Sciencemadness Discussion Board

A few questions

AngelEyes - 27-1-2003 at 09:53

Hello everyone - new member here.
I have a few questions that I am sure experienced fellows such as yourself could answer. Apologies if some of these seem to be in the wrong topic.

First off, let me say that I live in England so I can't just go out and buy chemicals - the rules here are ever so strict and almost everything remotely dangerous is banned. That said, there are still a few reagents availbale here and there...you can buy 95% H2SO4 as drain cleaner and NaNO3 is available as fertiliser. No KNO3 though, nor any Ca(NO3)2.

1. Is it practical to try and get NH4NO3 by mixing NaNO3 and (NH4)2SO4 in hot water, cooling it all down, and then trying to filter off the relatively insoluble Na2SO4? NH4NO3 seems like a perfect HE to me (non toxic, very insensitive etc) but you just can't buy it OTC here.

2. Has anyone tried the aluminium powder that you can get for resin castings? You can buy that here quite cheaply, but it seems to good to be true. There must be a drawback (like the powder is mixed with inert crap or something) - anyone used it in any formulations?

3. Is the only way of getting decent HNO3 (70% +) without buying it to distil it? Is it not possible to just let conc H2SO4 and xNO3 sit in a bow until all is dissolved and just use that (with extra H2SO4 if needed) as a nitrating mix? Is the yield bad or something? I am thinking just with cotton, no glycerine or anything - I am not that mad.

4. I have successfully made nitrocellulose (quite reasonable quality actually) and added acetone to get a lacquer. I let this dry and got a thin sheet of celluloid. This burned quite nicely in open air, but not when I sliced off a strip for use as a fuse in a thin paper tube. How come - I thought it had it's own Oxygen so it wouldn't go out? The un-gelled NC works good, that just flashes down the whole length.

5. I have heard much about Acetone Peroxide (AP), easy to make, powerful etc. It seems a real nice material apart from its sensitivity. Some people were saying that you could mix it with NC and acetone to get a putty which, when the acetone was evaproated, left a doughy substance that had the power of AP but wasn't nearly as sensitive. Anyone tried this? Does it work etc?

I know I have loads more questions, but my mind has gone blank all of a sudden, so I'll have to leave them for the moment.

Thanks for any help you can provide.

Darkfire - 27-1-2003 at 17:04

1. AN is not a very good choice, seeing as how small amounts are hard to set off, and its a sensitive as a rock, it will be hard to detonate.

2. Never used it.

3. Mixid acid will do for most nitrations, glycerine, starch, cotton, MNT and DNT.

4. Cant tell ya why, id just twist it into a fuse myself, less work and better performace.

5. I cant say AP is a good starting HE, but its not incredibly hard to make, just make TCAP by keeping temp low.

Sorry i coudnt help more, there are mch better posters than myself here, though.

CTR

DeusExMachina - 27-1-2003 at 19:41

for question 5, did you mean when you mix the nitrocellulose an dacetone you get a viscous putty which when you mix with AP, you get AP putty? or you meant that nitrocellulose and acetone make AP? if you meant that, that doesn't make AP. Making AP putty will make the stuff less sensitive but lesss powerful and harder to detonate. Also, be careful when mixing the putty with the AP (and use TCAP, not the dicyclo version) because you might accidentally detonate the AP if you mix the AP roughly. as long as you are careful with the AP, it's sensitivity shouldn't be a problem.

I hope I have helped a little.

Polverone - 27-1-2003 at 19:55

1) As Darkfire has said, you won't think "insensitivity" is good after you've experienced just how insensitive ammonium nitrate mixtures are. ANNM - ammonium nitrate and nitromethane - can be set off without a booster, but if you can't get ammonium nitrate I'd be surprised if you could get nitromethane. It is possible to process the ammonium nitrate to "activate" it, so that it becomes much more sensitive to initiation, but you'll probably still need a fairly powerful initiator. A mixture of ammonium nitrate with a low percentage of an organic peroxide (such as 90% ammonium nitrate, 10% acetone peroxide) is popular and easy to initiate, but given the sensitivity of organic peroxides I really can't suggest such a mix. There are other methods for sensitizing ammonium nitrate to be found in patent literature and more obscure references (such as adding a small percentage of copper salts), but you don't want to experiment with unusual materials until you have some more experience.

