Log in

View Full Version : No nitric acid - Archive File


megalomania
May 10th, 2003, 09:40 PM
radar
Frequent Poster
Posts: 73
From: Redding California
Registered: DEC 2000
posted 01-09-2001 01:42 AM
--------------------------------------------------------------------------------
Hey, any of you guys know some of the more common nitration recipes that are done without nitric acid but instead involve adding some nitrate to the bath to make nitric acid? Thanks.


sadsakjoel
Frequent Poster
Posts: 170
From:
Registered: OCT 2000
posted 01-13-2001 01:50 AM
--------------------------------------------------------------------------------
do you mean like picric acid with aspirin? where you mix the acid from aspirin with sulfuric and potassium or sodium nitrate instead of nitric acid? If this is what your talking about I'll post the rest later.


radar
Frequent Poster
Posts: 73
From: Redding California
Registered: DEC 2000
posted 01-13-2001 02:12 AM
--------------------------------------------------------------------------------
No, I already know about that one, something like maybe NG or RDX, or TNT, or EGDN.


Stone
Frequent Poster
Posts: 140
From:
Registered: SEP 2000
posted 01-13-2001 04:20 AM
--------------------------------------------------------------------------------
Yes, recipes LIKE the picric acid one. Does that idea work for any other nitrations that usually require HNO3?


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-13-2001 09:56 AM
--------------------------------------------------------------------------------
Apparently it will only work for simple nitrations like NG/NC etc. I'd say RDX without HNO3 is asking for a bit much! (i.e no chance!)


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-13-2001 11:47 AM
--------------------------------------------------------------------------------
Yeah, I've heard that impurities of sulphur compounds can cause very low yields when making RDX by decomposing one of the intermediate reactants I think.
I know for a fact that it works when making NC, because that's the method I use.


radar
Frequent Poster
Posts: 73
From: Redding California
Registered: DEC 2000
posted 01-13-2001 07:48 PM
--------------------------------------------------------------------------------
Well, Mr. Cool, can you give me your exact method for making NC, I bet this would work for EGDN as well due to the acids being the same.


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-14-2001 07:22 AM
--------------------------------------------------------------------------------
Sure. I use 1 gram of sodium nitrate, added to 4ml of cold 98% H2SO4 and stir it to dissolve the NaNO3. Let it cool to around 5 C by placing the reaction beaker in a bowl of iced water. When this temperature has been reached, put in 2 grams of cotton wool (the absorbent stuff from pharmacies etc.), and hold it under the acid with a glass rod, while stirring continuously for 20 to 30 minutes at 5 to 15 C. Then get the NC out with the glass rod and plunge it into 100ml of 10% NaHCO3 solution, then rinse it with water, then again with sodium bicarbonate solution and so on until the wash with water is neutral, pH7. Then dissolve the NC in acetone to form a runny liquid (not very concentrated NC solution), and filter it through a fine mesh to remove any unreacted cotton. Evapourate the acetone, and you'll be left with pure NC. I then CAREFULLY file it into a powder, slowly with a hand file and store it under 2% NaHCO3 solution. Obviously this can be scaled up to produce any amount.
I suppose the same basic method would work for EGDN.


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-14-2001 09:02 AM
--------------------------------------------------------------------------------
Sounds good! Two questions, can you use KNO3 instead of NaNO3? Will 91% H2SO4 work or will I need to go out and buy a hotplate to concentrate it?


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-14-2001 09:27 AM
--------------------------------------------------------------------------------
KNO3 will work, but remember: K (39 atomic mass units) atoms are heavier than Na (23 a.m.u.) atoms, so each gram of KNO3 will contain less NO3- ions than a gram of NaNO3, so adjust the amount accordingly.
91%? Hmmm.... I think that'd work, but it might be worth getting a hot plate because it won't work for many other explosives. Where did you get the H2SO4 from? I'm having to boil battery acid, which is dangerous, boring, time consuming and very expensive.


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-14-2001 12:08 PM
--------------------------------------------------------------------------------
Ok, I'll get the calculator our later and work that out. The H2SO4 is "one-shot drain cleaner" available from B&Q Wharehouse stores, £4.99 for 1L.


radar
Frequent Poster
Posts: 73
From: Redding California
Registered: DEC 2000
posted 01-14-2001 03:51 PM
--------------------------------------------------------------------------------
Will this work with ammonium nitrate? THanks


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-14-2001 07:20 PM
--------------------------------------------------------------------------------
Isn't NC hard to detonate? Or do you just use this stuff as a low explosive?


SATANIC
Frequent Poster
Posts: 237
From: australia
Registered: SEP 2000
posted 01-15-2001 01:21 AM
--------------------------------------------------------------------------------
what is the process by which you purify the H2SO4? straight boiling? I thought you couldn't boil it over a certain % before it will not purify any more. How do you test the conc. when finished? thanks in advance.


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-15-2001 01:30 PM
--------------------------------------------------------------------------------
It will work with AN if you: a) dry it in a low oven first, and b) adjust the amount used so that you have the same amount of nitrate ions.
NC isn't very hard to detonate, as long as it's got a high enough N percentage. It's much easier than TNT, ANFO or ammonium picrate for example, and about the same as RDX I think. Also, since it's a very energetic deflagrant, it can make the transition from deflagration to detonation if fairly large quantities are ignited in a strong container. I normally use it as a low explosive or a plasticiser for AN or RDX with things like NM, but I do sometimes use it as a base charge in detonators.
Boiling can get H2SO4 to about 95-98%. The boiling point will rise to something like 140 C, but I don't know the exact figure. You can test the specific gravity with a hydrometer which you can buy at places that sell wine making kits. 98% H2SO4 has a specific gravity of 1.84 (H2O = 1).


