get some really nice results out of it. I suppose military organizations can afford to be picky, and maybe C4 meets their criteria perfectly. Of course we have to remember safe storage for them is the biggest concern, and we aren't talking months, more like years. They want to grab it out of the box exactly how it was when it was manufactured.

I have had successful results with plasticizing ETN. I personally used the silicone oil route. I have plenty more testing to do with getting a perfect mixture, and have now decided to use PIB as a binder. I will dissolve it in a solvent and then evaporate the solvent away. Hopefully this will result in a near on perfect material. My sample here is over 2 months old, and is still really good. It's only small but it sticks to pretty much everything and still retains some moldable features. The PIB will hopefully give it just an extra bit of binding strength and keep it from tearing under pressure. I just have to get round to testing some.

[drsx]

Hi!

This is my first post. I hope the Members of the Forum find it useful.

I read some interesting patents about plasticising.
To get rid of "weeping effect", try colloid silica, sold under the name Aerosil or Cab-O-Sil. It used in pharmacy too. It prevent the free flow of fluids, assist to reach a more homogenous mixture, higher the viscosity (making a thixotrop mixture), and prevent the "weep" of mixtures (water-oil mixtures, solid-fluid mixtures).

For the binding, I think nitrated galactomannan gum is a very good choice. I read one patent (the number of patent: 4112220, try search at http://freepatentsonline.com) about this nitrating guar gum. The reaction is working with 67% nitric and 97% sulfuric acid (both analytical reagents,
added slowly 2.5g guar gum to 8ml Nitric 12ml sulfuric). The patent describe the need of an organic solvent in the nitration process, but this is not a must.
The (probably partially) nitrated product detonatable at 0.7 g/ml density, and 0,7g in a 1mm wall 11mm inner diameter pvc tube initiated with 1g hmtd is more powerful than same amount of 0.8g/ml hmtd, concluded from the whitness plates.

When the finely pulverized nitrated galactomannan gum mixed with, for example, ETN-PGDN mixture (I mean I suggest to use PGDN, not methyl-nitrate, even though ETN is solvable in PGDN; try add 0.5-3g nitrated gum to 1g mix), and with 0.5-5 weight percent anhydrous Aerosil,
get a homogenous, thixotrop mix. To make a plastique-like product, introduce
to the mixture a very little amount of water (probably the -OH groups in the
not fully nitrated gum make this working), or I think, borax is usable for
this purpose. The patent describes the use of lead oxide as a crosslinking
agent for nitrated galactomannan gums.
I think, the (not fully?) nitrated gum also able to make a (partially?) waterproof skin in case of contact with water or humidity.

[-=HeX=-]

Emil: I am afraid I cannot Test the material due to lack of NC among other things. I may obtain some in july. All however is not lost: a friend in the united states tested it a month ago and emailed me the report he wrote on it. Unfortunately my email inbox junked it but I remember most of the details.

He added enough nitrocellulose to 100ml of myrol to make a consistancy thinner than toothpaste. (He did not make many measurements because he thaught the ratios would depend on the humidity and so on of the area) Then he got 250 grams of ETN and added myrol/NC to it while kneading and rolling out until he had a nice, homogenous putty like play do. He wore gloves for this part and still he got a headache from the myrol and had to have a rest.

When he came back later it had became stiffer and harder to mold so he added 10ml more myrol to loosen it up. He set it off unconfined and claims it was stronger than 300 grams of PETN, but its toxic and volatile effects are bad which is why it is not used commercially.

[ETCS (Ret)]

For those of you who have Calcium Nitrate it is very much advantageous to pre-mix the Sulfuric Acid and the Calcium Nitrate in desired proportions. Let the mix stand in a closed container in a darkened location until the reaction is complete and the Calcium Sulfate settles to the bottom of the mix. Decant the clear Nitric Acid off into another container leaving the Calcium Sulfate behind.

Then when the resultant Nitric Acid is used for ETN synthesis you'll not be plagued by Calcium Sulfate deposit intermixed with the desired compound.

Anhydrous Calcium Nitrate would be best, but as it is difficult to obtain, the Tetrahydrate too works exceptionally well.

[Ethyl]

Do you mix the resulting nitric acid again with H2SO4 before making ETN?

[-=HeX=-]

It probably has some sulphuric acid in with it ethyl. Otherwise, maybe it is like the PETN synth I will attach tomorrow to the PETN thread. The one using only nitric acid and pentaerythritol. Personally I think that maybe the calcium nitrate should be converted to ammonium nitrate but I cannot remember how.

By the way, I am currently, with thelasttrueones inspiring idea, and some ideas off frogfots site, working on a method of mass production of ETN. I think that it would be able to churn out about a pound per batch using automated stirring and various other Doo dads. I will compile it as a .pdf and post it here.

[Lewis]

I didn't have any luck with letting the nitration bath settle. I left it for a day or two, and when I came back it was still a opaque white goop. Perhaps the Ca(NO3)2 I started with was too finely powdered?

[-=HeX=-]

Lewis: That is possible, as that could lead to the sulphate being very fine and floating in suspension... Try it with coarser Ca(NO3)2 maybe?

[Lewis]

Indeed. The first time I tried with calcium nitrate, I used straight prills, and still managed to get a half-assed yield.

[ETCS (Ret)]

Ethyl (#365 above),

Yes, if the Sulfuric Acid and the Calcium Nitrate are mixed in proportions to fully convert the Sulfuric to Nitric. The resultant clear, decanted acid is used as pure Nitric Acid.

Before decanting let the mix settle for several days to assure that the maximum amount of Calcium Sulfate will settle to the bottom of the reaction container.

I've had very fruitful results with Nitric Acid made in this manner.

[Lewis]

ETCS, can you go into a little more detail on your procedure for nitric acid via this way? I've been grappling with this problem for quite some time now and would like some new ideas.

[Charles Owlen Picket]

Of the solid polyols ETN may be more flexible than even Sorbitol in it's proportions for yield. I'm not sure how many have even experimented with Sorbitol or MHN but they have a "right way" & a "wrong way" of production and very limited flexibility in their production. The former having a bit less demands than the latter.

As we can see, ETN has more than a bit of the standard ester flexibility in it's proportions of nitric acid in it's mixed acids prep. ....So let's do our best to get this back on track to a ETN directed thread as we are veering off topic to a HNO3 production discussion for a time here....

[Jetex Kid]

Here I am with a bowl full of ETN-in-alcohol, marveling at the complexity of Rosco’s crystallization procedure, which is more than my resources, time and patience will allow. I’ve been permitting very slow evaporation over about a week, resulting in crystals almost one cm in length.

And I’m reminded of how nitroglycerin in a slushy condition contains long, thin, sharp crystals that can concentrate force, making NG dangerous in that condition. And wondering how much force can be stored in a crystal, and contemplating the 19th-century pharmacist who lost his life while grinding the vasodilator with mortar and pestle. I find that I prefer working with theoretical explosives, which are much neater, safer, and don’t emit bad odors.

Using cast ETN would eliminate the problems associated with crystallization, and cast explosives are the most desirable form, since peak pressure varies with the cube of density theoretically (and the square, practically).

If cast ETN in the business-end of a blasting cap can be made to detonate, then the cap, if of sufficient size, would initiate a cast ETN charge. I intend to make blasting caps with progressively denser ETN on top of a cast ETN plug at the end, and determine how much ETN of what density needs to be on top of the casting to make it detonate. And yes, the ETN would be stabilized.

I am not quite sure what procedure to use to determine that the cast part of the cap undergoes high-order detonation, but I’m thinking of sticking the cap through a tight hole in a piece of steel with just the cast part sticking through, and visually comparing the condition of the fragments on both sides of the steel shield.

Also note that a diphenylamine/ETN mixture that is 1.9% DPA results in an oxygen-balanced explosive exploiting etn’s 5% positive oxygen balance to yield a theoretical 9% improvement in heat of detonation. (1.5% CH2, e.g. wax, produces 9.5% improvement.)

Comments, please.

[Emil]

I'm personally not aquainted with Rosco's recrystallization procedure, But from what I gather, a recrystallization is a reasonably hassle free procedure??

I'm lead to believe one can dissolve all his material in a chosen solvent, which has been warmed slightly, then crashing into ice cold water and filtering? Why not try this method. Evaporating liquid is a pain in the ass at the best of times, even a damp explosive is a pain in the ass to dry, let alone one suspended in water.

I've yet to cast ETN, but sounds like an interesting idea. The only thing is I'm not to sure how ETN measures up as a primary in a blasting cap. I know it's been mentioned several times, with the obvious advantage being it's relatively good stability when compared to peroxides and other primaries. I don't think I've ever seen a conclusion as to whether it can be done. Is it really sensitive enough to be initiated by flame when concealed?? Answers I do not yet have but I'm sure one of the members of the forum does.

If it was to be mixed with another primary in order to get a detonatable explosive under the given situation, it wouldn't be worth the time. Overall the final mixture would be slightly less sensitive, however you still have the sensitive explosive present, which can be initiated all too easily (as we know).

If it did work, I know myself. along with many others, certainly wouldn't ever be bothering with peroxides again.

And a cast explosive is the most desirable in my opinion also. It needs no pressing, and has pretty much no chance of accidental detonation via crystals initiating with friction from movement. Liquid explosives slosh about making them just as bad as powders. Of course you have a nice high density aswell.

[Lewis]

I still haven't figured out a procedure I like for producing ETN from calcium nitrate. Here are the notes from my latest attempt:

50g finely powdered Ca(NO3)2 was added to 100mL of room temperature H2SO4. The mixture was stirred and left to sit for 15 minutes.

At this point, the contents of the beaker were poured through some undyed insulation fiber in a glass funnel. With some patience and squeezing, 70 mL of white liquid was obtained. The nitration bath was placed on ice and cooled to 12C. 12g of powdered erythritol was added in portions. Little temperature increase was observed, and the reaction did not exceed 16C.

Once the addition was finished, the beaker was taken out of the ice bath and left to sit for approx. 25 minutes. It was then crashed into a liter of water.

A tiny amount of white ppt. (>.5 g) was observed on the bottom of the 1L beaker, once the contents had settled somewhat. The contents were discarded due to negligible yields.
---
The reagents are fairly clean. The H2SO4 is clear and pure, and erythritol is industrially produced and said to be 100%.

The calcium nitrate is agricultural grade, so will undoubtedly contain traces of moisture and organic matter. Still, to the naked eye it appears clean.
The insulation seems completely inert to whatever it is exposed to, so it is unlikely to be the culprit.

And input on what happened here would be greatly appreciated.

[Yafmot]

Keep silicone oil, or uncured or partially cured silicone AWAY from epoxy or anything that will be used with it. It is absolute poison to epoxy and permenantly contaminates anything it comes into contact with. The oil is just unbelievable. It creeps along under horizontal surfaces and has even been known to creep UP.

Anything you have around that has even touched the stuff will never be bondable with epoxy. Just the barest, most minute film of it can wreak havoc in a composites shop. A lot of large aerospace entities (Lockheed, USAF etc) won't even allow it in the plant. Some got loose in the composites lab at Aerojet Propulsion and effectively shut the place down for a month and a half.

Just thought I'd let you know.

[Jetex Kid]

Lewis, I have heard here at the forum and seen in print reference to Ca(NO3)2.3H2O. If you are using this, your nitric acid may have too much water to produce good yields. In some cases hydrates can be dehydrated by heating, but in others (e.g. (Mg(NO3)2.3H2O), the nitrate is destroyed before dehydration occurs. I do not know about calcium nitrate.

I let my KNO3-acid reaction occur at room temperature for about twelve hours, and got over 31 grams. I don't know if all this time helped, but fifteen minutes seems brief.

Good luck.

[Jetex Kid]

The only thing is I'm not to sure how ETN measures up as a primary in a blasting cap. I know it's been mentioned several times, with the obvious advantage being it's relatively good stability when compared to peroxides and other primaries. I don't think I've ever seen a conclusion as to whether it can be done. Is it really sensitive enough to be initiated by flame when concealed?? Answers I do not yet have but I'm sure one of the members of the forum does.

If it was to be mixed with another primary in order to get a detonatable explosive under the given situation, it wouldn't be worth the time. Overall the final mixture would be slightly less sensitive, however you still have the sensitive explosive present, which can be initiated all too easily (as we know).