2) I've never tried this aluminum powder intended for resin castings. It probably is not suitable for flash powder, but it may be okay for other pyrotechnic compositions, for thermite, or as an explosive additive.

3) Darkfire is right but I think he used the wrong term. You can use a nitrate salt plus H2SO4 for many nitration reactions, but it does sometimes lead to a very thick nitration mixture and/or leave more contaminants to clean from the finished product.

4) ...

5) If you must make acetone peroxide, start small. Very small! It is pretty friction sensitive and extremely heat sensitive. I had it spontaneously explode in a container that had recently been rinsed under hot tap water, when I made it several years ago. It is a lot of fun, but no amount of fun is worth being maimed for life. One of my friends who experimented with it at around the same time I did (before you could look up all this info online) lost his left hand to it. One of these days I should scan and post the newspaper clipping I saved about the incident as a reminder of its danger. I wouldn't make NC putty with it, either. I don't recall where, but I remember reading about someone who had the putty explode as it dried, probably from stresses set up in the shrinking material. Basically, assume that acetone peroxide is going to be dangerous no matter what.

HMTD is slightly better. It, at least, won't sublime and form large, dangerous crystals like acetone peroxide will. But it is still far from safe.

I would suggest that DDNP is a better primary, safety-wise and performance-wise, but it seems that people usually have trouble making it, and you would need a considerably larger selection of chemicals than I think you have right now.

In the UK, aspirin is fairly expensive and cannot be purchased in large quantities - am I right about this? Because in other countries, aspirin is inexpensive enough to be used as an explosive precursor for picric acid, which can be used to make metallic picrates or DDNP.

AngelEyes - 28-1-2003 at 02:01

Thanks for those.

I appreciate Ammonium Nitrate would be real hard to detonate but I was just asking if the method I outlined for producing it would really work?

Yes, a larger selection of chemicals would be nice. Its possible to get some useful bits in this country but the good stuff (like perchlorates and the like) are just not to be found. There's nothing like Skylighter or Pyrotek in the UK. I know (per)chlorates can be made with chlorides and electricity but that seems like a lot of hassle for little product. I ough to point out that I do not live on my own and so any odd smells or noises or anyhtng get noticed quickly. It's also hard to get hold of glassware and other lab equipment. I have found places (like photography stores, ceramics stores) that sell materials like KMnO4, CuCl2 and denatured ethanol but not much else.

I don't specifically want to make Acetone Peroxide, it just seemed quite easy and cheap. The only reason I have made NC is because I managed to acquire a 1litre container of 70% HNO3 from a summer job at a large pharmaceutical company...but that's almost run out now. I used to make meal powder with NaNO3 and garden Sulphur - it worked but it was far from ideal and it needed SERIOUS confinement to make it bang.

Aspirin isn't that expensive - you buy the bog standard un-branded stuff - but I haven't tried to synthesize TNP...don't like the idea of the toxicity. Ammonium Picrate seems like a decent choice though.

I haven't come across Nitromethane anywhere in the UK, though I would imagine it is hard to get hold of as it has Nitro in the name.

I have given up fuses with the gelled NC - just take the raw nitrated cotton instead, washed of course, and wrap that in a thin paper tube. The flame will flash down it in, well, a flash. Very reliable.

I haven't yet made HMTD but it's on my list. I just don't know if the solid fuel I have is Hexamine or not. I suppose I could burn some, let it go out and then smell for the fish...

Cheers.

