Nitrocellulose? Something wrong.

[nuclearattack]

hi!
this days i tried making some nitrocellulose, i searched for nitrocellulose synthesis in the forum and also in powerlabs.org, after that i decided to use this ratios:

25g H2SO4 98% (boiled until white fumes appear from 38% H2SO4)

10g ammonium nitrate

1g cellulose (pure cotton for first aid)

i have mixed h2so4 with AN until all AN was dissolved and than i putted the cellulose in it.
after that i putted the beaker in a hot bath at 45 C° for 1 hour.

i have neutralized the nitrocellulose in the water with sodium bicarbonate and i have let it dry.
with few words i followed all the standard procedure to make NC but it seems that something went wrong!
the NC doesn't burns fast (deflagrate) it burns as the pure cotton does. i tried to burn it on open flame and it is a bullshit. what's the matter? i tried to remake it after that but it doesn't works!
reading others posts about nitrocellulose synthesis seems a simple and working procedure to make NC (i don't know another metod except for the one using H2NO3 instead of the AN) but i think that it is more difficult.
Has anyone encountered those kind of problems?
How have you resolved those problems?

i'm very interested about NC because i want to make some dynamite and plastic explosives with it.

thanks to all of you for replies!

[kingspaz]

i had similar problems untill i used drain opener H2SO4 so i concluded the problem to be with the H2SO4 not being of sufficiently high concentration since i also used to attempt it using boiled down H2SO4. try boiling the H2SO4 down even more or go to a plumbing type shop and get some 'acid based drain opener'.

[Dave Angel]

I've made NC once using drain opener H2SO4 and KNO3. Mine also burnt fairly pathetically, which I put down to under nitration or lack of purification, (I used sodium carbonate to neutralize acid remaining after washing, perhaps some remained).

I'm going to try again soon, I'm thinking that possibly using harsher conditions, a 2 step nitration and a more thorough purification should do the job.

[nuclearattack]

so the matter can be the insufficent acid conc, but how much have i to boil it?
in a post i read that when white fumes appear (not water vapor but dense fumes) is better to continue to heat the acid for 15 minutes to be sure to reach the max conc. i made it and the result was a dense trasparent acid slightly stinky. i think this is a good conc, however i noticed that during the acid heating the acid doesn't boil like water it is quite, without bubbles.
another thing: after the nitration process i tried to dissolve the NC in the acetone...something happen because when the acetone has gone the NC is in a different state, more dense and white colored. it doesn't burn quickly but i think this means a partial nitration. isn't it?

what is the right look of the 98% h2so4? is like my boiled h2so4?

[Mr Cool]

Wash the cotton first with dilute NaOH, or some strong detergent or something.
Then rinse it WELL, many times, with DISTILLED water.
Then dry it in an oven at 100*C or slightly more, to make it ANHYDROUS.
Don't trust the "white fumes" thing when concentrating H2SO4. If the room-temperature acid doesn't turn cotton black in a few seconds, it's not strong enough.
Neutralise the NC well, wash it many times, give it a good rinse with hot urea solution (read COPAE. Urea is good...), then rinse with more distilled water.
Dry it WELL - even when it feels dry, it can still have a good % of moisture in it.

Assuming you follow those, and you have a good ratio of reagents, you can't go wrong. Also, do make sure that your cotton specifically says that it is 100% cotton...

[tom haggen]

I found that using density tables to check the concentration of my boiled down H2SO4 works quite well. I like to concentrate my own that way you know there are no impurities. Although I haven't purified H2SO4 as of yet. I just start off with clear and clean dilute H2SO4. I've herd that drain opener crap is contaminated. Further more NC that I've bought at the store doesn't seem to have that fast of a burn rate.

[kingspaz]

NC bought at the store has been processed and made into a more dense mass (can't remember the word for this, like when you have NC/acetone and you leave the acetone to evapourate, the plastic mass of NC). the strore bought stuff thus has a low surface area:mass ratio so burns slow as not much is exposed. fibrous NC has many air pockets, hollow fibres, etc meaning a large surface area is exposed to the flame front, so it burns like a bitch.

[Bert]

NC that I've bought at the store doesn't seem to have that fast of a burn rate.
Where can you buy solid NC over the counter, except as flash paper in a magic shop or finished smokeless powder for reloading? I've bought raw, unprocessed bulk NC, but I needed an ATFE license to do so.

[kingspaz]

i think he means smokeless powder...

[SpiffyVision]

After the NC is made, does the nitrating mixture have any use? I want to use this method: http://www.angelfire.com/empire/megapyro6/Pyro/NC.html

[tom haggen]

Yes I did mean smokeless powder. Well you learn something new everday. I was unaware that homemade NC had such a fast burn rate.

[Dead mAn Walkin]

Can you use HCI in the sunthesis of NC? HCI can't be too concentrated as pure HCI is a gas. If you can use it, what would the method be?

