megalomania
June 8th, 2003, 12:43 PM
ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 02-01-2001 03:33 AM
--------------------------------------------------------------------------------
Well, today, i tried making some nitrocellulose. he nitration ran away and scared the shit outa me. Im using about 98% h2s04, kno3, and i never got to puttin the cotton in. I added the appropriate amout of acid to the kno3 and it suddenly got warm, even in a ice bath.I took the vessel outa the ice bath to feel the outside of the container to see how hot it was..the thermometer was throught the roof. While the vessel was in my hand, its started bubbling, then flames and crackilng started to appear. then, dense red-brown Nitrogen dioxide gas started pouring out, shit i said! I threw the vessel in my harbage can and got the hell outa dodge. I dont know why i didnt dump the continer in the bath. I hope i wake up tommorow, i inhaled tons of vapourized etheyeyne glycon, and a tiny bit of nitrogen dioxide. well cya. Hey, will you guys goto my funeral? BTW, i wanna be blown up instaed of creamated (holy cow SP?)
------------------
Explosives Archive
blackadder
Frequent Poster
Posts: 313
From: London
Registered: DEC 2000
posted 02-01-2001 06:16 AM
--------------------------------------------------------------------------------
Everyone has a little accident now and then.
Megalomania was making some NG and he put the glycerin in too fast, and the infamous Nitrogen Dioxide came.
A couple days ago I spilt half a bottle of NaOH all over my face and T-shirt. It wasn't concentrated, but still, I could have done without corrosive stuff all over my face.
I'll come to your funeral
------------------
"I'm not a slave, to a world, that doesn't give a shit!" -Marilyn Manson
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-01-2001 06:17 AM
--------------------------------------------------------------------------------
You added the acid to the KNO3 ????
ALL at once ??? If yes, it was no good idea!
Better ad the KNO3 to the acid in small portions and allow to cool between the additions.
------------------
for best catfood visit:
catfood.tsx.org
Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 02-01-2001 06:40 AM
--------------------------------------------------------------------------------
Well let's try and clear things up a bit...
First of all; what were you trying to make?
If it was nitrocellulose as you say, what were you doing with ethylene glycol?
Secondly, how much were you using? You shouldn't use more than, say, 6 mL SA, 4 grams AN and 1 mL ethylene glycol the first time. Not only because of safety considerations, but you'll avoid wasting a lot of chemicals while you get a feel for the procedure.
PS. I don't think you should be too worried about ethylene glycol fumes; I don't think it would be sold as anti-freeze if it was really deadly to breathe them. Don't drink it though.
Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 02-01-2001 10:15 AM
--------------------------------------------------------------------------------
Is it just me that's never got brown nitrogen dioxide? Mine's always been white wispy stuff still very choking though, maybe it just goes brown when hot?
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-01-2001 11:12 AM
--------------------------------------------------------------------------------
I think the nitrogen dioxide is only formed in considerable amounts if the nitrate was added too fast and/or the temperature is too high. When i dream of making picric acid with the H2SO4/KNO3 method i have no NO2 fumes, too. (only the first time i dreamt of it)
------------------
for best catfood visit:
catfood.tsx.org
ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 02-01-2001 03:11 PM
--------------------------------------------------------------------------------
i was making nitrocellulose..and i was aking egdn earlier..2 expermerments gone bad. Ithink ikk stick to ap until i getsome more pure kno3 And AN
------------------
Explosives Archive
[This message has been edited by ALENGOSVIG1 (edited February 01, 2001).]
no_name_available
New Member
Posts: 25
From: germany (?)
Registered: JAN 2001
posted 02-01-2001 04:04 PM
--------------------------------------------------------------------------------
hey, just think about making brown nitrogen dioxide intentional !
i think u could also make it by heating nitrats of heavy metals.
btw. - what happen if i heat NH4NO3 ? it decomposes to what ?
if u dont know what to do with all that NO2 - try to lead it in normal salpeter-acid to make it red & fuming !
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 02-02-2001 08:52 AM
--------------------------------------------------------------------------------
NH4NO3--->2H2O + N2O
N2O--->N2 + 1/2O
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 02-03-2001 12:08 PM
--------------------------------------------------------------------------------
AN heated at low temps. produces water and laughing gas. Heat it too strongly and it can decompose violently/detonate. Heating nitrates such as Pb(NO3)2 produces NO2 and the metal oxide.
Cool your H2SO4 to about 0*C or colder, and add the KNO3 a little bit at a time.
Anthony: What you have sounds like HNO3 vapours, not NO2. I have a bottle of 70% HNO3. It's completely colourless, and makes white fumes of HNO3 in moist air (4NO2 + O2 + 2H2O --> 4HNO3). In completely dry air, it makes a slightly brown mist.