Polverone - 28-1-2003 at 03:44

Hmm, I had recollections of aspirin being sold in the UK at high prices, and there being restrictions on how much you could buy. Maybe that was only a historical thing. I can get a bottle of 200 325 mg tablets for a dollar, so it works out to about $15/kg. Not too bad. Of course that doesn't take into account the time and cost of removing binders. If you can get aspirin for similarly low prices, I would definitely suggest that you look at picric acid/picrates. Toxicity isn't a problem if you do the nitration outdoors with good ventilation and wear gloves while you're working.

I'm positive that you can get sodium chlorate in the UK, as weedkiller. It is one of the few things you can find there that you won't find in the US. The chlorate can be precipitated as KClO3 if you add potassium chloride to a solution of it, even though it will be mixed with a fire retardant material (common salt?) The KClO3 can be used to make pyrotechnics and to make better fuse.

You can try mixing sodium nitrate and ammonium sulfate and see if the resulting ammonium nitrate solution is pure enough for pyro purposes. It would be easier if you could get calcium nitrate, but I suppose that is out of reach too. Even if your initial NH4NO3 solution isn't pure enough, you should be able to get something that's at least pyro grade by boiling the solution to a small volume and then cooling it to crystalize out the NH4NO3. NH4NO3 is extremely soluble at high temperatures. It's also impressively soluble at low temperatures, mind you. But you should be able to crystalize out about 7/8 of the NH4NO3 if you go from a saturated 100 degree solution to a saturated 0 degree solution. The sulfates don't show nearly so much difference in solubility with temperature, so it should be doable. It may end up taking a lot of time and effort, though.

Ammonium nitrate crystals are extremely hygroscopic. You might have to store them in a sealed plastic tub with a dessicant like calcium chloride.

AngelEyes - 28-1-2003 at 08:26

Right, aspirin IS cheap over there...not anywhere quite as cheap here but still not out of the question for TNP / Picrates.
I can get NaClO3 over here in weedkiller (53% w/v) but it does have a retardent added. You can use it as is for meal powder, again it's not great, but I haven't been able find out what the retardent is nor how to reliably separate the chlorate to at least 90% purity. Besides, chlorates are a little dodgy with metals, sulphur, acids etc and I had a bad experience with NaClO2 once.
I had planned to use the relative solubilities at temperatures to separate the 2 compounds as it does seem quite easy. I know NH4NO3 is hygroscopic - so's NaNO3 - but I thought it might not only be a good HE but also a potential rocket propellant? The one thing I have failed miserably at so far is getting a rocket airborne.
I do also need to get gloves. I have a coat (well, old shirt) and eye protection but no decent gloves. Are food industry gloves any good?

Thanks.

asprin source

rp3o8 - 30-1-2003 at 15:27

Try animal supply stores (PetsMart) for cheap aspirin. I’ve found 1lbs bags of horse aspirin for $10 USD. There is usually no binder so purification isn’t needed.

AngelEyes - 31-1-2003 at 02:11

never even considered that - cheers.

NaClO3 retardant

chemoleo - 26-7-2003 at 22:45

in the weed killer found in the UK is generally Na2CO3, sodium carbonate.

CROpyrO - 27-7-2003 at 02:45

can somebody tell me HOW toxic is dry picric acid and are the picrates also toxic ????? i made AP but it is very dangerous so i stoped with it,HMTD the same problem , AN-> i have 2 kilo and i just can't detonate it , NG->VERY DANGEROUS , no interests , TNT -> i can't find 95% HNO3 , with RDX the sam problem->no conc. nitric acid . i wan't to make some HE but i just don't know what would be the best and smartest choise .( medium sensetivity , high power ( velocity )...) please , can somebody help me with this ???

Nick F - 28-7-2003 at 07:12

Nitroglycerine would be perfect for you, don't believe all the crap about it being super-sensitive. It's probably hundreds or thousands of times safer to use than AP. After you've made it, mix 1 part of it with 9 parts of AN, or 2 parts with 8 parts AN, and you will have made what you're after - a medium sensitivity, high powered explosive.
Or make NC. Or buy some mannitol and make MHN. Or experiment with cheddites, various ANFuel mixtures, etc. There are many many choices.