[Blackhawk]

I'm going to say "no, you idiot" here because HCl will never be concentrated enough for the procedure. The purpose of the H2SO4 and xNO3 is to produce HNO3, nitirc acid, with which to nitrate of all things. Now the H from HCl would work (I think, correct me if there is some reason it wouldn't) except for the fact that as it is actually a gas disolved in water, as you yourself said you will never get it much more conc than ~35%. Dosn't the fact that the synth at the top of the page ask for 98% H2SO4 (boiled up from 38%) give you any hints as to why HCl won't work? why would you think that HCl would work at 35% while H2SO4 would only work at 98%? HCl hasn't got any magical properties of intense acidification.

[T_Pyro]

I don't get it. Why is it that people get the idea that just because HCl is "yet another strong acid", it can be used for nitration? 98% H2SO4 is required for the formation of the nitronium ion, which is essential for nitration. A lot has already been said on the topic. Dead mAn Walkin, search before you post.

[nuclearattack]

Mr.Cool

you said that if the cotton doesn't turn black in few seconds it means that h2so4 is not enought concentrated. In another procedure i read that the finally NC is white/yellow...so what is the right colour? white or black?
another question: what is the right look of 98% h2so4? i tried concentrating it to the limit but it seems to be only more dense, the colour is the same except it is slightly yellow.

[Anthony]

The H2SO4 is also required to soak up water formed during the nitration. Without a dehydrating agent, the concentration of acid would drop too low, and the nitration would stop.

[SpiffyVision]

OK, I just made some NC... I mixed 7.2 grams of KNO3 with the 12 mL of sulfuric acid, which gave me a really thick slury. When I added the cotton, I had to work it in really hard, I couldnt manage to even put half a gram of cellulose. It ended up looking like a small mass as it was nitrating, now Ive cleansed the cotton and it has a reddish yellowish hue out to it. Its had about 10 and a half hours to dry, some of it still has some moisture in it. I tried burning a very small sample that seemed to be dry and it burned with an orange flame, no poof though like ive seen on the videos...

[Dave Angel]

nuclearattack, I think what Mr. Cool meant was that to test if the sulphuric acid is concentrated enough, you see if it will turn cotton black quickly. When doing the actual nitration you wouldn't want this to happen so you add the cotton to the mixed acids / acid and nitrate, not cotton to sulphuric acid and then the nitric / nitrate.

My concentrated sulphuric acid from drain cleaner is a dense yellowish liquid once I've boiled it good. I think I've seen lab sulphuric acid that has this appearance too so it sounds about right.

[Mumble]

Mine always burnt with sort of a flare before it was dry. Once dry I get a nice poof though. Yours should poof once its completely dry. Just because a portion seems dry doesn't mean it is. I'd say give it a good 24 to 48 hours. Thats about how long mine took. I also dried it under a lamp for some extra heat. When I was doing it I just kept adding the cotton. It doesn't look like it will fit, but if you keep adding it, it will soak up the acid and proceed to work.

[SpiffyVision]

Will a common resperator (the paper filters with the elastic bands that go around your head) work to block the nitric acid gas thats created? That stuff makes you cough like no other, I would have added more cotton if I had one, its just that the gas got annoying.

[Dave Angel]

I don't think that type of respirator will be effective. I'd definitely consider buying a half face respirator with organic vapor filters as I've found these can block NOx to some extent despite not being specifically designed to do so.

[vulture]

Use ABE filters, they keep out NOx. Organic filters only keep out organics with a boiling point higher than 65C.

[Dave Angel]

Hmmm... makes me wonder what my filters must be then... I know they block high ammonia concentrations so that gives them K as well as A rating, and this was the only type of filter available (apart from the dust filter) at the DIY store.

vulture: Do you get your ABE filters from lab supply or is there a more widely available source?

[kingspaz]

i use a military gasmask. the filter contains many porous layes of activated charcoal. its clearly visible in the filter opening when unscrewed from the mask. i don't know about other filters though.....

[vulture]

I get them from the hardware store. They're not cheap though, €18 for 2 filters and my face mask uses 2 at a time.

[Dave Angel]

Yes the replacement cartridges from the B&Q hardware store in the UK are about £13 for 2. Maybe one could just refill them with activated charcoal from the pet shop (for fish tanks), though I wouldn't stake my life on them!

As a side note, if you don't have the luxury of a gas mask or full face respirator then swimming goggles are handy when working with formaldehyde and ammonia.

[Edit] spelling....

[kingspaz]

gasmasks can be had from military surplus shops for less than £30. then £5 for an out of date filter and you're sorted.

[Dave Angel]

ah thanks kingspaz, I'll have find one and pay them a visit sometime. I'll have a look out for some other goodies whilst I'm there too, surplus trioxane or hexamine fuel tabs maybe...