Blasting caps used since WWI or so generally contain two explosives: a bit of true primary, usually lead azide, sitting on top of a non-primary explosive, such as PETN, or particularly nowadays, micron-size RDX. Or for that matter, ETN. They are all easily detonable and exhibit similar performance (peak pressure) at similar densities.

The flour-like consistency of crashed ETN would be a deal-breaker for manufacturers, who seek a free-flowing material compatible with an assembly line. Crashed ETN dries slow, won’t flow, has low bulk-density, and is a pain to work with, but it is something rogue scientists will tolerate to produce the Big Booms.

US Patent 2,204,059, which applies to PETN, ETN and RDX, provides a procedure for producing friendly crystals. Rosco Bodine, who now posts mostly at ScienceMadness.org, has provided a very detailed procedure and explanation based on this patent which I’d be happy to re-post, except it runs on for about two pages, and the whole point of my posts is to avoid it, but if anybody is interested, I’ll re-post it.

My goal is to produce a blasting cap that will initiate cast ETN, and I think this can be achieved by using a cap containing cast ETN at the end. The questions are 1) the width and length of cast ETN necessary to propagate the detonation into more cast ETN, and 2) the width, length, and density of powdered ETN necessary to initiate cast ETN.

While a cap containing only powdered ETN could be made to initiate a large charge of cast ETN, I would be more comfortable beginning the initiation of the solid ETN within the cap, as a guarantee.

Commercial caps contain compressed powder, and since pressure is a function of density squared, a cast-ETN cap should generate more pressure than the best commercial caps!

Of course I would welcome comments and particularly results from others’ experiments.

[drsx]

Blasting caps used since WWI or so generally contain two explosives: a bit of true primary
Yes, you're right, and you must use a primary too when you want a "safe" DDT. Some times ago, I made some comparative "cap tests". I hope the following will useful for you.

The charges
case 1:
0.3 g. lightly pressed AP as primary, and 1.5 g. casted ETN as secondary in 1mm wall 11mm inner diameter pvc tube
case 2:
1.0 g. 0.8 g/ml HMTD as primary, and 1.5 g. casted ETN as secondary in same tube
The tubes sealed in both end with tissuepaper soaked in liquid epoxy. For timing, I used a simple commercial "blackpowder cord".

The whitness plates
in both cases are two coins:
coin1 d=16,3 mm, Cu Ni Zn, 2,05 g.
coin2 d=19,2 mm, Cu Ni, 3,10 g.
The coins secured to the bottom of the secondary charge, and the testcharge placed to the ground.

The result
case 1: the coins only indented, mostly plastic-elastic deformation, a _little_ "flowing" on the coin's surface because the pressure deformation
case 2: the coins shattered, coin1 more than 4 pieces, and in both coins clearly seeable the pressure deformation

My conclusion
Although ETN is a sensitive explosive with relatively thin critical diameter, she is not a primary, and to achieve the full detonation, proper initiation is a must.

[Charles Owlen Picket]

I have worked with EBW mechanisms for a few years and can say with some confidence that IF the individual experimenter knows how to set up the system....a primary-less cap is actually available for the hobbyist.

[Emil]

Interesting. My ETN that I have been storing for a couple of months now, has started to form needle like crystals all around the edge of the container.
They are really long and thing, almost look like little splinters of glass.

Am I right in thinking these needle like structures will be more sensitive to initiation?? If so I would like to remove it. I know ETN is a relitivley safe material, but even so. Or is this normal and I am just worrying for nothing???

The HMTD is fine, it is double the age and just remains the same structure as day one. Any feedback would be great guys. Cheers

[Rbick]

I have never seen this before. I stored a batch of ETN for nearly a year without any changes in structure. What were the storage conditions? How well did you wash it? More info will better help us understand your situation.

[Emil]

Well this could be the exact results I was looking for. I was basically testing a couple of materials to see how well they kept in storage without re crystalizing them, just out of curiousity.

They were just washed in a bicarb solution and then left to dry. There seems to be alot of nice needle looking crystals all over the ETN. It is stored in an open container, nice and dry. This is interesting to me as I was observing the conditions of them over time. The HMTD is twice as old, and hasn't changed what so ever, but the ETN looks like it is now starting to develop a strange crystal structure. I wonder why.

There is no signs of impurities or change of colour, just a shed load of these new crystals. Am I right in thinking that in general, long needle like crystals are usually a more sensitive type than that of a small even shaped one?

Well it looks like I have definitely found another good reason as to why recrystalization is such an important step.

[Charles Owlen Picket]

Re-crystallization is pretty much mandatory but I'd also suggest getting a microscope. Your needles indicate that the ETN is seeing as much acid as is practical. PETN forms needles naturally. ETN forms platelets. But you can tweak either to make whatever crystal form you want within reason by several factors.

A good microscope will allow you see if there are any large contaminants as well as the actual formation of the needle, etc, etc. There are very unique things that info can tell you.

What's more, you had better buy one soon before some idiot in Texas introduces a Bill that bans microscopes and petri dishes together in the same building.

[Setharier]

Is there phossibility that ETN would detonate if heated in flask floating in water over 60C that's warmed with torch? And if one casts it to an inch thick bar, could it detonate when cracked into pieces with bare hands or cutted with some sharp tool like knife? I'm planning of making some kilos of it and casting it into bars ready for use and able to cut them in smaller pieces like chocolate bar by casting them on some sort of ice cube dish.

I found out ratios to H2SO4(98%)/HNO3(90%)/Erythritol as 110g/140g/20g. I wonder what is the correct ratio when HNO3 is changed to KNO3? Call me yanker if it's the same.. :D I would like to use KNO3 stright for this instead of boiling it with H2SO4 to make HNO3, even it would be somewhat easier to stir.

[Intrinsic]

Setharier:
Did you even bother to read this entire post? I know it is 16 pages long, but if you want to know about a subject, you really should read the available info before asking.
Had you bothered to read it, you would have found in the very first post the answer to your question about using KNO3.

Also I am sure you realize that it is not as simple as boiling KNO3 and H2SO4 together to get HNO3. :rolleyes:

[Charles Owlen Picket]

Thank you Intrinsic ..... Yes, Setharier, you really HAVE to read the thread. There is a remarkable amount of information about the subject. I know a wee bit about this material. It is fascinating and some of the most remarkable things about this are it's history within the professional industry via the two giants and their vying for it's patent. There are some links to patents that have within THEM even more esoteric information.

One thing I personally do NOT want to do is retype information. This type of spoon feeding & repetition is actually a sin within this Forum. As another member has directed you, I will allow this as an abject lesson but many take this as appeasement and would castigate you or worse. I ask you formally NOT to repeat this type of behaviour; but to use this forum as a resource. NEW questions - even quite esoteric ones are welcomed; repetition is boorish & boring. Recognize the need for this and all will be well.

[Hinckleyforpresident]

Is there phossibility that ETN would detonate if heated in flask floating in water over 60C that's warmed with torch? And if one casts it to an inch thick bar, could it detonate when cracked into pieces with bare hands or cutted with some sharp tool like knife? I'm planning of making some kilos of it and casting it into bars ready for use and able to cut them in smaller pieces like chocolate bar by casting them on some sort of ice cube dish.


The idea of cracking cast bricks ETN is just asking for disaster to strike. Your snapping of an "ETN chocolate bar" is really no better then snapping a 2cm TCAP crystal; only instead of ripping off a finger or two it kills you.

If you value you life and wellbeing, never go about breaking large crystals of any explosive that is even REMOTELY sensitive. A safety conscious person would not even think of breaking large crystals of more insensitive explosives just out of good practice.

Here are a few things I recommend you study before considering such an act:

-Stability of ETN crystal structures (recrystallization from MeOH, straight from formation, cast, etc.)

-Casting ETN (can turn nasty, a member had a little mishap while casting once)

-Explosives safety

-Common sense

[NameWithheld]

Is there phossibility that ETN would detonate if heated in flask floating in water over 60C that's warmed with torch? And if one casts it to an inch thick bar, could it detonate when cracked into pieces with bare hands or cutted with some sharp tool like knife? I'm planning of making some kilos of it and casting it into bars ready for use and able to cut them in smaller pieces like chocolate bar by casting them on some sort of ice cube dish.

I found out ratios to H2SO4(98%)/HNO3(90%)/Erythritol as 110g/140g/20g. I wonder what is the correct ratio when HNO3 is changed to KNO3? Call me yanker if it's the same.. :D I would like to use KNO3 stright for this instead of boiling it with H2SO4 to make HNO3, even it would be somewhat easier to stir.

Due to my job I haven't had much time to post recently but this definitely requires some warnings.

I believe Hinckleyforpresident was actually referring to me when he spoke of a member mishap related to ETN casting.

Most of us are aware of ETN sensitivity in its powdered form. If you melt it you can throw those properties out the window. You will notice the melting powder separate into two or more layers of oily liquids. The heaviest of these layers is very sensitive to fizzling and igniting at low temperatures. Once ignition occurs, DDT usually follows within 20 seconds. There are very few good ways to put out a fire involving burning liquid high explosives- your best bet is to run.

If you melt it and cast it there are definite sensitivity changes as well, which you can confirm with a drop test (I've got the numbers, but I'm not at home..).

This stuff DDTs like mad. You can take straight powdered ETN and use it as a primary by running nichrome wire through it and applying current for a few seconds. The ETN melts, boils, fizzles and then DDTs.

Before you go making your Kilos of cast ETN consider learning enough chemistry that you don't have to ask for chemical ratios. These things can be figured out.

[Positron]

Hi All. This is just a quick report on my recent experiences with the stability of a small batch of ETN.

Made some ETN via the NH4NO3/H2SO4 method. The ETN precipitate was washed several times with distilled water, washed 3 times in a 10% NaHCO3 solution, then another wash of water. It was NOT recrystallized.

The ETN was tested "good" in a detonator, and the remaining ~3g of it was stored in a plastic pill bottle and placed in a dark outdoor shed from January to August. The shed is located near the Gulf Coast.

After 3 months in the shed, no changes to the ETN's physical properties was noticed. Tens-of-milligram amounts of it gave sharp reports when placed on an anvil and hit with a hammer.

After another 4 months (August) the ETN was a soupy, yellow, gelatinous, runny gooey mess that reeked of Nitrogen Dioxides. Some bubbling was apparent by the looks of it.

End.

[-=HeX=-]

It was NOT recrystallized.
After another 4 months (August) the ETN was a soupy, yellow, gelatinous, runny gooey mess that reeked of Nitrogen Dioxides. Some bubbling was apparent by the looks of it.

End.

Well there lies your problem - lack of recrystallization. This lead to some acid being locked inside the crystals causing slow decomp.

Out of curiosity, what ratios of NH4NO3, H2SO4 and Erythritol did you use? What primary do you use? Was the 'soup' detonable? Maybe try to 'set it off' to see if any ETN is left in it.

In a few weeks when I have time, money and erythritol I am going to try a 'Dynamite' which cuts ETN and NG with EGDN and Ammonium nitrate. It will be 10% NG, 10% EGDN, 30% ETN, 5% Nitrocelluloce and 45% AN. then I will try cut out the NG and replace it with Ammonium nitrate, corn flour or polyisobutalene. I estimate VOD at about 5000 - 5500 meters per second.

[thelasttrueone]

I have a similair report on decomposition. The ETN I made was with the NH4NO3/H2SO4 method as well. The ETN was filtered, washed with water and put in a 500 mL sodium bicarbonate solution(saturated) overnight. This was not enough to totally remove all traces of acid but I was out of time.

When finally dried and weighed the ETN sample was 45.5 grams. Now, about a week later the same sample left in open air, indoors weighs a mere 39.8 grams.

From this and positron's post we can probably conclude that speedy recrystallization is very necessary if you want a stable, long lasting product.

[Deceitful_Frank]

From this and positron's post we can probably conclude that speedy recrystallization is very necessary if you want a stable, long lasting product.

It is indeed.

For me, ETN is one of the most powerful and cheapest to make explosives at my disposal as I can use inexpensive yellow dyed drain cleaner and technical grade prilled AN.

This does result in an impure product but when a hot saturated purple solution of ETN in MeOH at 60 celcius is poured into three times the volume of icy water, a fantastically stable and pure white precipitate finer than bread flour is rewarded to the patient chemist who is willing to go the extra mile and take the time to produce an excellent sample of this truly fantastic explosive.