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-15-2001 06:00 PM
--------------------------------------------------------------------------------
Ah, I was thinking of smokeless powder NC, I didn't think it would be easier to nirate further than that.
I worked out 1.7gm of kno3 should give the same number of nitrate ions as 1gm NaNO3.

I tried it today, I used five timmes your figures, 20ml 91% H2SO4, 8.5gm KNO3, 10gm cotton wool. Having added all the kno3 (in an ice bath) and after a while of stirring, there were crutsy white lumps left, I figured either these were impurities in the kno3 (the only thing I could think would be in there would be chalk which should have dissolved) or the solution was saturated. I ran the solution through a fine sieve that got rid the crap, the solution was yellow at this point.

While I was weighing out the cotton wool I relaised that there was no way in hell I was going to get all that cottn wool into such a small volume so I shredded and added enough so that ther remained enough liquid to cover the soaked wool (I reckon about 1/2gm). I stirred it for 20mins then left it for another 20 to have a cup of tea. I washed it in 10% sodium bicarbonate solution (lots of foaming!) 3 times with and equal number of plain water washes in between. I fished out the lump of wool and put it in cheap, clear, no additive nail varnish remover, I'm going to leave it till tommorrow to give it fair chance to dissolve (had a white soup after a few mins so I guess at least some of it has dissolved).

I kept a check on the temperature of the solution when stirring the wool and it stayed at 7*C throughout.

How on earth do you get 2gm cotton wool into 4ml of liquid?! Does it sound like I've seriously messed up? If this works it would be good because it's really thrifty with the acid and cotton wool costs nothing.

Thanks for the procedure!



Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-16-2001 01:13 PM
--------------------------------------------------------------------------------
Sorry! I made a mistake in the method. I meant to say 0.2 grams of cotton wool per 4ml of H2SO4, not 2 grams! I can see why you might have been a bit confused!
Also, I really think it would be better to use 98% H2SO4, because during the nitration, water is produced. When the acid conc. gets below a certain point, the nitration practically stops. It would obviously reach this point a lot sooner if you're using 91% acid, so the cellulose might not be as fully nitrated.

Don't worry, the nitration mixture should be yellow, due to the formation of nitric acid and nitrogen oxides in it.

Potassium nitrate is considerably less soluable than sodium nitrate (in g/100g H2O), and also more of it is needed so maybe this is why it didn't all dissolve.

If the nail varnish remover is an acetone/water mixture, the NC might not dissolve fully, but it shouldn't really matter.

Also I forgot to mention (sorry!) that it's good to soak the NC in a weak, 1% or 2% sodium bicarbonate solution for 10 minutes or so at about 60 or 70 C to make it contain less acid, although the method I gave you should have done a pretty good job of that already.

So it should have worked the way you did it, but if it's not fully nitrated then try concentrating your acid further. The fact that it's dissolving in the acetone is obviously a good sign.

Let me know how you get on!

Hope this cleared things up a bit.



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-16-2001 02:11 PM
--------------------------------------------------------------------------------
Ah, 0.2gm, certainly clears that problem up! I ran the NC/acetone through a fine sieve, the cotton wool recovered iso only about half of what went in so at least some of it hould have dissolved. It's evaporating now.
As I was doing the procedure I glanced at some of my stuff and realised I already have a box of NaNO3, doh.

I'll concentrate the acid for next time. I'm moving house at the end of the month and this one's got a nice shed I can permanetly setup as a lab, sort out a still and start doing things properly.



Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-16-2001 02:19 PM
--------------------------------------------------------------------------------
Yeah, a nitric acid still is essential for most high explosives if you're serious. And try to get an extractor fan in the shed, to get some nice clean air in while you're using it!
Does anyone know how much a couple of acres of land is?! I really want a pyrotechnics liscence!



Smartguy
New Member
Posts: 11
From:
Registered: JAN 2001
posted 01-16-2001 02:45 PM
--------------------------------------------------------------------------------

quote:
--------------------------------------------------------------------------------
Originally posted by Anthony:
Apparently it will only work for simple nitrations like NG/NC etc. I'd say RDX without HNO3 is asking for a bit much! (i.e no chance!)
--------------------------------------------------------------------------------

Well, Anthony, you're wrong. One of the better recipes for making RDX doesn't use HNO3. It uses ammonium nitrate and acetic anhydride. The latter will be a problem, though: you probably will have a difficult time obtaining it.

I'll try if I can retrieve this recipe for you...

[This message has been edited by Smartguy (edited January 16, 2001).]



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-16-2001 02:50 PM
--------------------------------------------------------------------------------
Shall do. I suppose it depends what kind of land! Land suitable for beuilding on is about £12 a square yard (or metre)IIRC but a field that's is useless for growing stuff or grazing should cost very much at all. Have you got something that lists the requiremnts for a pyro license? COuld be an interesting read.


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-17-2001 10:55 AM
--------------------------------------------------------------------------------
As far as I'm aware, the NH4NO3/acetic anhydride method for making RDX uses a different reaction than nitrate/H2SO4 reactions, which use the H2SO4 and a nitrate to form nitric acid in solution.
I've got the requirements for a liscence that enables you to make small amounts of low explosives written down somewhere. I'll try and find it for you if you like. Basically, the place where you make them has to be at least a certain distance from roads or anyone else's property, you need a well made place to make them in with all the safety stuff, and you need to convince them that you're not mad.