But I get the impression that first you need to do some more reading...

PS - you don't "find" 95% nitric, you make it.

AngelEyes - 28-7-2003 at 08:09

I'd heard it was NaCl as the fire retardent...

I have heard bad things about NG which is why I have never tried to synthesize it...like it'll go off if you look at it wrongly etc. I like NC as it's easy to make and relatively stable (especially if soaked in a carbonate before drying). I too would be interested in any practical data regarding picrates as picric acid seems to be quite an easy synthesis. Well, easy 'ish with OTC chemicals and no tricky distaillations etc. Are picrates any good for propellant purposes? Might it be possible to mix them with an energetic, but sluggish, filler to get a good composite rocket propellant? Like vaseline (OK - vas isn't energetic) or NC?

Nick F - 28-7-2003 at 08:41

With an oxidiser then yes, it could be made into a rocket fuel. But it is way too negative in OB to work without a good oxidiser. I would use only picric acid or ammonium picrate to avoid sensitivity problems. Adding TNP to NC would only reduce the NC's performance as a propellant.

Those bad things about NG are lies (or exagerated half-truths at best), if you made it you would see that... From my point of view, its ONLY drawback is the fact that it's a liquid, which can make charge construction tricky. Although for some purposes it is an advantage - no pressing needed and it's at a constant density.
But if you don't like it as a liquid, just soak a bit onto some anhydrous AN. Only a few % is needed to make it detonatable. And so you only need to make a few mL for a half-pound charge, for example.

Think about it - NG has been used in huge quantities for the past 100 years or more. So it can't be that bad.

CROpyrO - 28-7-2003 at 08:50

i heard that the TNP is a great explosive , only problems is that it forms sensitive metal picrates and it is very toxic . but it is great that its so powerful and easy to make ( but not very safe specially if you make it out of aspirins(NOx) . i could make some to test . how much ammonium picrate will i get out of 1 g of picric acid and 100 ml ammonium hydroxide ? if somebody knows some information , please post reply.

Madog - 28-7-2003 at 09:30

my cnclusion with metal picrates is that they suck

ive heard ammoniumpicrate is pretty damn insensitive, i dont have any examples though.

makeing it from asprin can be a pain in the ass, doesnt always work well, and if you get NO2 that means you did it wrong, too high temp, something else in there being oxidised, etc.

your going to get less than a gram from a gram of picric acid, sience your going to loose some of the product sience it will be stuck on your reaction vessel. theoreticaly you would get 1.07g
http://flashbangboom.homestead.com/procedures.html
look there for an experimental yield.

its definately not worth makeing ammonium picrate IMHO, you loose explosive, the product isnt as powerful(and has an even worse OB), and its relatively insensitive.

CROpyrO - 29-7-2003 at 01:15

good site , i like that he calculated the cost of every explosive. picric acid and isopropyl peroxide are momentarily only HE that i can make becose i don't have any more HNO3. yes i heard that metal picrates are shit becose of the sensetivity, and ammonium picrate becose you get small yield , i don't have many choise, i'l do some more tests with them , i guess . :D

AngelEyes - 29-7-2003 at 01:19

I appreciate what you're saying about NG, but it does have a really bad rep. Maybe 'cos it's the best known explosive (with the possible exception of TNT), one of the oldest etc, could even be a cynical ploy by the establishment to deter would-be experimenters from playing with such an easy to make and damn powerful substance.
The subject of headaches worries me - I get them sometimes and the last thing I want is a nitro headache (although it would have to go some to compare with the migraines I sometimes get).
On the plus side you do get uniform density and you can lessen the shock sensitivity by soaking in sawdust (or other suitable porous material). I can see that a few ml would be good to sensitise AN, but I don't have any AN, nor do I know any friendly farmers. I would probably use it to form a composite with NC for propellant purposes, but at the end of the day I am just too paranoid about making something with such a bad name from drain cleaner and fertiliser. I will try TNP next, and go back to the drawing board as regards black powder - if I can't even get correct then I have no right to play about with other materials. I think I need a ball mill...