When ten grams per metre bead is wrapped in a constricting layer of self amalgamating tape there is no end to the fun that can be had.

[-=HeX=-]

When ten grams per metre bead is wrapped in a constricting layer of self amalgamating tape there is no end to the fun that can be had.

By this do you mean improvised Detcord, or some kind of plastique? I am unfamiliar with this 'Self amalgamating tape' material. Maybe some media could help, or just a detailed explaination. Is 'Self amalgamating tape' the stuff in the following link?

http://www.tapes-direct.co.uk/index.php?main_page=product_info&products_id=939

Just curious...

[Positron]

Sorry, I didn't mean to sound "surprised" that my non-recrystallized ETN went to crap. I'm very much aware of the fact that it must be recrystallized for long-term stability.

However, (referring to thelasttrueone's post) I did not realize that ETN would decompose that quickly! Wow, a 12.6% loss of product after only a WEEK! Are you sure it wasn't AP? :D

I seriously doubt that my yellow goop was detonable, but I didn't try. I did try to burn it with a propane torch...it just got runny and smoked some.

HeX - I don't remember what ratios were used...but it was the same batch of ETN that was used for the detonator on P. 14 of this thread.

[thelasttrueone]

I am quite sure! I was shocked myself. My room did have a pleasant NO2 smell the whole week though so I expected it. I decided to weigh it when i saw that the actual volume had decreased enough to be visible. No doubt a good amount of what I have now is normal erythritol.

[Deceitful_Frank]

By this do you mean improvised Detcord, or some kind of plastique? I am unfamiliar with this 'Self amalgamating tape' material. Maybe some media could help, or just a detailed explaination. Is 'Self amalgamating tape' the stuff in the following link?

http://www.tapes-direct.co.uk/index.php?main_page=product_info&products_id=939

Just curious...

Yes, sorry if I sounded a little vague. Improvised detonation cord, IMO the best thing that you can do with your ETN.

Yes, that's the stuff. Its basically PIB tape with a small quantity of solvents within the rubber. When its stretched it has a slightly tacky feel. You know its the right stuff if it comes with a plastic layer that you need to peel away and discard.

The great thing about this tape is that when you wrap your ETN, stretching it as you go, it constricts the core and compresses it to great density and the layers of tape fuse into themselves and produce an effectively seamless and water proof layer over the explosive core.

With care you can get 10g/m or ETN into detonation cord just 6mm in diameter and that's with two layers of tape! Its very flexible, tough, obscenely powerful and has been tested to initiate another length of cord bound to it with a 30mm overlap. Just make sure you hit in really hard though. No pissy one gram TATP caps here. I would go for a good gram of pressed ETN to be sure and avoid any chance of disappointment.

[Cobalt.45]

Its basically PIB tape with a small quantity of solvents within the rubber. When its stretched it has a slightly tacky feel. You know its the right stuff if it comes with a plastic layer that you need to peel away and discard.There's a brand of tape called "Magic Wrap" in the US that is a poly-butyl rubber compound that performes as you've described. It's used to form a weather-proof seal when splicing electrical connections, etc.

I don't know if the "compound" portion of it has polyisobutylene or not. It's 1" wide and has a textured white plastic protective film on one side- that's what reminded me of it.

It came from Home Depot in the electrical/wiring dept. where the tie wraps and heat shrink tubing is found. IIRC it costs ~ $5/roll.

[Deceitful_Frank]

There's a brand of tape called "Magic Wrap" in the US that is a poly-butyl rubber compound that performes as you've described. It's used to form a weather-proof seal when splicing electrical connections, etc.

I don't know if the "compound" portion of it has polyisobutylene or not. It's 1" wide and has a textured white plastic protective film on one side- that's what reminded me of it.

It came from Home Depot in the electrical/wiring dept. where the tie wraps and heat shrink tubing is found. IIRC it costs ~ $5/roll.

Hmmm... that could well be it but at just $5 per roll it seems a little cheap to be the real deal to me. Unless home depot is some kinda discount lo-cost store? I don't know.

Either way the key features of the shit you need are elasticity, tackiness and the need for that peel away backing. If you can get your hands directly on it, cut off a couple inches, remove plastic and stretch and wrap around summit.... say a pen or whatever.

If after after a few hours you are having trouble peeling it back off 'cos its all fused together then thats the right stuff. Key words on the packaging are "self amalgamating PIB"

[-=HeX=-]

:) If this months experiments go well, we wont need TATP anymore because we will have Lead Azide to make really good compound caps. Could you try to get media of your 'Detcord', because I find the stuff fascinating.

The decomp of non recrystallized ETN is phenomenally rapid. I never recrystallized my very first batch, and it was gone in 2 weeks. I now always crash it out with water, filter, add to bicarb soln, filter, dissolve in acetone with bicarb in it, crash into distilled water, wash in distilled water, filter, dry. The purification process is lenghty but I only want pure produst to ensure duplicatibility of tests and performance, and for storage.

[Deceitful_Frank]

I posted a link in the "making your own detcord" thread, page 3. I am clean out of ETN now, well save for just over a gram and need to make a new batch. I could use what I have and make a short length to test its cutting ability against sheet metal but all I have to hand is a stolen Aluminium sigh of 3mm thickness, not sure this would be suitable. Either way, What d you guys think of setting off <2 grams of ETN indoors? Maybe in a cubic foot sized container wrapped in blankets... all placed in a larger container wrapped in a duvet, Think it would be load/destructive enough to arouse suspicion next door through a brick wall?

You could probably omit the bicarb if you are gonna recrystalize straight away. I have found that a lot of time is spent waiting for the foam to subside and ETN wasted in the ensuing mess. 30 grams ETN is little enough to end up with recrystalized and dried from 20 grams of erythritol!

A couple washings with water and pressing dry between newspaper should leave you with a touch dry and pretty neutral material ready for that hot methanol and ice water crash. What do you think or am I just being lazy?

[-=HeX=-]

You could probably omit the bicarb if you are gonna recrystalize straight away. I have found that a lot of time is spent waiting for the foam to subside and ETN wasted in the ensuing mess. 30 grams ETN is little enough to end up with recrystalized and dried from 20 grams of erythritol!

A couple washings with water and pressing dry between newspaper should leave you with a touch dry and pretty neutral material ready for that hot methanol and ice water crash. What do you think or am I just being lazy?

Nah, you arent being lazy, its what works for you. Me, personally these days I am a 'Chemical Purity whore' which means LOADS of washing, recrystallization, testing a sample from each batch, purifying the precursors until I am satisfied with them.

My H2SO4 is 95%, and pink, but boiling in a pyrex jug for 10 minutes and an activated charcoal filter removes most of the pink stuff, and my Ammonium nitrate is recrystallized from fertilizer twice, washed with MeOH, and stored in a airtight plastic box with a tub of MgSO4 to help dehydrate the ammonium nitrate. The erythritol is 99% pure right from the bag anyway (ebay) so I am happy with that also.

I personally strive toward the most chemically pure product I can physically obtain in every synthises, but that is simply how I like to do it. THe acetone is cheap and easy to get, as is the distilled water and bicarb so I just go that bit farther, because I really do NOT want ANY acid in my detonators, for fear of the lead azide I like to use reacting with them to form the unstable HN3. However having no sodium azide at the moment, and having found a *gasp* OTC source of LEAD AZIDE (yet to be tested for viability however, but the initial test was positive) I also dont want it reacting with the TATP or HMTD I am yet again stuck with.

I also dont want any residual acid in my product in case it reacts with the NG and NC I use to 'plasticize' it for 'heavy' work. I am looking into the PIB tape however and may try the 'detcord' soon enough, that being if the school work or social life doesnt interfere, removing valuable lab time.

[Cobalt.45]

...after after a few hours you are having trouble peeling it back off 'cos its all fused together then thats the right stuff. Key words on the packaging are "self amalgamating PIB"
The orig. packaging is gone so don't know how it reads. Otherwise it performs as you've stated- becomes completely fused together.

Price now could very well be different- I bought mine prob. >10 years ago as best I recollect. Salient point is that they have it, AFAIK.

Similar material is used in the roofing industry. Comes in various thicknesses and width/lengths.

And there is an OTC source of liquid SBR that is suitable, as well. It's >98% pure.

[Positron]

Hi All,

A high-quality Exploding Bridge-Wire (EBW) detonator is in development, utilizing ETN as the active material. The Bridge-Wire element will be exploded using an excess of electrical charge (100uF @ 1kV, Bridge-Wire diameter < 0.003") to guarantee enough current, and current rise-time (di/dt) to fully initiate the "initial pressing" of ETN within the detonator.

The design of the detonator is based off of the great information from risi-usa.com:

http://www.risi-usa.com/0products/8td/page03.html

From the same link:

"The first increment, or the increment next to the bridgewire, is pressed into the header at a density of approximately 50% of crystal density."

"The second increment consists of either the same type or a different type of secondary explosive which has been pressed to approximately 90% of crystal density. This increment is called the output charge of the detonator. The first increment is called the initial pressing."

This company's initial pressings seem to always be made of PETN and the output charges made with RDX+binder (no doubt due to it's power). The actual weights of their initial pressings/final charges are as follows:

RP-1, 251mg/375mg (251 milligrams PETN/375mg RDX+binder)
RP-2, 32mg/18mg
RP-3, 16/13
RP-80, 80/123 (they say this one will initiate pressed TNT, and C-4)
RP-81, 80/450 (they say this one is the equivalent of a #8 and will make anything go high-order)

When complete, the ETN cap in development will have the initiating power of the RP-81 (really damn powerful, #8).

Based on this, what would be your recommendations for loading density within an all-ETN cap? The person working on this cap feels like explosives science is a bit like black magic, and doesn't yet fully understand the mechanisms of transitioning to full VoD.

Could it be as simple as swapping out the PETN and RDX for ETN (in say, the RP-81 detonator), whilst maintaining the same loading density and mass?

Thing is, we don't know the loading density of their cap's, but we do know that in their other texts, they stated 50% of crystal density for the initial pressing and 90% crystal density for the output charge :)

Throwing it out on the table: How about an initial pressing of 80mg ETN @ 0.8g/cm^3 up against the bridgewire, and an output charge of 450mg ETN @ 1.6g/cm^3? Mass ratios were taken from the RP-81 detonator above, but absolute loading densities were taken from general information found within this thread. It was stated somewhere here that 1.6 - 1.7g/cm^3 is about as far as you want to push ETN, above which it starts to dead-press.

OR:

Bridgewire ---> ETN @ 0.8g/cm^3 ---> ETN @ 1.6g/cm^3 ---> CAST ETN

Yes?!

[Deceitful_Frank]

Fantastic. I have been mulling over the idea of making an EBW system for a while but without access to MHN, or indeed the chemicals needed to render it stable even after recrystalization, this has very much been on the back burner for me.

Am I right in thinking that ETN will actually cook of and DDT simply from being heated or are we actually talking about a EXPLODING bridge wire arrangement here?

A while ago I took the liberty of grabbing a photo flash bargain in the form of 100 330V caps at 150uF a piece. Enough in theory to store enough energy to kill myself MANY times over. I was thinking less exploding wires and more providing a good amount of juice at 330V to fire at least a fairy light bulb with 30mg HMTD at hundreds of feet through THIN speaker wire. Obviously with a view to initiate sensitive low density ETN and then the pressed shit that really does the work.

You can see in the pic uploaded what 750mg ETN at 3500 psi (approx 1.3g/cc) can do. It was pressed in a 5/16" brass tube with 90Kg on a 1/4" dowel and fired with 250mg HMTD and a sprinkling of ETN to get it going.

You can see at the top of the pic the 3/4" aluminium channel has been penetrated by fragments of brass and buckled at a distance of 4cm from the cap. Although on a tiny scale I consider this to be the most brisant explosion I have yet initiated. I have built a small pressing jig and would feel comfortable with putting 100Kg+ on a 1/4" dowel (with ear defenders of course!) though I am not sure that 1.6g/cc is within the capabilities of the home experimenter, 1.4-1.5 maybe.

To be able to do away with primaries would be fantastic and a blasting cap that's literally safe enough for children to play with... I think I'd pour my H2O2 down the sink!

IMHO, forget the cast ETN. It ain't that dence, 1.4g/cc, probably susceptable to LVD with a large critical diameter and heating ETN to >60C for no real good reason can't be great.