How's the NC?!



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-17-2001 02:02 PM
--------------------------------------------------------------------------------
The NC worked, it wasn't very well nitrated so it didn't burn very fast but I will try again soon with higher conc H2SO4. Once again, thanks for the synthesis!
"you need to convince them that you're not mad" - Damn.

Can acetic anhydride not be synthesised from glacial acetic acid? If do manage to synthesise RDX using H2SO4/NH4NO3 and post your results I'll gladly eat my words.






Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-17-2001 02:38 PM
--------------------------------------------------------------------------------
Try a more concentrated H2SO4, and if you like I bet you could take the reaction temperature higher, to about 25 C without any danger of runaway nitration. And I think NaNO3 would be better than KNO3 due to it's higher soluability, but make sure you dry it first.
The sanity problem has always been the main obstacle for me as well! Quack quack.

Where exactly did you buy your H2SO4 drain opener? I've just looked in the Nottingham B&Q Warehouse, but they didn't have it! What section is it in? Would you consider selling me some if I can't find it?! If so, how much would you ask for 3L, including postage etc? I really need some!

Acetic anhydride can be made from glacial acetic acid by bubbling the thermal decomposition products of acetone through it. I forget what the gas is called. It shouldn't be very hard to do, but might take a bit of adjustment to make it work well (temp. etc.)



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 01-17-2001 03:41 PM
--------------------------------------------------------------------------------
I think it's ketane, it'd be a lot of effort to set up, but once yoy have it working then it'd be easy to run off batches.
I got my H2SO4 from Northampton B&Q Warehouse, it's in the plumbing section (same isle as the copper plumbing IIRC) with a bunch of other drain cleaners. There's also a small diy shop a few miles from me that sells it, it's £4.99 for a 1L bottle, I can send you some if you can't find it. It's need packing well because parcels get chucked about "a bit".

I'll try the NC without the ice bath next time (maybe have one on standby) if 25*C is OK. What are the dangers of run away nitration aside from the solution boiling and billowing toxic fumes? Is there a detonation risk?



Agent Blak
Frequent Poster
Posts: 766
From: Sk. Canada
Registered: SEP 2000
posted 01-17-2001 04:44 PM
--------------------------------------------------------------------------------
What about for PETN?
does anybody know if you could use this method for that? and if so how much would you need to replace the HNO3?
Your help it greatly appreciated.

------------------
A wise man once said:
"... As He Waits For The Time When The Last Become First And,
The First Shall Become last"
--RATM

Agent Blak-------OUT!!



sadsakjoel
Frequent Poster
Posts: 170
From:
Registered: OCT 2000
posted 01-18-2001 04:10 AM
--------------------------------------------------------------------------------
If your problem is that you cant find nitric acid i know of an explosive (primary) that doesnt use any, TACC it involves copper sulfate which is what your looknig for and wither the copper sulfate you make TACC tell me if this is of any use and i will post the entire pocess later.
------------------
All there is to fear is your own co-ordination



Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-18-2001 02:12 PM
--------------------------------------------------------------------------------
That's what I thought: Lots of effort to set up, but simple to run.
I've heard, although I didn't really want to try it, that there's absolutely no risk of a detonation or rapid decomposition from runaway nitration until you get to about 80 or 90*C for NC. At 25*C it would nitrate substantially quicker than at 5*C or so.

I've never seen a method like this for PETN, but I can't think of a reason why it wouldn't work. I'll try and find out for you. Where can you get PE? Or do you make it? I know how to make it, but it seems quite hard because I'd also have to make the reactants.

I know of TACC, but have never tried it. I'd like to see the methid you use.



Agent Blak
Frequent Poster
Posts: 766
From: Sk. Canada
Registered: SEP 2000
posted 01-18-2001 02:53 PM
--------------------------------------------------------------------------------
I am going to find out if I can do it via this method before I start looking for it.

------------------
A wise man once said:
"... As He Waits For The Time When The Last Become First And,
The First Shall Become last"
--RATM

Agent Blak-------OUT!!

megalomania
May 10th, 2003, 09:41 PM
SofaKing
Frequent Poster
Posts: 399
From: YEAH RIGHT !!
Registered: SEP 2000
posted 01-19-2001 01:57 AM
--------------------------------------------------------------------------------
Accoording to KID (kitchen imprvised detanators) M.M.A.N. (monomethylamine nitrate)can be made with nitic acid in concentrations of 20%. I would think the sulfuric/nitrate method would work. The only problem would be procurring the methylamine.
------------------
"ARE YOUR PAPERS IN ORDER" -- Jack Booted Thug

[This message has been edited by SofaKing (edited January 19, 2001).]



Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-20-2001 08:03 AM
--------------------------------------------------------------------------------
MMAN should work for absolutely any concentration of NA, because it's an ionic compound. Any concentration of NA will have NO3- ions in it, so any concentration should make MMAN with methylamine solution.
Look under the "NM sensitising?" topic to find out how to make methylamine. it might help.


sadsakjoel
Frequent Poster
Posts: 170
From:
Registered: OCT 2000
posted 01-23-2001 09:13 PM
--------------------------------------------------------------------------------
Heres the copper sulfate part: (from FEMFEP)1.5 Preparation of Copper Sulfate (Pentahydrate)

Copper sulfate is a required material for the preparation of TAC.