[vulture]

Activated charcoal might stop V and G agents, but it doesn't stop small inorganics like HCN, NOx and other nasties.

[SpiffyVision]

Between these two, which one if any would be the best?

http://store.yahoo.com/cdnn/m1gasmaswfil.html

http://store.yahoo.com/a2zoutlet/newgasmawine.html

[blindreeper]

http://store.yahoo.com/a2zoutlet/newgasmawine.html I'd go with that one, protects against -Hydro cyanic acid, cyanogens chloride, arsine, phosgene, chloropicrin, bromomethane, lewisite gas, mustard gas, sarin, vx gas, toxic smoke, The plague, cholera, anthrax, radioactive dust.

Thats just my personal opinion.

[Sparky]

Blindreeper: :eek:

"MASK01 Retail: $169.00 Discount price: $19.95"

If I lived in the US one of those would be probably on it's way here right now.

[SpiffyVision]

It doesnt block cabon monoxide, does that say anything about it that I should know before buying it? Other then it doesnt block carbon monoxide? Maybe because it doesnt block it, the mask doesnt block other things?

[Bert]

Nothing (that I know of) will deal with CO except a self contained air supply. It can't be filtered out by activated charcoal.

Edited to reflect the fact I don't know everything...Here's a mask that WILL convert CO (http://www.safetyinfo.com/safetyinfo/html/equipment/disaster/disaster-smokemask.htm)

[nbk2000]

There are filters that catalytically oxidize CO into CO2, which is then absorbed by soda-lime. I believe these type of filters are available as mine rescue equipment.

Surplus gas masks are asking for death.

Remember the saying "You get what you pay for?". It especially applies to life and safety equipment. Spend $200 on a brand new mask and filters from someone like MSA, rather than $10 at the local surplus store. You only have to take one breath to find out that your mask doesn't stop (Insert one-breath lethal chemical here) before you die.

[SpiffyVision]

Surplus gas masks are asking for death if your handling CO? Really all I plan on handling is the NC. Maybe more things once I actually get some beakers and a distiller...

[vulture]

You're making NC so you're handling NOx fumes, which are just as lethal as CO, only the symptoms will show with severe delay. So it's not because you're not noticing a headache that you're not being intoxicated. I wouldn't use surplus filters for NOx and other small molecules (ie SO2, HCN) since they're not being stopped by activated charcoal IIRC.

[Anthony]

I see a surplus mask as being a comfort thing, rather than required protection. I.e. if working with war gases, a mask you can be certain of would be essential. Working with HNO3 vapour, NOx, NH4 is something else. I'd class these things as unpleasant, but not immediately threatening. Many people handle exposure to them without any protection, using basic ventilation, staying upwind, controlled breathing (i.e. turning away from the bench to inhale) etc. So if a cheap mask fails you, you're only back to where you would have been.

In other words:

"Low" risk - cheap/uncertain mask possible
High risk - no fucking about

[vulture]

Anthony, I wouldn't classify NOx as low risks. They're vicious inhalation poisons in low concentrations.

[kingspaz]

vulture, maybe my gasmask filters have something else in them also. NOx doesn't pass through, NH3 doesn't, can't remember anything else inorganic right now that i've worked with using it...HNO3 doesn't either.

[SpiffyVision]

What kind of gas mask do you have, spaz?

[Anthony]

I thought my inplying that NOx was low risk might cause a response.

I agree that it's nasty stuff, and I wouldn't want to be trapped in a room full of it. Although, it isn't like HCN where a half lungfull may well cause death. In the quantities encountered by most pyros (a few hundred grams of mixed H2SO4 and KNO3), I personally wouldn't classify it as high-risk.

Perhaps I'm biased towards my own experiences - I avoided it without many Personal Protective Equipment, and suffered no effects besides the acrid smell.

[kingspaz]

spiff, i have a UK army issue S10. check out some surplus shops. the prices of gasmasks should have dropped down a fair bit by now after they were stupidly high after 11/9 (thats dd/mm ;)).

[tom haggen]

man I want to get an israeli made gas mask so bad! they are 29.90 us$. They are effective againts NBC agents. The Israeli government issues them to there citizens for free. We americans have to pay for them. Kind of Ironic our government is being jewish with the israeli made gas masks. The best respirators sold around here at the hard ware store are 50 bucks and they are effective against SOx I don't think they are effective againts Nitrogen dioxide and I wouldn't want to find out. They sell Israeli made gas masks around here somewhere but I have yet to find them besides the internet. They are by far a superior gas mask

[nuclearattack]

To Mr.Cool:

Thanks for your help, i followed your procedure about nitrocellulose synthesis and it worked very well! The problem was the H2SO4 concentration, now i'm able to make a good final product.
Well, now it's time to think about nitroglycerine and then...dynamite!
Thanks a lot Mr Cool!
I saw your site...very good, i like your photos and the way you made the site!