Bridgewire ---> 200mg ETN @ 1g/cm^3 (hand pressed) ---> 600mg ETN @ 1.5g/cm^3 (5000psi?)

[Cobalt.45]

Thing is, we don't know the loading density of their cap's, but we do know that in their other texts, they stated 50% of crystal density for the initial pressing and 90% crystal density for the output charge :)
Fig. 5 (left), shows the initial PETN load (next to the bridgewire) to be 1.0g/cc, the "output pellet" is pressed to 1.65g/cc (RDX or PETN).

[Positron]

Cobalt.45 - An important piece of the puzzle. Thanks.

Am I right in thinking that ETN will actually cook off and DDT simply from being heated or are we actually talking about a EXPLODING bridge wire arrangement here?


With a rate-of-rise of current in the 1kA/uS range and the exceedingly small diameter of the bridge-wire element, we should be would be well within initiation-via-shockwave territory.

The equipment and know-how to accurately measure and characterize the bridge-wire explosion event has been acquired :)

A while ago I took the liberty of grabbing a photo flash bargain in the form of 100 330V caps at 150uF a piece. Enough in theory to store enough energy to kill myself MANY times over.

I'm not sure that photo-flash capacitors are going to work for this :( . Hopefully they will, but I think they have too much internal inductance and resistance. These "parasitics" have the effect of limiting the maximum current rise-time. If the rise-time isn't fast enough, the bridge-wire element may just "deflagrate" or "burn explosively" without the intense shock-wave that is needed for full initiation of the initial pellet of ETN.

You can see in the pic uploaded what 750mg ETN at 3500 psi (approx 1.3g/cc) can do. It was pressed in a 5/16" brass tube with 90Kg on a 1/4" dowel and fired with 250mg HMTD and a sprinkling of ETN to get it going.

This will make for a great reference to use when comparing the initiating power of future EBW-ETN cap's...impressive brisance...very good.

...though I am not sure that 1.6g/cc is within the capabilities of the home experimenter, 1.4-1.5 maybe.

Yeah, 1.7 may be a bit much. I'll have to go back and look up how much pressure it takes to achieve that density...probably upwards of 10kPSI or more.

Bridgewire ---> 200mg ETN @ 1g/cm^3 (hand pressed) ---> 600mg ETN @ 1.5g/cm^3 (5000psi?)


Yeah ok! :D

[Cobalt.45]

I see that both pressings are done w/o the bridgewire being anywhere near. The output pellet is "stand alone" and can be inserted into the sleeve on assembly, as can the BW/header assembly itself. Pretty slick!:D

The header material is sited to be "plastic or a metal/ceramic combo. What do you all suppose is meant by the latter?

The material of the "sleeve" that contains the ETN initial pressing isn't specified, but I'd imagine metal tubing would be needed in order to hold up. I found no mention of reaction w/metals. Is this correct?

Is soldering the BW to the leads the plan?

[Deceitful_Frank]

Its funny, but in all my years of learning about energetic materials and blasting around I have never actually been able to find a convincing figure for for its TMD.
There seems to be infinitely more information available for PETN. Even MHN which is far less less chemically stable has still found use in commercial blasting caps, I believe that until recently erythritol has remained prohibitively expensive with the need to extract it from a certain variety of seaweed.

I've seen figures like 1.6, 1.7, 1.59 for ETN and 1.72 and 1.604 for MHN. I am enclined to go with the 1.72 for the MHN considering that NG is well documented to have a density of 1.59g/cc with half the carbon backbone.
This for me put the TMD of ETN at <=1.65g/cc or just 93% that of PETN.

Now according to Urbanski, 703g/cm^2 or pressure will give a density in PETN of 1.638g/cc. Reaching into my ass and grabbing some more figures, lets say that 750 will give you 1.65 in PETN :D

Now here's a pretty big assumption... applying said pressure to a sample of ETN will take it to the same percentage of TMD as it would with PETN. unlikely but these compounds are from the same family and my way to recrystalize ETN gives a random selection of particle shapes hopefully not too dissimilar to those of the PETN they used.

Our target density for our ETN would be 1.538 under a pressure of 10,645 psi.

That's some 270Kg on a 1/4" close fitting dowel!

[Positron]

The output pellet is "stand alone" and can be inserted into the sleeve on assembly,

Yeah I noticed that too. Looks like they're just screwed together (when they both blow up at the same time :D) for final assembly.

The header material is sited to be "plastic or a metal/ceramic combo. What do you all suppose is meant by the latter?

If I had to guess, I'd say that they're depositing the Gold bridge-wire itself as a film onto a ceramic substrate :cool: The ceramic piece could be held in position with the housing. There are many excellent reasons that I can think of for doing this (Ultra-low reactivity of ceramic and Gold, pressure-focusing effect of the substrate when the explosion occurs, great mechanical and electrical termination due to larger copper traces being deposited on same piece of substrate so big lead wires can be soldered directly on, etc!!)

The material of the "sleeve" that contains the PETN initial pressing isn't specified, but I'd imagine metal tubing would be needed in order to hold up. I found no mention of reaction w/metals. Is this correct?

They appear to be extremely high quality. I didn't see any mention of shelf-life, but I imagine it's excellent.

Is soldering the BW to the leads the plan?

The best I've come up with is to scribe the surface of a copper-clad circuit board (tiny piece of ckt. board from ANYTHING) with a razor to make a small insulated gap. The bridge-wire can be laid across this gap and soldered to the copper on both sides. This leaves two really great termination "lands" (copper pads) for the bigger lead-wires to be soldered onto...which makes for easy soldering, and great strain-relief of the fragile bridge-wire element.

If you're good, you can solder the tiny BW straight across the ends of heavier lead wires. Gotta be careful though, the lead wire will push and pull on the fragile BW (See orange wires in p. 14 of this thread).

EDIT - Added the following: Deceitful_Frank:

Our target density for our ETN would be 1.538 under a pressure of 10,645 psi. That's some 270Kg on a 1/4" close fitting dowel!


OWW. Maybe it should be cast after all.

[Deceitful_Frank]

This wouldn't be that hard to achieve, some cheap 2by2 could be used with a door-hinge to improvise a scissor type device with maybe 4 or 5:1 leverage and placed over a 3 metre high tree branch.

I am sure that with a rope and this kind of setup, most people could generate a 270Kg force using their own bodyweight.

Plus remember that there is no real need for the output charge to be any longer than 1.5 times its width. This amounts to a 450mg slug inside a 1/4" ID (5/16" OD) brass tube when pressed to 1.5g/cc. pressing such a small amount of explosive, The penalty for failure shouldn't be too severe so long as hands and eyes are out of the way and ear defenders are used.

Getting the dowel out would need a whole new setup though. Maybe a metal ring through the end of the dowel attached to a long string with the brass tube in some kind of secured clamp?

I am a great believer in striving to acheive results with as little time, effort and expense as possible and I reckon this method makes this stage of the process real simple.

Also, the addition of 5% by mass of vaseline, montan wax etc using a syringe and a cup of hot water would surely increase safety when pressing, help to achieve higher density, lubricate the ETN and help it hold its shape within the casing whilst hardly impacting on its power or sensitivity. Obviously this would just be used for the output charge with 150mg of hand-pressed pure ETN used on the top for good measure

[Cobalt.45]

Quote:
The material of the "sleeve" that contains the PETN initial pressing...So ETN wouldn't be used?, was wondering why. (It would be used, just not in the risa-usa cap, sorry for my confusing the issue)

Would the use of Ag for the BW be problematic?

[Positron]

For the bridge-wire, you could use anything that doesn't react with ETN. Personally, I'd just use small-diameter copper wire if you don't intend to store the detonator very long. If anyone's worried about ETN's reactivity with copper, then use insulated (enameled, very thin coatings) copper wire (magnet wire, motor wire, etc.). Keep the diameter less than 0.003" or so, in order to keep your capacitor size down. Less wire there means that it takes less energy to make a shock-wave out of it.

No need for Gold or Silver in homemade cap's...

[Positron]

Hi All,

First, let me post the results, as they are somewhat inconclusive. All I can say is that the remaining brass of the detonator casing was absolutely pulverized into tiny bits. The largest piece of brass that was found was less than 0.010" in any dimension. The casing was shattered into glitter that was sprayed around the inside of the hole in the ground where it was fired.

EDIT: The 0.090" thick steel plate was dented by 0.21".

...The plate was deeply gouged from flying brass, but was otherwise unharmed. A curious hole was found in it, about 0.010" in diameter, with the inside coated in brass (weird pressure jet?).

Judging by the damage to the plate, the detonator must have fallen off-center before firing.


http://www.choiceelectrophysics.com/forumfiles/EWF/steelplate.jpg

CONSTRUCTION:

DETONATOR BODY:

.30 Carbine rifle shell with primer already fired.

EXPLOSIVE USED:

ETN, created via the NH4NO3/H2SO4 method and recrystallized with hardware-store denatured alcohol. No effort was made to stabilize the ETN, other than several washes with a weak baking soda solution.

EXPLOSIVE TRAIN:

EBW ---> 180mg @ 0.75cm^3 ---> 180mg @ 1.125g/cm^3 ---> 180mg @ 1.5g/cm^3 ---> 1.0g @ 1.75g/cm^3. It is realized that this may have been "pointless" but it was hard to get a feel for how much pressure to press with! Measurements were taken after each pressing to find out where to "land" at 0.75g/cm^3 for the initial pressing (high-density was extremely easy to achieve!).

TOTAL MASS OF EXPLOSIVE:

1.54g ETN.

EXPLODING BRIDGE-WIRE CONSTRUCTION:

0.003" diameter copper wire, 0.05" in length, soldered between the copper pads of a 1/4" square piece of copper-clad circuit board. A dremel tool was used to make a small "slice" in the middle of the 1/4" land of copper. The tiny wire was then carefully soldered across this gap, making sure to not thicken the bridge-wire with solder. 20 gauge lead wires were then soldered to the copper lands for connection to the outside World.

ASSEMBLY DETAILS:

The 1/4" piece of circuit board, with the tiny bridge-wire on the surface, was hand-pressed onto loose powdered ETN to "cake" the ETN onto and around the bridge-wire. This was then hand-pressed onto the surface of the initial 180mg pressing of ETN, and epoxied into place using "J.B. Qwik" (great stuff!). An endcap was also J.B. Qwik'ed on to seal the device.

CAPACITOR CHARGING CIRCUIT:

A 6kV neon sign transformer was plugged into a variac (variable transformer) to provide 0 - 6kVAC of output voltage. This was then rectified and filtered to produce 0 - 8.5kVDC. The filter capacitor was also used as the main energy discharge capacitor.

Capacitance: 2uF. Firing voltage: 4kVDC. Input energy: 16 Joules.

TRANSMISSION LINE:

30 feet of RG-8 (50 ohm) coaxial cable to minimize inductance and maximize current rise-time.

SWITCHING CIRCUIT:

Simple bridging of two wires with a screwdriver. This is, in effect, the same thing as the "over-voltage" of or "self-firing" of a spark gap.

RESULTS:

A 0.21" dent in 0.090" mild steel. And a hell of a bang, and tiny brass particles. The 1/8" thick steel plate that the detonator was sitting directly on was NOT heavily dented. It WAS heavily "gouged" by flying brass.

Significant energy remained in the capacitor after firing, as evidenced by a goodly-sized spark when shorted. Remaining voltage wasn't measured, but was probably more than a kV.

Bridge-Wire Element Before Soldering:
http://www.choiceelectrophysics.com/forumfiles/EWF/EBW.jpg

Detonator and Coax Cable:
http://www.choiceelectrophysics.com/forumfiles/EWF/coax.jpg

Fire in the Hole:
http://www.choiceelectrophysics.com/forumfiles/EWF/downhole.jpg

-----------

My interpretation of the results:

1). A better witness plate is needed (thin aluminum) and 2). The result of that needs to be referenced to a similar load of ETN initiated via HMTD.

Otherwise, I think it pretty much worked, with most if not all of the ETN going high-order.

Sound reasonable? Thanks.

[NameWithheld]

Well... this is rather a departure from the previous conversation (sorry).. but it is rather ETN related, as well as a question related to safety, so.. here goes..