MATERIAL REQUIRED:

Copper wire or pieces
Sulfuric acid (battery)
Potassium nitrate or nitric acid (field grades)
Alcohol
Water
Two heat resistant glasses or jars, one pint
Paper towels
Metal pan (for hot water bath)
Wooden rod
Cup

PROCEDURE:

1. Place 10 grams of copper into one of the jars and add one
cup (240 milliliters) of sulfuric (battery) acid. To this
mixture add 12 grams of potassium nitrate, or 1.5
teaspoons of nitric acid. NOTE: Nitric acid gives a
product of greater purity.
2. Heat the mixture on a hot water bath (near boiling) until
the bubbling has ceased (requires about two hours).

* CAUTION: This reaction evolves strong toxic fumes, and
therefore must be performed in an open, well
ventilated area.

3. Pour the hot blue liquid into a second vessel (keeping
the unreacted copper in the first jar) and allow to cool
at room temperature.
4. After the crystals have formed, carefully pour away the
liquid and crush the crystals. Then add 1/2 cup (120
milliliters) of alcohol to the powder and stir.
5. Pour the solution through the towel filter and wash the
solid left on the paper three times, using 1/2 cup (120
milliliters) portions of the alcohol each time.
6. Allow the product to air dry for two hours.

And the TACC (KIBC)
TACC (Tetraminecopper (II) Chlorate)

DETONATION VELOCITY - Not given

FRICTION SENSITIVITY - This primary explosive is as sensitive as is lead
azide

BEHAVIOR TO FLAME - Deflagrates with a green flame. Requires confinement to
detonate.

Tetramine copper chlorate is a very interesting primary explosive.
While it has these good properties it is also easily made. It's drawbacks
are the tendency to "deadpress" or become so packed that it will not
detonate the base charge in the cap and water contamination problems. For
this primary explosive to detonate it must be loose in the detonator shell.
It would be best used in caps where the base charge is pressed in first.
Rifle shell improvised blasting caps would not work well with this
explosive due to this property. In this reaction the sodium chlorate and
the copper sulfate are heated together with methanol. This reaction
produced copper chlorate. This copper chlorate dissolved in methanol. It
then has ammonia gas bubbled thru the solution. The tetramine group is
added in this step. So the main actors in this chemical play are copper
sulfate other wise known as "blue vitriol". Copper sulfate is available
from feed stores or electroplating chemical supplier. Sodium chlorate is
also a chemical required and would be available from matches, dyes,
textiles manufacture and as a weed killer. "Kitchen Improvised Plastic
Explosives" has a section on chlorate manufacture in chapters four five and
six. Ammonia is the last building block. This can be generated in one of
two ways which will be explained in the manufacture section. The methanol
used is just a reaction liquid and a carrier, as it does not actually enter
into the reaction. One problem with this process is the contamination of
the methanol with water. This allows the sodium sulfate to become soluble
in the first reaction and will remove the ability to separate the products
of the reaction. The process is longer than others but is simple and
produced a good purity, stable product. This primary explosive should be
kept dry, as it could begin to decompose in the presence of moisture.

MANUFACTURE-

Measure 15 grams of sodium chlorate into a large mouth pint bottle.
Sodium chlorate is the oxidizer in matches. It is also available as a weed
killer. Add 360 ml of methanol or ethanol to the sodium chlorate in the
pint jar. To this add 24 grams of copper sulfate. Place this liquid in a
hot water bath. Heat at the boiling point for 30 minutes with occasionally
stirring the liquid during the reaction.

CAUTION: Remember methanol is very flammable and great care should be taken
to ensure the lack of open flame in it s proximity. Avoid
breathing the vapors of methanol.

Keep the volume constant by continually adding alcohol to replace what is
being boiled away. After 30 minutes remove the jar from the water bath. The
color of the solution should change from blue to light green. Filter the
solution into a jar through a paper towel or drip coffee filter. The
filtrate (liquid) should be caught in a jar similar to the one used in the
first step. Label this liquid #1. In a narrow necked gallonjar or flask
and a stopper (one hole) place 1500 ml clear ammonia water in the solution.
This is available from the grocery store in a clear non-soapy form. In the
mouth of this is placed a stopper with one hole and a plastic or rubber
hose. This is placed into a hot water bath. Ammonia will begin to generate
out of the gallon jug. A better ammonia generator could be made by filling
a long necked bottle or flask with 250 grams lye (sodium hydroxide). 500
grams of dry ammonium nitrate fertilizer or ammonium sulfate fertilizer is
added. Addition of small quantities of water and closing with a stopper
hose set up could generate greater quantities of ammonia and it would be
drier ammonia due to the nature of its generation. Generation would be
maintained by the addition of more water. But with either method the hose
should be placed in the liquid in the liquid #1. The ammonia gas should be
bubbled through the liquid. It will begin to absorb ammonia turn light
blue. Continue bubbling for 10 minutes.

CAUTION: The ammonia gas generated will kill or cause grave damage if
exposure is severe. Use with good ventilation.

The solution will turn dark blue. Bubble the ammonia gas through solution
#1 for ten more minutes and remove the hose from the solution. Reduce the
volume of the liquid by pouring into a shallow pyrex dish. Set this dish
under a fan and allow 1/2 the alcohol to evaporate. Filter (paper towel
or drip coffee filters) the crystals that remain in the liquid and wash
them with 50 ml very cold methanol. Set these aside to dry for 16-24 hours.