SofaKing
Frequent Poster
Posts: 399
From: YEAH RIGHT !!
Registered: SEP 2000
posted 02-04-2001 12:09 PM
--------------------------------------------------------------------------------
Hey PHILOU wouldn't that be 1/2O2 instead of 1/2O. As I recall oxygen is diatomic so you don't write it as just O or O1, but instead 1/2O2. Also 1/2O doesn't make much sense. I know this is a minor thing but it's not often I notice mistakes, esspecially from you
[This message has been edited by SofaKing (edited February 04, 2001).]
megalomania
Administrator
Posts: 751
From: USA
Registered: SEP 2000
posted 02-06-2001 08:48 AM
--------------------------------------------------------------------------------
You can try to concentrate nitric acid by decomposing a batch. If you add copper metal to dilute nitric acid you will get NO, which combines with air to form NO2. If you add copper to conc nitric acid you get NO2 fumes. These fumes could be channeled into another batch of nitric to concentrate it, but this would be kinda wasteful, what with copper nitrate formation and all.
------------------
For the most comprehensive and informative web site on explosives and related topics, go to Megalomania's Explosives and Stuff at http://surf.to/megalomania
Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-01-2001 04:01 PM
--------------------------------------------------------------------------------
SHIT ! My goose was nearly cooked just now.
I tried to make RDX using 50cc 70% nitric acid and 200cc of sulphuric acid. I let it cool down and put the mix in an ice bath. I put the hexamine in slowly, but then I accidently screwed up and dropped a load in.
Along came the brown fumes accompanied by a sort of a 'mini-detonation' similar to what happens when you set light a small amount of unconfined AP.
It's a good job I was wearing 'the suit' when this happened- it could have been nasty had the lot gone off.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-03-2001 08:54 AM
--------------------------------------------------------------------------------
Yes it was 1/2O2!
N2O--> N2 + 1/2O2 (sometimes I forget to take may finger off that shift button and then numbers becomes arrows....happens sometimes when I type fast and when I'm tired).
Hey bitter! When will you learn to follow recipes!!!! Never add H2SO4 in a RDX process!
RDX is unstable/decompose in conc H2SO4 medium so does most nitramines.Yield 0% and useless risks of explosions!!!!!
Read twice before acting or learn to read!
It is hexamine + conc HNO3 ALONE!
Other processes uses H2SO4 conc but via methylenesulfamate of K!!!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-03-2001 09:39 AM
--------------------------------------------------------------------------------
Sorry, Philou, but it was only an experiment...which, as you say didn't work. Plus, there is so much bullshit posted about this subject that it's hard to differentiate the right from the wrong anymore. Speaking of which, it's about time we all tried to make a definitive info collection on this subject rather than the 'mixture' we have at present.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-04-2001 07:19 AM
--------------------------------------------------------------------------------
OK but be careful next time and use less quantity as a first shot! Never use more than what is necessary to generate 2g-just to see how it behaves...! I suspect you have tried to make like 30g of RDX...right?Even if it goes wel for 2g then scale up slowly!
Usually, scientist make a thermic study on 5g reactant mix by putting it in an uncooled insulated reactor (frigolite is OK); just to let you see what can happen on runaway or when scaling up (since then heat dissipates much slower; that equals to an insulation towards cooling!).
Usually recipes on Mega's site are OK; also it is a good idea to ask here before acting on something new..it can spare your time, money, lungs, eyes, hands, life!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-04-2001 11:31 AM
--------------------------------------------------------------------------------
Don't worry, all of the stuff was 'free' and I was heavily protected.
Come to think of it, I don't think it was actually the nitration process that caused that 'pop' at all...probably a slight crust of KClO3 residue that I hadn't managed to clean off the bottom of the fume cupboard. It was probably the sulphuric acid that did it. I just noticed a bit after cleaning up yesterday's mess.
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 02-01-2001 03:33 AM
--------------------------------------------------------------------------------
Well, today, i tried making some nitrocellulose. he nitration ran away and scared the shit outa me. Im using about 98% h2s04, kno3, and i never got to puttin the cotton in. I added the appropriate amout of acid to the kno3 and it suddenly got warm, even in a ice bath.I took the vessel outa the ice bath to feel the outside of the container to see how hot it was..the thermometer was throught the roof. While the vessel was in my hand, its started bubbling, then flames and crackilng started to appear. then, dense red-brown Nitrogen dioxide gas started pouring out, shit i said! I threw the vessel in my harbage can and got the hell outa dodge. I dont know why i didnt dump the continer in the bath. I hope i wake up tommorow, i inhaled tons of vapourized etheyeyne glycon, and a tiny bit of nitrogen dioxide. well cya. Hey, will you guys goto my funeral? BTW, i wanna be blown up instaed of creamated (holy cow SP?)