I created recently a batch of ETN, probably will be about 120g after it dries.
I chose to try a very slow recrystallization, just for kicks. I dissolved the fresh ETN in near-boiling methanol and let it cool slowly over several hours, not more than 10 degrees an hour, until it reached about -10 degrees. I brought it into light and took at a look... the crystals were freaking humongous. People have talked about crystal size before in this thread but never mentioned any specific numbers (that I saw, sorry if I missed it). There were crystals in this batch that looked to be nearly a centimeter. I'll upload pics when I get my other computer up and running again (if anyone is interested).

Is something like that safe to work with? To be honest I'm terrified of this stuff. I've got all these horrific images in my head of the stuff detonating when its dry from having crystals break while I'm working with it :eek:

I've still got it sitting in methanol at about -10 degrees... should I just reheat it and crash it into water like normal, or is it possible to work with it as it is now?

[-=HeX=-]

Jesus man, I would dissolve in methanol immediately and crash it out. You, my friend, are inexpendable. We need people like you who have the balls for large blasts to keep us sane. Large crystals are dangerous, last year a big TATP crystal fell, shattered, and detonated. It was fucking scary. Take caution man. Btw, can we see some pics of the crystals? They sound fascinating.

[Deceitful_Frank]

Jesus man, I would dissolve in methanol immediately and crash it out. You, my friend, are inexpendable. We need people like you who have the balls for large blasts to keep us sane. Large crystals are dangerous, last year a big TATP crystal fell, shattered, and detonated. It was fucking scary. Take caution man. Btw, can we see some pics of the crystals? They sound fascinating.

I agree.

ETN is no primary but as secondaries go it is quite sensitive and the penalty for failure if one of those crystals did detonate in a 120 gram batch is death. Plain and simple.

Why do you want large crystals of ETN?

If you wanted one purely for shits and giggle then you could separate a couple and try growing them in a saturated solution in MeOH. If thats your thing then great but I'd advise you to get your shit back in to hot saturated solution and pour it in to three times the volume of iced water.

Safe, fine pure crystals of ETN that pack better for a stronger blast :)

[Hinckleyforpresident]

@NameWithheld

I would get those crystals dissolved in MeOH as quickly as possible...

Methanol should be added to the crystal cake, with very gentle stirring and heat. Over the course of 2-3 hours, bring it to a boil and speed up the stirring. No matter what - you DO NOT want to snap those crystals apart. Just let them slowly go back into solution.

[Cobalt.45]

It may be an overstatement to say you stared death in the face, but not by much.

The scary thing is, is just how "un-scary" those crystals look.

120g is too large of a batch in the first place, IMO. There's a lot to recommend making what you need, when you need it rather than storing it, even though storage is less a problem than with some HE's.

Here's what wiki has to say on recrystallization of ETN, and why wiki should always be doubted unless verified:

"ETN dissolves readily in acetone and other ketone solvents though for the purpose of recrystallization, slow cooling of a saturated solution in ethanol from 55 °C gives much better results with purer and better formed crystals."

Purer and better formed, possibly. But this would also yield large crystals.

[Hinckleyforpresident]

@Cobalt

Acetone doesn't produce very clean crystals of ETN... The other junk is just too soluble in it too. Also, rapid cooling = small crystals, slow cooling = large crystals. The larger the crystals, usually the more pure the product. Methanol is certainly the ideal solvent for ETN recrystallizations.

[Cobalt.45]

Also, rapid cooling = small crystals, slow cooling = large crystals.Thus, "Purer and better formed, possibly. But this would also yield large crystals."

If one were to take wiki literally, one might be led to believe that slowly cooled (read- large) crystals were preferred over rapidly cooled (small) crystals.

This might be true if one were propagating crystals for crystal's sake, but would not be the preferred method or crystal form for use as a secondary HE.

I would rather have small "acetone" crystals with whatever small amount of contaminants that they might contain, rather than large, pure "methanol" crystals, though no one is disputing methanol as the preferred solvent. If the amount of impurities are so excessive that using acetone poses a risk, the procedure/precursors should be brought into question, IMHO.

[fluoroantimonic]

Well if you haven't already redissolved them, you could carefully pull out one or two for testing (obviously if it looks dangerous don't do it), I think it would be interesting to see just how sensitive they are using a drop test. Then again you might want to grow a smaller batch of crystals for testing to be safer... I can't wait to see some pictures.

[Hinckleyforpresident]

I would rather have small "acetone" crystals with whatever small amount of contaminants that they might contain, rather than large, pure "methanol" crystals, though no one is disputing methanol as the preferred solvent. If the amount of impurities are so excessive that using acetone poses a risk, the procedure/precursors should be brought into question, IMHO.

Perhaps I'm misunderstanding you here... But crystal size doesn't really have to do with the solvent. So, one could crash a solution of ETN in MeOH or acetone into water and yield the same sized crystals. However, the acetone crystals would contain more junk just because acetone is a less selective solvent.

[Cobalt.45]

Perhaps I'm misunderstanding you here... Perhaps.

Let me repeat, this time I will highlight the salient points-

"Here's what wiki has to say on recrystallization of ETN, and why wiki should always be doubted unless verified:

"ETN dissolves readily in acetone and other ketone solvents though for the purpose of recrystallization, slow cooling of a saturated solution in ethanol from 55 °C gives much better results with purer and better formed crystals."

My earlier observation in re the above:

"Purer and better formed, possibly. But this would also yield large crystals."

That's it!:)

[-=HeX=-]

Hmmm the forum was down for a while there... Anyway, Cobalt.45, 120 grams is an acceptable batch size for a secondary, and I am trying to design a nitrator for 1 pound amounts :Eek: because some people here like to think big. For me its all for some tests I will be conducting, requiring a whopping 650 grams of ETN alone, about 500 grams PETN and 250 grams RDX. Details will come soon.

Anyways, for Recrystalizations, do two of them. First a slow meth one to get pure crystals, then a quick acetone one to lower their sizes. Its actually that simple.

[Cobalt.45]

If using methanol, the contaminants that don't dissolve wouldn't be in solution in the first place.

If there needs to be multiple crystallization's because of so much contamination, the method/precursors need to be questioned, IMO.

[tijo77]

What about casting into sticks ? :eek:

I am not new to ETN but I'm asking myself if what I always do could be dangerous... (etn temp. of fusion is 61 Celsius degrees).

I make my etn with 70% Nitric / 95% sulphuric acid and dump the resulting white creamy mixture into cold water. There is after a neutralisation process and, the very wet powder (I don't press it in the filters to avoid waste of time) is (more like a cream mixture) warmed to about 80 Celsius degrees in a water bath (to avoid over-warming) so the ETN (now liquid) separates and falls to the bottom. This is allowed to cool down. The water is thrown away and the solid cake of ETN is dried with towel. The cake is melted again and cast into tubes. I put a spacer in the middle to leave a space for a detonator (like real dynamites).

see my long post here on page 13, 5 posts before the end of the page (http://www.roguesci.org/theforum/showthread.php?t=2712&page=13)

I would really appreciate feedback because I love my hands and I would like to know if I could potentially lose them .:rolleyes:.

[fluoroantimonic]

Hmm... It's hard to say exactly how dangerous that is. I have heard rumors that cast ETN can be quite sensetive, but I've never seen any actual tests done. I would definately recommend doing some testing on those cast sticks before you handle them much. Maybe try a drop test or something similar to make sure they won't go off if dropped. And maybe try a crush test too, to see how much force they can withstand dropping onto them.

By the way, a 150g stick of ETN will do much more than remove a hand.. Like kill you. So be careful.

[tijo77]

I did not have time to make real tests but I have some interesting info from myself here : Breaking several sticks of cast ETN did not set it off. Even repeated dropping and crushing did nothing. Also poor quality TATP (probably DADP) had not been enough one day to set off a stick (the detonator was placed inside the stick as always) resulting in a loss of ETN.

From these facts cast ETN seems to be fairly safe but we need to remember here that the "1000 time" could be the bad one...

Also... that was probably stupid, but I always broke my solid dried cakes of ETN into smaller parts before re-melting them without accident.

I am actually reading each page of this subject, but what you guys know more about ETN sensitivity and also when it is in powder/crystals form ? I saw here some members claiming that there is some danger with crystals of ETN.
And why don't you all cast your ETN if crystalline ETN is dangerous and also weaker (as it has not its full density)?

I don't care what language you normally speak. If I can't understand you, I will ban you. If I can, then it is all good. Buy an English/French dictionary if you are worried about it. Also it isn't "casted" it is cast.

[-=HeX=-]

Well, in my experience with cast ETN the cast ETN is fairly insensitive to abuse. Also I remember Thelasttrueone had a failure to detonate with cast ETN, the TATP detonator merely spread the cast ETN around without detonating it.

When I cast ETN I learnt the hard way to use a booster of about 10 grams powdered ETN which was overkill but hey, I did not want a failure to initiate. This summer I am planning to do many tests with ETN regarding its power in various mixtures and densities. Anybody want anything tested with videos?

[thelasttrueone]

Yes indeed, the 5g TCAP cap just scattered and split the cast ETN. I later took the cracked apart pieces and recrystallized them for re use. What a let down that was, I'm sure it would have set it off if it had been set inside the ETN as opposed to being taped on top of it.

[totenkov]

You will need absolute direct contact between secondary and cap. When casting ETN, pour it into a tube or your preferred shape, and then stick in a 1/2" roll of paper as it hardens, the cap should sit in this space when you are going to do a det. Also, I have used cast ETN on several occasions, and I was never able to initiate it with AP. 1.5g of HMTD or 2g of silver acetylide both were able to initiate with relative ease.

When you are making your caps, I would advise packing a 1/4 of the cap full of DRY ETN in crystal form and then packing in the primary. This makes a much more professional cap and will increase you chances of a successful detonation. After looking at the blasters training manual (not written by the Al-Qaeda :p) I started making caps like the solid pack electrical cap, which is by far the most effective, especially for more hard, compact secondaries like cast ETN.


http://i215.photobucket.com/albums/cc6/totenkov/400px-BlastingCapsAndDetonators.png

[iHME]

But wouldn't you have to coat the bridge wire with something to prevent the HMTD from "eating" it away? At least in the the solid pack electrical cap style.

[totenkov]

How long were you planning on keeping your caps? Weeks or years? HMTD is not nearly that bad. There seems to be this rumor that HMTD will dissolve and eat away any metal in its way, that's just not the case. I've had caps fire after 8 months of being stored in a drawer.

[-=HeX=-]

Well, if you as so anxious about the HMTD reacting with the copper, coat the copper strand with pyrogen or another prime like bound black powder. This not only helps reduce the oxidation of the wire but it also makes the cap more reliable.

Also, I think ETN will go off from just a hot wire by deflagrating to detonating transition. So maybe primary is not needed. I will test that in the summer.

[tijo77]

I always detonated ETN electrically with TATP and a timer. It worked every time except once. The detonators were always placed inside the stick. I never had accidents with AP but after well thinking I feel it is too sensitive and dangerous so I plan to use Mannitol hexanitrate. Should be the same with HMTD, no ? What do you think about MHN + ETN ? More stable, less sensitive and not becoming ultra sensitive with age ?

I used to make small bags of AP+2 or 3 small rocks (or cents) with saran wrap that I throwed where I wanted (away from people) making sometimes holes on no more used no parking sings:D.
I don't do it anymore as manipulating AP could make your hands fingerless or at least remove your skin (happened to someone I know). Am I the only one here to be suddenly afraid of TATP and HMTD ?

[Hinckleyforpresident]

Also, I think ETN will go off from just a hot wire by deflagrating to detonating transition. So maybe primary is not needed. I will test that in the summer.

ETN DDTs from heat pretty well so long as it is contained. This property can be demonstrated by taking a very small amount of ETN (<.05g) and making a little ball out of it with Al foil. When flame is applied it will sit for a moment, and then suddenly detonate in a cloud of foil dust.

I've seen examples of primary-less ETN charges (~10g) being initiated by simple cannon fuse. Once again, containment is very important when attempting to make a substance reach DDT.

[-=HeX=-]

Tijo77: mannitol hexanitrate is not a primary explosive. It is a sensitive secondary. Its about as sensitive as nitroglycerin, which is far less sensitive than TATP or HMTD. I too am scared of TATP and HMTD because of my TATP accident. Organic peroxides now scare the bajesus out of me.

You are french right? Then send me private message and I will give you a source of sodium azide for all europe. Lead azide is a good primary.

As for ETN, I may be comparing it to PETN and RDX and their plastiques, aluminized mixtures, plastiques with nitroglycerin and any other mixes I can make. Those tests will be this summer.