CAUTION: Explosive is shock and flame sensitive and great care should be
exercised during handling.

There is another method from FEMFEP that is similar to this one, say so if you want it.

Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 01-24-2001 02:25 PM
--------------------------------------------------------------------------------
Thanks

Field Expedient Methods for Explosives Production, or something like that? I think I've got that somewhere... Does it tell you how to make lead azide from hydrazine and isopropyl nitrite and a few other things? If so, I already have it. I must have over-looked the TACC section.



sadsakjoel
Frequent Poster
Posts: 170
From:
Registered: OCT 2000
posted 01-24-2001 08:12 PM
--------------------------------------------------------------------------------
yeah thats the one, The production of TACC might not be in there, but from memory I thought it was.


Chainsaw
New Member
Posts: 34
From: Estonia
Registered: SEP 2000
posted 04-09-2001 08:29 PM
--------------------------------------------------------------------------------
Hello.... i found this old post and tried to make nitrocotton like Mr Cool described. The interesting thing is that this 'cotton wool' (that is used to clean wounds... um... this white stuff... ) disolved in H2SO4/KNO3 solution.... and mr Cool said "Then get the NC out with the glass rod" how can i get it out if it is disolved ? ...i mean there was only liquid left... like syrup, yellow, almost transparent.
[This message has been edited by Chainsaw (edited April 09, 2001).]



Rhadon
Frequent Poster
Posts: 95
From: Germany
Registered: OCT 2000
posted 04-09-2001 09:31 PM
--------------------------------------------------------------------------------
Something went wrong with your reaction. The cellulose was probably dissolved in the sulfuric acid because of a condensation reaction (just a theory of mine). This also explains the yellow color of your liquid. Perhaps the nitric acid you used wasn't concentrated enough or you used too little. It might help if you tell us the ratio and the concentrations you used.


Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-10-2001 04:12 AM
--------------------------------------------------------------------------------
Chainsaw: Did you cool your acid solution before adding the cotton? I seem to remember having my cotton dissolve, and I think it was because I didn't cool the acids down after mixing them. I can't really remember; this was about 15 years ago and I wasn't that old.


Chainsaw
New Member
Posts: 34
From: Estonia
Registered: SEP 2000
posted 04-10-2001 11:24 AM
--------------------------------------------------------------------------------
i tried it again... now i cooled it somewhere 5 celsius. this time cotton wool went very sticky mess... like homemade napalm (from gasoline and styrofoam).


Nitro
Frequent Poster
Posts: 51
From:
Registered: SEP 2000
posted 04-10-2001 01:06 PM
--------------------------------------------------------------------------------
You can make lead azid with HN3
HN3 can made bye the reaction of HNO2 and Hydrazine.


c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 04-10-2001 03:14 PM
--------------------------------------------------------------------------------
Are you sure the "cotton" you're using is real cotton? Some of the cotton-like products used in pillbottles and sold for wiping and cosmetic purposes are actually synthetic materials, which might account for the difficulties you describe. I don't think *real* cotton should dissolve (even partially) during the reaction stage of the process.


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-10-2001 03:17 PM
--------------------------------------------------------------------------------
The cotton wool shouldn't dissolve in the H2SO4/KNO3 solution... It should just be a wet mass, like when you put cotton wool in water. At least mine did.


Chainsaw
New Member
Posts: 34
From: Estonia
Registered: SEP 2000
posted 04-12-2001 09:19 PM
--------------------------------------------------------------------------------
YEEEEEHAAAWWWW!!!!!!
My first nitration completed ... successfully... (i have tried to nitrate evrery kinda stuff for 30+ times i could say... and every time something went wrong...) Last time this "cotton wool" fucked up... i dont know... the package said 100% cotton wool... but this time i got it from friend... and got it right



nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 04-13-2001 12:17 PM
--------------------------------------------------------------------------------
So did it flash like it's supposed to? And I assume you're talking about the nitrocotton, right?
------------------
"The knowledge that they fear is a weapon to be used against them"

Go here to download the NBK2000 website PDF.

Go here to download the NBK2000 videos.



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-13-2001 02:26 PM
--------------------------------------------------------------------------------
What a day...
I decided to have another go at NC today so I concentrated my H2SO4 and used NaNO3 this time.

The NaNO3 would dissolve fully so I warmed the a acid up on the hotplate and stirred it (I say "warmed" but it went upto 100*C before it dissolved). So I let it cool down, decided it was taking too long and put the dish in a water bath. Miss-judged the depth of the water and some ended up in the reaction dish.

So, start again...

Again the NaNO3 wouldn't dissolve properly so I warmed teh acid to 40*C and with a lot of stirring decided to sod the small amount that wouldn't dissolve and just leave it. Got fed up waiting for it to cool and decided that 35*C wasn't to high so put a little cotton wool in and kept a close eye on the temperature. No rise so gradually added the lot, the temperature actually dropped another 5*C by the I'd finnished the addition. Trouble was the cotton wool comletely dissolved... I've put the solution in the fridge/freezer just incase it helps, but I doubt it.

So will try *again* at 10*C another day.