CROpyrO - 29-7-2003 at 01:33

here are some information about picric acid that i found on net :

Attachment: TNP Synthese23.doc (348kB)
This file has been downloaded 7588 times

Madog - 29-7-2003 at 07:33

i meant they are shit because their power and initiation ability sucks.(metal picrates)

i seem to be pretty reesistant to nitric ester headaches, ive taken whifs of methyl nitrate and not gotten a headache. ive gotten NG on my skin with no headache, too. the times i did get headacheswas from getting NG solution in acetone all over my hands,and tasteing NG, twice.

if you make ammonium picrate and atempt to detonate it, definately make a good amount, and use a good booster to det it. i heard someone used something like 10 grams of picric acid, something bigass like that, and failed. dont take that word for word though, i read this probaly 2 years ago in the E&W archives, perhaps doing a search there could yield some info on sensitiveity.

AngelEyes - 29-7-2003 at 07:56

I'd love to...but every time I click search it says I do not have permission. I have a username and p/w, and can login, but can do nothing else. I corresponded with Megalomania about this and he said that a wait of 2 weeks was mandatory. Fair enough, but 6 weeks later I still can't do anything but look under the topic headings - even clicking 'view todays posts' gives me a permission denied error....which is a bit of an arse.

CROpyrO - 29-7-2003 at 09:22

i heard that ammonium picrate is slightly less sensitive than AN . only bad thing by ammonim picrate is making it. you need lots of ammonia water ( it is expensive , at least where i live ) and the yield smaler then picric acid that you used to make it . advantage is that it doesn't form sensitive picrates any more and it isn't sensitive ( you can detonate with a better homemade blasting cap/booster ) . when i find cheap horse aspirins i will make it . by then il have fun discussing with you guys. :D

Madog - 29-7-2003 at 10:40

holy shit! slightly less sensitive than AN! dont bother with it! just use the TNP!

blip - 29-7-2003 at 20:26

Quote:
i seem to be pretty reesistant to nitric ester headaches, ive taken whifs of methyl nitrate and not gotten a headache. ive gotten NG on my skin with no headache, too. the times i did get headacheswas from getting NG solution in acetone all over my hands,and tasteing NG, twice.

Hmm, Madog, do you ingest a lot of caffeine or something similar?

CROpyrO - 30-7-2003 at 06:26

angleleyes!? , have you made picric acid ???? i made experimental yield just to see if it will work with chemicals that i have. i say it was good. i got about 200 mg of picric acid with one 225 mg ACA pill ( not aspirin , i didn't momentarily had any so i used other pill containing ACA ) . tommorow i'l maybe make larger amounts. for a few days i go on vacation so i have to detonate all stored explosives that i have . ill have fun :D ;)

AngelEyes - 30-7-2003 at 07:12

Officially, I have never made any illegal energetic materials, nor do I have any desire to.

Unofficially, no, I have not made TNP. Not yet, anyway. It is next on my list. With the exception of my unspectacular BP, which fizzled and pearled, I have only ever made Cellulose Nitrate. This was quite good, though, with just 1 gram giving a loud report in a cardboard tube with basic confinement. Would make a good payload for a rocket...if I could ever get one of the ground. Maybe I should try to purify NaClO3 from weedkiller and try that with carbon for a propellant - think I'll leave the sulphur out though...

Madog - 30-7-2003 at 08:45

nope... i dont drink coffee, sometimes mountain dew but not much at all. im a real big guy, that might have something to do with it

edit: oh yeah, i dont do cocain either, in fact, i dont do any stimulants at all

[Edited on 7/30/03 by Madog]

CROpyrO - 30-7-2003 at 09:37

yeah ,sure ,and i only made black powder ... ;)