Also, iHME, the azide source is indeed the one I told you about.

[tijo77]

HeX : I speak french but I am from Montreal, Canada. If you have found also a source for Canada, let me know.

Even if MHN is a secondary, would it not be good for detonating ETN as it has just a perfect sensitivity ? (edit: I read somewhere(think it's powerlabs) that MHN is used in commercial detonators / Here microtek says he makes caps (http://www.roguesci.org/theforum/showthread.php?t=2100)) Do you think MHN would not fully detonate from bridge wire detonator ? AP detonates instantly with heat coming from a light bulb filament. I think that if ETN could detonate that way, MHN could even more.

I have access to many chemicals here in montreal from a chemical supplier. They never ask any questions, but I ordered one day 5 liters of sulfuric acid, 25 kilos of KNO3 and 500g of potassium permanganate (I felt like they really don't care what they are selling) and they canceled my order because they got suspicious. So, at least that you do not buy too much (less than 13 000 Kg !) and too many different chemicals (mostly oxidizers which they told me are controled by gov.) at a time you'll be ok. I bought 20L of H2SO4 for about 100$ CA. I know they sell in the U.S. also. Send me a PM if you are interested. They also have an online catalog.

Edit: They sell 500g Sodium Azide for about 150$

[-=HeX=-]

Still on the lookout for an international source... It will be a while though. However microtek uses silver acetylide to initiate the mannitol hexanitrate in his blasting caps. And the powerlabs site is wrong, its PETN and lead azide that is used in commercial blasting caps.

The ETN 'Cooks off' from a hot wire which then causes a low order detonation akin to nitroglycerin which is set off with Blackpowder. The fact that all three, nitroglycerin, mannitol hexanitrate and ETN, are all extremely similar leads me to believe that the mannitol hexanitrate will detonate with more of a fizz than a bang.

[fluoroantimonic]

The ETN 'Cooks off' from a hot wire which then causes a low order detonation akin to nitroglycerin which is set off with Blackpowder.

Well maybe uncontained. But I know for a fact that under 1g amounts of PETN have been high order detonated with the right containment and EBW. And if PETN can do it, it should be even easier with ETN or MHN. I like this idea, both for safety and simplicity.

[-=HeX=-]

Hinkley: could you outline the method used to set off ETN using fuse? If its the thermite one then explain in detail because I never had any luck with it. I would like to try it out sometime.

Flouroantimonic: I did not mean exploding bridge wire, I meant hot bridgewire heating ETN to cook off where it normally melts then goes off. At least that is what I was meaning however exploding bridgewires are just another level of cool and sophisticated entirely.

[Hinckleyforpresident]

Keep in mind, this is an experiment preformed over a year ago, so I'm a bit fuzzy on the details.

10g of recrystallized ETN was pressed into a tube with a long length of cannon fuse running down the inside of the charge. Upon ignition is sputtered for a second, followed by a few small popping, followed by detonation.

Charges like that don't work all of the time, and when they do it takes it a few seconds to reach DDT. These are certainly not as powerful as a cap initiated charge, but they can be used to demonstrate how readily ETN can reach DDT.

[-=HeX=-]

Ah so the ETN I ignited by continued heating rather than by the spit of the fuse. That makes sense to me. Now using a thermolite fuse would make it more reliable in my opinion... But it would still only be low order detonation... Maybe it can be sped up to a high order detonation using mannitol hexanitrate coprecipitated with the ETN or something. I will think more on this.

[Setharier]

In about every scene and accident on earth, the cause is people, not an malfunction in system. But, mistakes do occur and luckily nothing wasn't actually happened.

To the topic. There was an ETN preparation in process, but for a long time there was still chunks of erythritol in the sulfuric acid. Could that be cause of too small amount of H2SO4, too cold nor hot(carbonisation non?) or too little stirring?

http://img201.imageshack.us/img201/2546/76729134fw3.jpg
http://img98.imageshack.us/img98/8920/79013678zv0.jpg

That solution is only ET&H2SO4, waiting for nitration. That chunk is about an 1½ inch long.

[Setharier]

The attempted make of ETN was really an attempt there. The ET&H2SO4-mixture was poured slowly into the HNO3 solution(65%) taken out from freezer and placed into glycol bath, being very cold during addition. The solution was left to sit for nearly two hours in the bath, of course slowly warming and then poured into cold water, but no-thing crystallized. The water was checked five hours later and it was clear as pure water can be.

What went wrong? The preparation of that solution is based on this guide:

http://img505.imageshack.us/img505/8489/88274312yt3.png

Used substances:

ET 20g
H2SO4 98% 110g
HNO3 65% 220g

Possibly too cold? During addition all the material was at least under 0C, probably much lesser due to that they were kept in the freeze for hours before use. H2SO4 was left to warm up to room temperature for at least 6 hours after all the ET was added and after that it was placed into the freeze for about 12 hours.

Am I the only one who is capable of ruining a process so simple as ETN synthesis even there are pure and reagent grade materials in use? :(

[tranquillity]

Whenever making ETN I always mixed the H2SO4 and HNO3 first. This mixture warmed quite a bit and gives off white fumes so I put it, covered, in an ice bath and allowed it to cool to about 5C. I then make slow additions of erythritol to this mixture making sure the temperature does not exceed 30C. I stir the mixture to break up the quickly precipitating ETN and allow it to react for about 30 minutes. It is then crashed, filtered, neutralised and recrystallised. This process has always worked for me.

Note: Because you are using 65% HNO3 instead of 90% suggested in the other synth you need more H2SO4 to absorb the excess water. Ill let you do the stoichiometry. Also, you need to crash and neutralise your product as fast as possible as ETN will slowly hydrolyse in dilute acid. Leaving for 5 hours would probably have destroyed all the ETN if there was any to begin with.

[fluoroantimonic]

By using 65% nitric you greatly increased the amount of water in the system. That is point of using sulfuric acid after all, to dehydrate the system, and without adding a bunch of extra sulfuric, I doubt you'd ever get any ETN. Some nitrations seem to quite sensitive to water, and ETN is not the most chemically stable thing around.

I agree with tranquillity, mix the acids first and then slowly mix in small amounts of erythritol.

[Rbick]

Being a very powerful dehydrating agent, Sulfuric acid will not only remove water from the reaction but, if left in contact too long with the Erythritol, will dehydrate it also. Sulfuric dehydrates organics. For example, look what happens when it comes in contact with your skin. Erythritol is organic and will decompose if left in contact for too long. This could be the source of your problem, along with using Nitric that isn't conc. enough.

I was once making some ETN and I had just finished adding the Erythritol. My buddy came over and we went to have a few drinks. A few turned into a few more and I was gone for about 4 - 5 hours. After returning, my nitrating mixture completely dissolved into a clear puddle. I was sad :( Point being is that you want to minimize the time that the product is in contact with Sulfuric but make sure you give it enough time to fully nitrate for a good yield. Its a fine balance.

Anyway, that is my guess as to the source of your problem. Good luck.

[Setharier]

The H2SO4 exposure was most probably the reason for zero yield. The solution was left there for nitration process for at least 4 hours. Immediately when the H2SO4&ET solution was poured into the HNO3, there was formed slightly yellow yield at the bottom, which dissolved into the overall mixture but laid down if left untouched for a while. I wonder could that have been some sort of ETN yield..

The procedure will be re-attempted with using AN&H2SO4 mixture. I found ratio 20g ET, 60g AN and 100ml H2SO4, is this in ratio and feasible?

[Lewis]

My guess would have been that the temperature was too low. Do get a thermometer if you don't already have one.

I've always got good results with temps between 10ºC and 20ºC.

[katey]

Hi guys, firstly let me start by saying that ETN is quite an explosive! I've seen the videos of it on youtube! So I thought I'd give it a go.

I've read this whole thread and I apologise in advance if I ask a question which has already been answered.

Firstly, I got some battery acid and boiled it to get conc H2SO4. I then put it in a freezer to reduce the temperature.

After that I followed Axt's method, by adding 60g of KNO3 to 100ml of acid. The problem is that my solution was no where near as thick as some people on this thread have described it to be! (mine was about as thick as mushroom soup) Furthermore it turned a pink/purplish colour! Is this normal? Or could it be that my acid is not conc enough (I got 38% battery acid, and boiled 500ml till there was about 175 ml left) or could it be that my KNO3 has impurities?

After 'nitrating' the erythritol for 35 minutes , i crashed it as per the instructions and filtered it, after that i washed it in a soda bicarbonate solution. I then thought wow, here we go, so i went out and tested it. Nothing. The only thing I got was a small poof. thats it!

What do you think I could have done wrong? I followed the instructions to the letter! Furthermore, do you think it would be a good idea to add some soda bicarbonate to the precipated ETN in order to neutralise the acid? So that I can skip the step of filtering and then neutralising.

****************************

You must fix your spelling and i/I in the future.

-Hinckleyforpresident

[totenkov]

I don't think you did anything wrong. Contams in your chems is the most logical reason for this:

Furthermore it turned a pink/purplish colour! Is this normal?

Depending on the source of your acid (drain cleaner, batteries) you may encounter other factors that could change the consistency of your nitration solution. I am not sure if a purity of the acid will have effect on the viscosity, anyone? I have only synthesized ETN myself a few times, all with analytical re-agents.

After 'nitrating' the Erythritol for 35 minutes , I crashed it as per the instructions and filtered it, after that i washed it in a soda bicarbonate solution. I then thought wow, here we go, so i went out and tested it. Nothing. The only thing I got was a small poof. that's it!


Well, what exactly where you expecting? An understanding of the universe? :rolleyes:

It's an explosive, it job is to go bang. Be more specific, so we can furthur analyze any problems that you encountered.

[Alexires]

Katey - Did you boil the H2SO4 till white fumes appeared? It may be that you didn't have 35% acid to begin with, and hence you have don't have very concentrated acid now.

Pink/purple almost sounds like the colour of potassium as it is.... Perhaps you had some PbSO4 which formed a complex or reacted in some way to fuck up your reaction.

totenkov - You don't see an understanding of the universe when you set things off? Perhaps they need to be a little bigger so you can fully appreciate the power of the dark side.... :p

[katey]

Katey - Did you boil the H2SO4 till white fumes appeared? It may be that you didn't have 35% acid to begin with, and hence you have don't have very concentrated acid now.

Yes of course I boiled it till white fumes appeared. Took about 2 to 2.5 hours. It says on the bottle that its 38% so when 500ml is boiled and theres only 175ml left, I'm pretty sure that the H2SO4 is conc enough!


Pink/purple almost sounds like the colour of potassium as it is.... Perhaps you had some PbSO4 which formed a complex or reacted in some way to fuck up your reaction.


Well I bought my KNO3 from a garden store, so I think it has impurities in it. I'm waiting for my reagent grade KNO3 so that I can try it out again.

Also, I was on ebay earlier, and I saw this guy selling a Nitric acid KIT. Yes KIT. Apparently with one kit you can make 70% HNO3, has anyone heard about this kind of thing? As I think it would make my ETN synthesis very much easier if I had 70% HNO3!

*********************************

Use proper quotes

-Hinckleyforpresident

[Hinckleyforpresident]

@katey

I would imagine that 70% is satisfactory for a reaction like ETN, however, it will not yield as highly as 100% HNO3 or 98% H2SO4 + nitrate salt. Water anywhere in the reaction will substantially drop yields, even if you add H2SO4 to your 70% nitric.

I would imagine the kits comprise of a nitrate salt, sulfuric acid, and some simple method of distilling it to red fuming. I never purchased one, so I can't be sure. Also, remember that all ebay sales are public.

[Alexires]

Yes of course I boiled it till white fumes appeared. Took about 2 to 2.5 hours. It says on the bottle that its 38% so when 500ml is boiled and theres only 175ml left, I'm pretty sure that the H2SO4 is conc enough!

Then include more information in your first post. You said you obtained battery acid and I assumed that you obtained it from a battery.

If your KNO3 is from a garden store and your acid is fairly pure, then there is no reason for your acid to go pink.

[katey]

Well, I think my H2SO4 is conc enough, from my previous posts, I think its about 95%, after boiling battery acid which is 38% (thats what it says on the bottle, and after boiling 500ml I have 174ml left) but I tried again today and I got the same pink/purplish colour! I dont know why! Thats why I am tempted to do it with 70% HNO3 from ebay( see my previous posts) Please help, and if you're in the UK pls get in touch, then maybe we can do this together!