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-13-2001 03:17 PM
--------------------------------------------------------------------------------
Nope, just checked it and it's very cold but still very much in solution. Seeing as it was nice and cold I put in another load of cotton. The mass soaked up all the liquid so I poured in some more H2SO4 to maintain a "bath". The mass was a sticky mess at this point and the goo had to be scraped off of the stiring rod. I put in some more NaNO3 for good measure and stirred some more and the cotton wool go started to thin and eventually dissolved. I'm not sure whether the addition of the NaNO3 caused the cotton wool to dissolve or whether it was just a gradual dissolvtion that had started when the cotton wool was added. The mixture didn't warm at all at any point. Something wierd is going on. I take it that boiling the solution presents an explosion hazard or could it be done as a last ditch attempt?


Chainsaw
New Member
Posts: 34
From: Estonia
Registered: SEP 2000
posted 04-13-2001 07:28 PM
--------------------------------------------------------------------------------
.
[This message has been edited by Chainsaw (edited April 13, 2001).]



Chainsaw
New Member
Posts: 34
From: Estonia
Registered: SEP 2000
posted 04-13-2001 07:36 PM
--------------------------------------------------------------------------------
Your "cotton wool" dissolves because it is not real... it is probably synhetic (don't beleive what package said that you bought it in) ... (that was where i failed first time)... try to get real cotton wool
I thik when you add cotton wool it shouldn't generate heat... (much) at least mine didn't.



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-13-2001 07:42 PM
--------------------------------------------------------------------------------
The strange thing is, this is the same brand of cotton wool that I used last time (which worked)... I'll try with another brand.


frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-14-2001 10:57 AM
--------------------------------------------------------------------------------
d
[This message has been edited by frostfire (edited August 17, 2001).]



Chainsaw
New Member
Posts: 34
From: Estonia
Registered: SEP 2000
posted 04-15-2001 10:33 PM
--------------------------------------------------------------------------------
umm... what's this fuss about nitrating at low temperatures. It isn't because of danger of detonating is it? for exammple this text from megalomania's site "If the temperature ever rises above 20 °C it is ruined as no more nitro will be made" ...this was description of making nitro clycerin. I thought that rising teperatures makes nitrating better.


Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-16-2001 06:55 AM
--------------------------------------------------------------------------------
frostfire: NC is actually more brisant than AP if it is sufficiently nitrated, but it should be initiated with a cap rather than just ignited. Batches that are nitrated close to the theoretical limit will probably make the DDT on its own, but to avoid burning a lot of power in this process you should use a cap.


frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-16-2001 06:17 PM
--------------------------------------------------------------------------------

d
[This message has been edited by frostfire (edited August 17, 2001).]



FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 04-16-2001 06:22 PM
--------------------------------------------------------------------------------
Im pretty sure he means DDT as the transformation deflagration-detonation (burning to exploding). Not dichlorodiphenyltrichloroethane (the insecticide)


frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-16-2001 06:51 PM
--------------------------------------------------------------------------------
understood


shooter2
Frequent Poster
Posts: 56
From:
Registered: NOV 2000
posted 04-16-2001 07:29 PM
--------------------------------------------------------------------------------
Frostfire. I read in an old tech. manual that guncotton ,in freshly nitrated form, is very friction and shock sensitive! Please don't try to pack it hard into anything. It is also very unstable because of 1. residue acid 2. cotton is an insulator and doesn't quickly dump the heat caused by decomposition. It can easily detonate all by itself.


Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-17-2001 10:18 AM
--------------------------------------------------------------------------------
Yes, DDT is deflagration-detonation transition it's just a bit long. DDT is a common abbrevation for the phenomenon.
I know of only one test that is simple to make, and that is to light it with a match.
If it is highly nitrated it will go off with a slight thump and very intensive light much like unconfined acetone peroxide.
It is probably better to use the NC in its cotton form and pack it in a pipe like you suggested rather than colloidinizing it with acetone:
- The cotton form will be less dense and thus easier to initiate.
- It is very difficult to get colloidinized NC without additives such as AP, to harden in a uniform fashion.

Regarding sensitivity, well-washed NC is quite stable; it is very flammable, but is totally impervious to shock. I don't know about friction. It is not that hard to purify it sufficiently, but it does take some time. Just put the cotton in a jar with lid, add lots of clean water then shake vigourously, replace the water and add sodium bicarbonate. Shake again ( and release the pressure ). Repeat until no bubbles are formed.

megalomania
May 10th, 2003, 09:41 PM
JB
New Member
Posts: 27
From: UK
Registered: MAR 2001
posted 04-17-2001 10:30 AM
--------------------------------------------------------------------------------
I've had a search through some of the topics and not found an answer so I'll ask here:
Is it possible to manufacture small amounts of AN by the addition of potassium nitrate in ammonia in an ice-salt bath? I know it would be far wiser to buy the stuff but I was curious whether this method of nitration would work.
Also - I was told that a good source of aluminium powder is from costume & theatre shops to give a silver/grey colour to hair.



frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-17-2001 08:29 PM
--------------------------------------------------------------------------------
hi, thanks alot for the info Microtek & Shooter2
I usually wash it over 'n over again in excessive number but that bubling indication will save a lot of time, thanks again.
PS: collodinized NC has unregular form, but what I do is to stuff a hollow pipe into the paste while it's still wet, (maybe insert the detonator) then dry it, so when it dry it will take the pipe shape and is quite hard



frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-17-2001 08:44 PM
--------------------------------------------------------------------------------
I'll just add one more question of my failed nitroglycerine
I use boiled H2SO4 until it lets out white fumes, 72 % HNO3 (test gravity), and lab grade glycerine
I take just about 30 ml of each acid, mix them, gets hot, then I wait and cool it.
Once it's cold, I began adding glycerine with a pipet drop by drop
There's about 30 seconds period between each dropping and I stirred gently and continuously
After 3 minutes, I saw that the glycerine looks like just floating around & no particular reaction or temp increase happen..
I think that the HNO3 conc is too low so I believe it's over and squirt the rest of the nitro into the solution.
Suddenly it's red NO2 gas all around.
Now, should I have succeded only I need more patience or is the HNO3 conc is too low that it's only sufficient to decompose the mixture?( I think someone say NG & NC can be made using not so high HNO3 conc)Could it be the glycerine or H2SO4?
Anyway , thanks for any thoughts..


Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-18-2001 09:16 AM

frostfire: When using 70% nitric acid to make NG, I think you should use more H2SO4; maybe about 2 SA to 1 NA.
Nevertheless, I think you should consider this method that I use:
4 grams of NH4NO3 is dissolved in 6 mL H2SO4, the solution is cooled and 1 mL glycerine is added slowly. I reccomend stirring gently with a thermometer and keeping the temp between 10 and 15 degrees C. Note that if using these small amounts, the H2SO4/NH4NO3 solution will be quite thick especially at low temperatures, but this does not affect the process.
Once the addition of the glycerine is complete, pour the solution into crushed ice bit by bit and keeping an eye on the temp.
I guarantee this process will work, and give a good yield. I use store-bought glycerine, which means 85% glycerine 15% water, lab-grade will probably give a better yield.
Regarding the hardening of colloidinized NC in the pipe: Have you tried cutting the end product open? My guess is that you will see a lot of cavities in the mass, which will lead to lower performance.

Oops I forgot to give credit to gcic who first ( to my knowledge ) suggested this
method on the forum.

[This message has been edited by Microtek (edited April 18, 2001).]



frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-18-2001 11:01 AM

eheh, I believe that NC cavities appear to be true....nice observation
I'll try that method and how about the promising one that glycerine is added into H2SO4 first then nitric acid is added into the cooled solution
Have you ever tried this and any good yield?
(wonder how the nitration process can be flipped-flopped?!?!?)


Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-19-2001 04:27 AM

No I haven't tried that other method, as the one I have works so well; I get 1 mL NG for every mL glycerol ( when you take the water content into account, so 0.85 mL NG per mL glycerine 85% ).


YTS
Frequent Poster
Posts: 61
From:
Registered: MAR 2001
posted 04-19-2001 05:35 PM

Does any one know a non nitric acid formula for mercury fulminate .and microtec or anyone do you reckon you could substitute the NH4NO3 for NANO3 by upping the H2SO4 & the NANO3 ?


YTS
Frequent Poster
Posts: 61
From:
Registered: MAR 2001
posted 04-19-2001 05:46 PM

Sorry i meant microtek . mr cool the only hydrometer i have found in a wine making shop or have used for that purpose goes from 0.990 to 1.150 sg at 20c know where near 1.82 even battery hydrometers only go to amax of 1.4 id like to know where to get one that goes up to 1.82 if any knows cheers


nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 04-19-2001 08:15 PM

I whipped up a MS works spreadsheet for calculating the amount of chemicals needed and the cost for making nitro according to microteks method. Adjust the cost according to your local prices.
It's in my video link. 1KB in size.

It would cost me about $130 for 3000mL (3 quarts) of nitro.

Microtek, what amount of sodium nitrate would you use instead of the ammonium salt?

------------------
"The knowledge that they fear is a weapon to be used against them"

Go here to download the NBK2000 website PDF.

Go here to download the NBK2000 videos.



frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-19-2001 09:20 PM

3 L for $130,
is that lab grade chemicals or improvised?
Man, then it should be made in 3rd world country
BTW, NBK2K, what is *.wks? I can't open the file with ordinary excel 97.....is that the same of MS Works Spreadsheet?


nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 04-20-2001 03:37 AM


The $130 price is at "improvised" prices. That's drain opener, fertilizer, and ag. glycerine.
But 3 liters of nitro is a lot of explosive. Almost 9 pounds of HIGH explosive. And it can be mixed with a lot of other things to make other high power explosives, like with nitromethane or AN. So you'll get at least double the nitros weight.

The biggest expense is the sulfuric acid. If you can recycle it than that would dramatically cut down the price.

Mind you, as quantities are increased, ratios change. So it may require more or less of each chemical, so prices may go up or down, depending on what's what.

I also reposted an excel version of the spread sheet. The first version is for MS works 4.5 which comes with windows I believe.

------------------
"The knowledge that they fear is a weapon to be used against them"

Go here to download the NBK2000 website PDF.

Go here to download the NBK2000 videos.



PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 04-20-2001 07:37 AM

Make your own liquid densimeter!
Use a straight Polyethylen or a glass pipe long and with a little diameter with one end enclosed! Add lead in it to allow a free floatation of the densimeter (immersion far over the gravity center in distillated water- near the open end of the tube).
Now put a mark where it floats...it is density 1.00 in distillated water at 20C.
Now use another fluid like CCl4 carbon tetrachloride at 20C mark the level on it; it is density 1.594 (approx 1.60). Now you have two lines at 1.00 and 1.60 divide this lenght in 6 equal segment with lines to get 1.10;1.20;1.30;1.4;1.5....you thus have a scale; report this length under the 1.60 line and you get 1.60 to 2.20; divide and you have a full scale between 1.00 and 2.20 density ....Simple is it? Wel maybe that you will have to do it several times to be stil in equilibrium (floatation line over the center of gravity!).