[Cobalt.45]

Well I bought my KNO3 from a garden store, so I think it has impurities in it.As what product did you buy the KNO3?

If you mix a small amount of the KNO3 with water, do you see any color change?

[Hinckleyforpresident]

Well, I think my H2SO4 is conc enough, from my previous posts, I think its about 95%, after boiling battery acid which is 38% (thats what it says on the bottle, and after boiling 500ml I have 174ml left) but I tried again today and I got the same pink/purplish colour!

Watch the temperature. You could just be letting it get too hot and causing breakdown. NOx's are red/brown, and when in solution they could probably look pink/purple.

Please help, and if you're in the UK pls get in touch, then maybe we can do this together!

Let's get together and commit a felony! Sounds like a wonderful way to spend a weekend :rolleyes:.

[katey]

As what product did you buy the KNO3?

If you mix a small amount of the KNO3 with water, do you see any color change?

I bought the KNO3 as KNO3, it actually says KNO3 on the cover, its meant for aquarium use. I don't see any contams within it.

You think this is a problem??

*****************

Write words out, and use the proper amount of question marks.

[katey]

Watch the temperature. You could just be letting it get too hot and causing breakdown. NOx's are red/brown, and when in solution they could probably look pink/purple.

When you say watch the temperature what do you mean by that? Do you mean I shoudn't let the H2SO4 reach too high a temperature when I am boiling it? Or do you mean I shouldnt let the temp get too high when i mix KNO3 with H2SO4? When mixing KNO3 with H2SO4, I hardly let the temp go above 20*C. In fact, even if I dont do anything, the temp barely goes over 20*C.

Let's get together and commit a felony! Sounds like a wonderful way to spend a weekend :rolleyes:.

Yes it does doesnt it!! And I'm sure it would be quite an enjoyable wkend! have a good one!

[Alexires]

Do you see any problems with it? Because as far as we are concerned, you purchased a bag full of KNO3, with no contaminants, had acid with no contaminants so everything should be fine.

There must be something, or you are letting it get too hot and getting NOx fumes as Hinckley said.

It is unlikely (very) but your KNO3 could be slightly wet, causing the acid to have localised hot spots leading to NOx formation. Make sure your KNO3 is dry (oven works well at its lowest setting ~100C). Make sure your acid is cold and add it slowly.

If you still have a problem, then you must have contaminants. Then again, you are getting a yield, so I don't see the problem.

Edit: Congratulations Katey, you have irritated me enough to get HED. Try thinking for yourself next time, not double posting. Besides, you smell slightly like bacon, but stupidity smells much the same. :rolleyes:

[Jenni]

Just read through this whole post, and decided to make some of my own and try it out! I followed axt's method using H2SO4 and KNO3. Had a few problems though,

1) My KNO3 did not fully dissolve in my H2SO4. I know my H2SO4 is conc enough as I did what katey had done. i.e. boiling battery acid until I achieve the right conc. Is this supposed to happen? Or does my KNO3 have to fully dissolve in my H2SO4, and thereby left with a colorless liquid?
2) When trying to dissolve the KNO3, I could see that small lumps were being formed in the solution. The temperature was never allowed to rise above 20*C so I dont understand why these lumps would form? Also, my KNO3 is in nice powder form.
3) Does anyone have any ideas on how to detonate ETN? I wrapped a little in some aluminum foil and put it in a fire, but of course I want to know how to detonate it using a less crude method!

Also, I see that Katey and I are the only girls on this forum as far as I could tell! Go girls! LOL.

Any help would be appreciated.

[totenkov]

Hmm isn't this interesting!

Registration IP Addresses:

* Jenni 90.208.186.43 [Find Posts by User] [View Other IP Addresses for this User]
* katey 90.208.186.43 [Find Posts by User] [View Other IP Addresses for this User]

Now I am going to IP ban you so you don't come back a day later, with the same old bullshit. Did you honestly think this would slip by me?

I don't believe for a second that you are a female, and next time (though there won't be one), use your brain and search for your answers, you are hereby banished from RS for all eternity you perverted little shit.

[Alexires]

There are WOMEN on the internet??!!!

Now I KNOW you are a troll. There are no women on the internet!;)

[iHME]

There are WOMEN on the internet??!!!

Now I KNOW you are a troll. There are no women on the internet!;)

Well there is one on sciencemadness

[Cobalt.45]

I wouldn't believe it for a second, n'less you've personally gone face-to-face with her beard of god.:p

[Rbick]

AH! This thread has gone dreadfully off course due to a k3wl! No worries. I had today off and decided what the hell, I'm gonna do a lab. Since I'm running low on ETN I decided to do another batch, except using OTC products only. Normally I use reagent grade chems only due mostly to the fact that I have OCD. It was so hard not using reagent chemicals :(

The AN was fertilizer I had bought for my house plants a while back and the sulfuric acid was the "Rooto" brand drain cleaner. The erythritol was from a health food store. There are A LOT of health food stores on the west coast... The total cost of the materials used in this lab was about $2.50 USD. The full bottle of Rooto was 8 USD, the AN was 14 USD for 2.2 kg and the Erythritol was 13 USD for .7 kg. Anyway, here are my lab notes.

NOTE: Anything with a * has a foot note (except when it is used as a degree symbol, self explanatory) which can be found at the bottom of the post

Materials:
200 mL H2SO4
120g NH4NO3
30g Erythritol
500 mL Pyrex beaker
Thermometer
Ice bath
Cold water bath
Bi-carb bath
Coffee filter
Fine metal Strainer*


0925 - Began adding AN to acid.

1000 - AN addition complete. Maximum temperature reached was 38* C. Noticed unusual bubbling on surface of mixture*. Try and keep below 30*C. Placed reaction vessel in ice bath. Cooled to 12*C. Mixture became clear brown due to impurities in AN and H2SO4

1022 - Addition of erythritol started. Added about 2g per minute with a 10 minute pause after half of the erythritol was added.

1045 - Addition complete. Mixture thick with ETN crystals (pic (http://i164.photobucket.com/albums/u6/pudgedog69/beaker.jpg)). Let stand for 30 minutes.
1115 - Mixture crashed into 2L of cool filtered water and then filtered. The mass of ETN filled an entire coffee filter (pic (http://i164.photobucket.com/albums/u6/pudgedog69/strainer.jpg)). The collected crystals were washed with bi-carb solution several times by dipping the strainer in a bi-carb bath *. Water was then run through and the product was tested with pH paper. pH was 6.

1220 - ETN set out to dry (pic (http://i164.photobucket.com/albums/u6/pudgedog69/final.jpg))

I still have to recrystallize it, but I will do that later with ethanol. Final yield appears to be around 40g if not more. I'll weigh it when it is dry. Not a bad yield for using OTC only :cool:


* The metal strainer is the best thing to use for filtering. I put the coffee filter in the strainer and it creates a perfect way to filter and rinse your product. This allows the quick removal of acid so you don't loose too much product due to decomposition.

* The bubbling that I saw occurred only when the temperature got to about 35* C. I think it was due to the impurities in the AN. This caused no noticeable problems with the nitration.

* After the crystals had been filtered and were sitting in the strainer waiting to be washed with bi-carb, red NOx fumes started bubbling up through the ETN. This was an obvious sign of rapid decomposition and I quickly started running water through it. After about 10 seconds, the fumes subsided. My point is that I should have used more water while filtering. When pouring the 2L of water used to crash the nitration mix into the filter, it may help to have a separate source (faucet, hose, whatever) feeding fresh water through the strainer to prevent this.

[Setharier]

I mixed up 110g of H2SO4 and 60g of AN just simply placing the beaker into snow and pouring all the AN in. Well, it fumed a little(point of view :D) and I let it cool down at 0C. I then later attempted making ETN and placed the nitration beaker in a glycol-water bath of -20C approx. and started pouring 20g of ETN in small amounts, ~1-2g per time. I used metal rod(! it was brass-al or something like that) for stirring. I managed to get about 3/4 of the process, but then it suddenly started fuming viciously(white, no red) and I immediately, very dissappointed on the way, poured the whole shit in the coolrant water and transported the bucket under flowing cold water. I anyway managed to save and filter out about 2-3 grams of ETN.

Man I am out of chemistry equipment!

[Deceitful_Frank]

Might I suggest a 4:1 by mass mix with NG. It won't be as dry as you might imagine as some of the ETN will dissolve in the NG. You could fire this dence mix straight or with 20% flake aluminum :)

What do you have planned?

[Khan]

I managed to get about 3/4 of the process, but then it suddenly started fuming viciously(white, no red) and I immediately, very dissappointed on the way, poured the whole shit in the coolrant water and transported the bucket under flowing cold water. I anyway managed to save and filter out about 2-3 grams of ETN.

That's just nitric acid fumes, seeing them is no reason to kill the reaction. You actually might cause it to partially run away by dumping it in water prematurely. The water coming into contact with sulfuric acid can cause localized hotspots and lead to nitric decomposition.

Nitric fumes are toxic, but nowhere nearly as toxic as NOx gasses.

[Rbick]

Frank: I did in fact try that ratio with NG and ETN. The results were impressive. I didn't even use a container for the charge. I just pressed it into the size of about a quarter and placed it in a plastic bag. Adding the NG allows you to reach greater density with ease. It packed a punch and I had the video but it was erased unfortunately. I need to try adding aluminum though. No need to waste all of that excess oxygen! :)

Setharier: You don't need to dump the mixture until red fumes appear. White fumes are from the nitric acid and isn't a problem. Watch the temperature though! Keep the reaction below 20*C when adding the erythritol and you'll be fine. Follow my lab notes :p

[sbovisjb1]

Hmm isn't this interesting!

Registration IP Addresses:

* Jenni 90.208.186.43 [Find Posts by User] [View Other IP Addresses for this User]
* katey 90.208.186.43 [Find Posts by User] [View Other IP Addresses for this User]

Now I am going to IP ban you so you don't come back a day later, with the same old bullshit. Did you honestly think this would slip by me?

I don't believe for a second that you are a female, and next time (though there won't be one), use your brain and search for your answers, you are hereby banished from RS for all eternity you perverted little shit.

The poor guy/girl, he/she is from the UK http://www.infosniper.net/index.php?ip_address=90.208.186.43&map_source=1&overview_map=1&lang=1&map_type=1&zoom_level=7 From Ruislip if I am not mistaken and using the ISP Easynet. Point being considering the UK's draconian deterioration of personal freedoms, I won't be surprised if they get cut off the internet in the near future for even discussing activities such as these.

[Deceitful_Frank]

Frank: I did in fact try that ratio with NG and ETN. The results were impressive. I didn't even use a container for the charge. I just pressed it into the size of about a quarter and placed it in a plastic bag. Adding the NG allows you to reach greater density with ease. It packed a punch and I had the video but it was erased unfortunately. I need to try adding aluminum though. No need to waste all of that excess oxygen! :)
:p

Agreed... though to be fair the mix is only less than 5% oxygen positive, and that's assuming you have 100% nitration and no impurities. If I add 600 mesh German flake to this mix it isn't to correct oxygen balance for CO2 and H2O, its more about sensitizing a damp dence mix and increasing "power" without being too much at the expense of brisance.

35% will reduce all your CO2 to CO and strip that water of its oxygen atom AFTER detonation has taken place. With the extra heat liberated from the Al the extra gas volume gives maximum "power" against softer targets but shattering ability must suffer.

I have tried with 20% and I must say it was probably the most viscious detonation I have witnessed with that slightly disconcerting but rather cool effect of shrapnel striking the dusty ground in front of the shock wave! I believe that up to 5% high quality shit can actually take part in the detonation so next time I would shoot for 10% as a happy compromize against a steel target with maybe a wooden one at close proximity :)

[Lewis]

I've always aluminized my ETN as well. Since I went to all the trouble of making quality Al, I have this indescribable urge to use it whenever possible. :p

Usually about 5% is all I use. Seems to make detonation easier, too (as if ETN needs it). Will brisance really suffer if there is only enough Al to give zero oxygen balance? :confused:

[fluoroantimonic]

I think it doesn't take much Al at all (any?) to reduce the brisance at least a little. IIRC this is because the Al doesn't oxidize nearly a fast as the explosive detonates, meaning very little Al (depends of particle size etc.) will take part in the actual initial shock wave that has the shattering power.. Only once the initial pressure spike is gone and more time passes the Al oxidizes and releases tons more energy and holds the overpressure much longer.. So I would hazard a guess that in respect to the initial shock wave, an explosive with X% Al would act very similar to an explosive with X% SiO2 in it.. Correct me if I'm wrong here..