It should look like this:
top
d=1 line pure H2O
d=1.1
d=1.2
d=1.3
d=1.4
d=1.5
d=1.6 line of CCl4 (carbon tetra chloride)
d=1.7
d=1.8
d=1.9
d=2.0
d=2.1
d=2.2
/
/
center of gravity
/
.
.
.
lead weight
bottom

Let's hope it helped! ASAT (As Simple As That). Never problems, only solutions!


------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"



Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-21-2001 05:56 AM

You just need to have the same amount of nitrate ions to form the nitric, so the number of moles needs to be the same.
Since NH4NO3 has a MW of 80 grams and NaNO3
has one of 85 grams, you'd need 4*85/80=4.25
grams of sodium nitrate per mL glycerine.
The amount of H2SO4 remains the same.


Alchemist
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 04-21-2001 06:31 PM

Hello all,
Here are two froms of Mercury Fulminate that do not need Nitric Acid.

1.Mix red oxide of mercury in ammonia water for 8 to 10 days. The material becomes white and then finally crystallizes. Rince the product several times with distilled water, then dry on filter paper.The dried product explodes loudly from fire,or a heavy hammer blow! I do not think this is really a Fulminate but the Nitride of Mercury ,Hg3N2.

2.For real Mercury Fulminate the Sodium salt of Nitromethane gives with an aqueos solution of Mercuric Chloride Hg(CLO3)2 at zero degrees a white precipitate of the Mercuric salt of Nitromethane which gradually becomes yellow. Then when treated with warm dilute Hydrochloric Acid HCL, gives true Mercury Fulminate Hg(ONC)2.

P.S., I think YTS asked!

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




Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 04-23-2001 01:18 PM

You mean chlorate, not chloride I assume.
Regarding the cavities in NC: surely these would make it more sensitive if they are quite small, which in my opinion is a good thing. Does anyone know whether this is true?



Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 04-23-2001 01:40 PM

I agree that it would, but the cavities are
rather large and, perhaps more importantly, very irregular.
This would give a rather unpredictable performance. To get an idea of the extent of the cavities, consider how much of the volume of the colloidinized NC is actually acetone. Then consider that all of this acetone evaporates, leaving cavities.
I'm not sure how they prepared the NC blocks that the patent in nbk's pdf mentions.


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-23-2001 06:37 PM

Maybe they pressed the wet NC?


frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-24-2001 03:35 PM


if nitric/sulfuric acid solution is strong enough to decompose glycerine, is that mean that it's strong enough to nitrate it?


Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 04-24-2001 04:06 PM

I think they probably pressed NC, maybe with a little bit of acetone just to make it bind a bit better.
I don't think that just because it'll decompose it it will nitrate it effectively, but I could be wrong. It certainly isn't true for everything.



PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 04-25-2001 04:22 AM

No frostfire! That doesn't mean this...HNO3/H2SO4 when slightly diluted loses its nitrating power and becomes only an oxydising mix decomposing the glycerin into, aldehyds,cetons,acids and CO2!

"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"



Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-26-2001 06:09 PM

For the NC, I tried again using the ratios Microtek uses for HG (4gm NH4NO3 6ml H2SO4) and the same brand cotton wool that I used before in NaNO3/H2so4 (1gm/4ml) and it didn't dissolve this time! I also put in some bits of NC ping pong ball to see what happened. I'll wash and test it tomorrow to see if it's worked. Conclusion - there's something fucked up with my NaNO3!
Also, I tried a small test batch of Microtek's NG procedure, if NG burns with a yellow flame then it worked, anyone know what coloured flame NG burns with?



simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 04-27-2001 04:57 AM

Yesterday I made some very high nitrated nitrocellulose. I used about 80-90% nitric acid made with lead nitrate and 98%sulphuric acid. This recipe for nitrocellulose is the best I've used since I haven't access to 90% pure nitric acid! (I posted the recipe before 1-2 months). The nitric acid is mixed 1:1 with sulphuric acid (in volume) and then the cotton is put (temperature in first 7 minutes about 8 degress in the next 7 minutes 15 degrees. The nitrocellulose burns really fast with no ash. I will convert this nitrocellulose to acetone peroxide putty.
As I have read the nitroglycerine burns with blue flame, actually i've never made it...



ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 04-27-2001 11:20 AM

Anthony: Well nitrated NC burns with a green-blue flame. Although your product must be slightly nitrated. None of the chems needed in NC are flammible. Except for glycerine, which is not that flammible anyways. If you can place a match on it and it light its nitrated something. Just soak i tiny piece of paper in NG and hit it wil a hammer.
------------------
technology is a wonderful servant, but a bitch of a master.

Explosives Archive



frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-27-2001 02:58 PM

nitroglycerine burn test? =green-blue flame means right product ?!?!??!
how did you lit it and see the burning flame?
I thought NG is heat sensitive as well as shock???


Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 04-27-2001 03:34 PM

I messed up last time and only had a few bubbles of "nitro" I sucked some of them out of the water with a pipette and squirting onto a hotplate. There was water in pipette with the NG but it still went pop with a flash of organge flame. I've made another batch now and I appear to have a nice thick layer of NG settling out.
The NC with KNO3 is only slightly nitrated. Methinks it's time to sort out some HNO3...