[Lewis]

That makes sense the more I think about it, Fluoro.

Although if that was the case, perhaps OB can be disregarded in this instance altogether, as finely dispersed reactive Al will always add to the total pressure/heat effect.

I suppose this is one of those things that is only practical to determine by experiment.

[Deceitful_Frank]

Put very simply, I think that if your pressed ETN or ETN/nitro mix is touching the target and it is heavy and metallic or steel then best results would be gained buy leaving out the Alu.
A few percent O2 either way makes no difference. In this instance, power and gas volume is of secondary importance to pure shattering power.

If your mix or ETN is not touching the target or the target is less dense, larger or more elastic, polymer, wood, scavenging pigeons, annoying seagulls etc :)
Go ahead and add 10-20% Alu to reduce those gasses after detonation and keep that over pressure higher for longer to better tear apart that target.

[fluoroantimonic]

scavenging pigeons, annoying seagulls etc

Hah, that would be an interesting video to see. Set a charge off near a hovering bunch of seagulls and watch the shock wave go through them and then watch them fall like confetti... A good high framerate camera would help a lot. It would be interesting to see how far away they would have to be to not get knocked from the air. Don't let the PETA see! :p

Although if that was the case, perhaps OB can be disregarded in this instance altogether, as finely dispersed reactive Al will always add to the total pressure/heat effect.

Exactly. I suspect that an explosive formulated to have a near neutral OB and then mixed with Al, not accounting for its oxygen requirements, would perform better than one formulated with a neutral OB while accounting for the Al. Probably not a big difference though.

I suppose this is one of those things that is only practical to determine by experiment.

That is by far the best! Unfortunately I get to do so little of it under my current circumstances...

[Rbick]

While we are on the subject of thermobarics, I found this video to be pretty informational. It is from the tv show "Future Weapons". While the host is kinda corny and the information is presented for the lay viewer, it still provides a good overview of the thermobaric effect and why it is used.

www.youtube.com/watch?v=Jh-I1mr2h98

[-=HeX=-]

I have found that adding MgAl to the ETN:NG mix in these ratios 75:15:10 (ETN:NG:MgAl) increases its 'blasting' power by a fair bit, but lowers the 'pitch' and 'hardness' of the shockwave. However the shockwave seems to be a bit 'longer' than normal, closer to a ETN:AN mix than pure ETN. The positive OB of both ETN and NG is utilized to a certain extent, however it certainly reduces the VoD and supposedly brisance.

For cutting and SC devices, leave out the Al/Mg/MgAl but with blasting or tree stumping leave the Al/Mg/MgAl in.

I will be dong extensive tests (also expensive!) on ETN, PETN, MHN, NG and hopefully RDX, depending on how my making of HNO3 goes. The PETN, ETN, and NG are a certain positive, MHN is almost certain and RDX is probable. I will be testing 10 gram charges of them pure, with PIB, with Al and with Ng to make a 'plastique' on concrete blocks, Al witness plates and 20mm plywood plates. It also doubles as tests on the Caseless detonator I am working on extensively. The FAE tests will come after that as the CLD and witness plate projects are my top priority.

I shall be videoing the tests, for I am getting a video camera soon, and will be making every possible measurement before and after of the material to be tested. It is going to be my 'super project' and I am already preparing for it, even though its happening in July or August.

Could someone good at chemistry please post the optimal synthises for ETN, PETN, MHN, and NG using the AN and H2SO4 method? So far my results are varying. My H2SO4 is between 92 and 98%, and will be boiled and filtered over activated charcoal, then re-boiled before use. Is there any thing else that should be done to the sulphuric to make it optimal? I may even be able to make SO3 and react that with the H2O remaining in the H2SO4 to concentrate it further if nessecarry. I am soon to order my 'huge lot' of chems from my new NaN3 source (yet to be tried, but I have corresponded extensively with them, and they WILL supply the individual. EU members PM me...)

[Rbick]

Hex:

I'm excited to see the results! Good luck on your project. For ETN synthesis with H2SO4 and AN, the ratios I have listed above seen to work extremely well. The best that I have seen anyway. As for NG and the others, I need to go dig up my lab notes. I'm in a rush as of now to go help a friend move though :(

The link I have listed above is faulty. Sorry about that, but I posted from a phone. Anyway, here is the correct one.

http://www.youtube.com/watch?v=Jh-l1mr2h98

[Deceitful_Frank]

Could someone good at chemistry please post the optimal synthises for ETN, PETN, MHN, and NG using the AN and H2SO4 method?

I must be brief.

To make NG and EGDN or indeed mixture of the two you should use the following ratios of precursers by MASS.

Polyol... 1
Ammonium nitrate... 4
H2SO4... 10 (this needs to be the good stuff, dyed shit wont work if you are nitrating liquids)

These numbers should give you at least 1.65 grams of EGDN or up to 1.82 grams of Nitro per gram of glycol or glycerin used after all neutralization and removal of unwanted water from your blasting oil. These are the best yields I have achieved using this acid/nitrate method and I challenge anyone to do better.

To make ETN you should use the following ratios of precursers by MASS.

Polyol... 1
Ammonium nitrate... 4
H2SO4... 12 (dyed shit works fine when nitrating erythritol, its MUCH cheaper and the brown colour will be gone after recrystalization.... you MUST recrystalize!)

These numbers should give you around 1.5 grams of ETN per gram of erythritol nitrated. Yields are lower as its easy to waste you product down the sink with careless filtering and recrystalization. TAKE YOUR TIME!

I am not in the business of spoon-feeding so I'llwrap this up by saying that you will find everything you need to know about making NG, EGDN and ETN in good yields by searching for my posts on here, APC and Sci-mad.

Looking forward to this one!

[-=HeX=-]

Rbick: Phone posting is what normally makes a bollocks of my posts... However its fine once you get used to it. The project is part of my research into the caseless detonator and some charactaristics of initiation.

Decietful_Frank: Thanks for the help, however it was NOT a spoonfeeding request, I did my homework, but was getting relatively low ETN yields as of late, so I was wondering about other methods. I get at best 1.3 grams of ETN from 1 gram Erythritol using the 'Axt' metod with AN.

Seeing as I am still relatively new to the 'advanced chem' of nitration (Off topic I think but... Today I worked out how the nitration of PETN proceeds, it was not too hard after all. The four OH- groups are replaced by NO3- groups and the four OH- bind to the free H+ from the HNO3, or am I completely way off?) and I do not completely understand it (RDX nitration is getting on my nerves, according to wiki its (CH2)6N4 + 4HNO3 → (CH2-N-NO2)3 + 3HCHO + NH4+ + NO3- but WTF? Would the NH4+ and the NO3- not just form
NH4NO3? And does formaldehyde (HCHO) not react with AN to make more RDX? Or is my reasoning off yet again...)

Anyways, back on topic, Has anyone made ETN:PIB plastique? Would 10% PIB make even a cohesive mass? Or just an undetonable mess. Frank, I know your PIB and ETN detcord one, and thats on my to do list... However what about a plastique like a cheap, shitty C-4? Put that Ragnar's so called 'C-4' to shame...

[Alexires]

Frank - Don't quote whole posts. You only needed one line to get the point across.

I'm getting sick of more senior members quoting whole posts. Any more and the ban hammer comes out and we get to play the waiting game.

[Deceitful_Frank]

Frank 0- Don't quote whole posts. You only needed one line to get the point across.


Sorry Alexires, I was in a rush to get that post in and didn't think to shorten the quote. Hope this is better!

-=HeX=-, I believe the fist part of your third paragraph shows you understand the process more than enough for the purposes of amateur nitration of PE though I like to think of nitric acid as HO-NO2 and the hydroxyl group on the carbon backbone of the polyol as -O-H.
I think that the nitric acid is attacked by the polyol giving -O-NO2 and the free hydrogen atom combines with the -OH from the acid giving H-OH... water :)

This is how I understand this process and it works for me but feel free to correct my if you believe I am wrong.

Synthesis of RDX goes by NITROLYSIS not nitration. Of course you can nitrate hexamine with cheap HO-NO2 (HNO3) to give yourself a head start and make the process more efficient (HDN is half way there as far as nitric acid needs go)

I am not going to pretend to understand the full process enough todirect anyone in a synthesis. I kinda get it in my head but not on paper if that makes sense.

Personally I see not real need to make RDX as long as PETN is available to me as in small scale experiments, the latter is better in almost every way.

IF you can get the ETN into small cubic crystals of two sizes, one 6 times the size of the other and in like a 4:1 ratio (this is going to take a LOT of work) then you MAY get a cohesive has with 15% PIB and oil/plastisizer.

Otherwise shoot for 20% but hit it HARD and I mean HARD and in strong confinement or you will just coat the surroundings in creamy goo...

[-=HeX=-]

Frank: Thanks for the advice on plasticizing, I find that after my extensive purification that making a really hot, super concentrated solution of ETN in acetone (propanone) then crashing into a large amount of ice water gives a flour like powder which is perfect for pressing and casting but is annoying to pour into detonators because it 'clumps' into lumps (try dripping a SMALL amount of water onto flour and try to press it, or make it into a det because it is highly annoying. In terms of crystal and de-clumping it acts like my old TATP...) I have bought a cheap microscope set which was for biology work (I enjoy examining fly's wings under high power) and because of my nice chem teacher I may be able to borrow a camera attachment and data collection kit (temperature) for a while.

Yesterday she (My chem teacher) and I discussed esterification at length, however it was mostly how acetates work, then she briefly mentioned nitration. I believe Urbanski was a bit wrong when he claimed sulphonation occurs before nitration in PETN syntheses because I see it as unnecessary and impractical for some abstract reason which I cannot put into words. The RDX is all for the tests, ETN and PETN will remain my main secondaries, however for the CLD project RDX will be used simply because that is what Microtek used.

Believe it or not, the tests are part of a project which I am doing for next years national science competition, last year I saw coil guns, a project on modified airsoft weapons (ballistics on the ballistics gel, and on humans and animals! The guy shot himself repeatedly in the arm at varying velocities and projectiles) seeing as my RFID project did not qualify this year. Therefore I am giving it my best shot, and putting all my time and money into it.

Methanol I believe makes the lovely cubic crystals, so slow and fast recrystallization would give the two sizes I think. I am not aiming for a 'perfect plastique', just a sticky, shapeable mess for now, but seeing as I can get PIB, styrene-butadine (sp?) rubber and more I can try a few plasticizers anyways.

Rbick: I loved the video, and I found a supplier of airsoft pyrotechnics through a 'Related video' and they sell 'Thermobaric grenades' however they are really just amazing flash devices. UK and EU members PM for details if you so wish. Also, I have an interesting article on the effects of shockwaves on the brain, which I shall be OCR'ing soon, once I dig up the magazine. The plastique demo was really interesting, it shows what I meant by high VoD giving a short, sharp shock wheras low VoD gives a more sustained, crushing one.

Alexires: There ARE female members, Frostfire was one. Also the first professional pyro I worked with was female... However they are few and far between. anyways I see the Katey/ Jenni person as a cop posing as a FEMALE PYRO to entrap young male pyro's for the FedGov. What male pyro could resist meeting a female pyro :P

[Alexires]

With the ETN synth, I would say the H2SO4 donates a proton to HNO3 which then seperates into water, giving H2O + HSO4- + NO2+.

HSO4- then takes proton from the Erythritol leaving RO- which the NO2+ then adds to to give ETN, H2SO4 and H2O over all.

With straight HNO3 and Erythritol, I would assume it goes as you stated Frank.

[tranquillity]

The reaction of NO2+ with R-OH proceeds via Sn2 with an intermediate R-O(NO2)(H)+ formed when NO2+ attacks a lone pair on the oxygen (The positive charge is, formally, on the oxygen). The electrons in the bond O-H are then donated to the O and H+ leaves. RO- couldn't exist in the strong acid conditions of nitration.

Using conc. HNO3 (>90%) you get spontaneous dissociation 2HNO3 <--> NO3- + NO2+ + H2O and the reaction proceeeds as above I believe.