------------------
Explosives Archive
blackadder
Frequent Poster
Posts: 313
From: London
Registered: DEC 2000
posted 02-01-2001 06:16 AM
--------------------------------------------------------------------------------
Everyone has a little accident now and then.
Megalomania was making some NG and he put the glycerin in too fast, and the infamous Nitrogen Dioxide came.
A couple days ago I spilt half a bottle of NaOH all over my face and T-shirt. It wasn't concentrated, but still, I could have done without corrosive stuff all over my face.
I'll come to your funeral
------------------
"I'm not a slave, to a world, that doesn't give a shit!" -Marilyn Manson
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-01-2001 06:17 AM
--------------------------------------------------------------------------------
You added the acid to the KNO3 ????
ALL at once ??? If yes, it was no good idea!
Better ad the KNO3 to the acid in small portions and allow to cool between the additions.
------------------
for best catfood visit:
catfood.tsx.org
Microtek
Frequent Poster
Posts: 205
From:
Registered: JAN 2001
posted 02-01-2001 06:40 AM
--------------------------------------------------------------------------------
Well let's try and clear things up a bit...
First of all; what were you trying to make?
If it was nitrocellulose as you say, what were you doing with ethylene glycol?
Secondly, how much were you using? You shouldn't use more than, say, 6 mL SA, 4 grams AN and 1 mL ethylene glycol the first time. Not only because of safety considerations, but you'll avoid wasting a lot of chemicals while you get a feel for the procedure.
PS. I don't think you should be too worried about ethylene glycol fumes; I don't think it would be sold as anti-freeze if it was really deadly to breathe them. Don't drink it though.
Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 02-01-2001 10:15 AM
--------------------------------------------------------------------------------
Is it just me that's never got brown nitrogen dioxide? Mine's always been white wispy stuff still very choking though, maybe it just goes brown when hot?
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 02-01-2001 11:12 AM
--------------------------------------------------------------------------------
I think the nitrogen dioxide is only formed in considerable amounts if the nitrate was added too fast and/or the temperature is too high. When i dream of making picric acid with the H2SO4/KNO3 method i have no NO2 fumes, too. (only the first time i dreamt of it)
------------------
for best catfood visit:
catfood.tsx.org
ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 02-01-2001 03:11 PM
--------------------------------------------------------------------------------
i was making nitrocellulose..and i was aking egdn earlier..2 expermerments gone bad. Ithink ikk stick to ap until i getsome more pure kno3 And AN
------------------
Explosives Archive
[This message has been edited by ALENGOSVIG1 (edited February 01, 2001).]
no_name_available
New Member
Posts: 25
From: germany (?)
Registered: JAN 2001
posted 02-01-2001 04:04 PM
--------------------------------------------------------------------------------
hey, just think about making brown nitrogen dioxide intentional !
i think u could also make it by heating nitrats of heavy metals.
btw. - what happen if i heat NH4NO3 ? it decomposes to what ?
if u dont know what to do with all that NO2 - try to lead it in normal salpeter-acid to make it red & fuming !
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 02-02-2001 08:52 AM
--------------------------------------------------------------------------------
NH4NO3--->2H2O + N2O
N2O--->N2 + 1/2O
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 02-03-2001 12:08 PM
--------------------------------------------------------------------------------
AN heated at low temps. produces water and laughing gas. Heat it too strongly and it can decompose violently/detonate. Heating nitrates such as Pb(NO3)2 produces NO2 and the metal oxide.
Cool your H2SO4 to about 0*C or colder, and add the KNO3 a little bit at a time.
Anthony: What you have sounds like HNO3 vapours, not NO2. I have a bottle of 70% HNO3. It's completely colourless, and makes white fumes of HNO3 in moist air (4NO2 + O2 + 2H2O --> 4HNO3). In completely dry air, it makes a slightly brown mist.
SofaKing
Frequent Poster
Posts: 399
From: YEAH RIGHT !!
Registered: SEP 2000
posted 02-04-2001 12:09 PM
--------------------------------------------------------------------------------
Hey PHILOU wouldn't that be 1/2O2 instead of 1/2O. As I recall oxygen is diatomic so you don't write it as just O or O1, but instead 1/2O2. Also 1/2O doesn't make much sense. I know this is a minor thing but it's not often I notice mistakes, esspecially from you
[This message has been edited by SofaKing (edited February 04, 2001).]
megalomania
Administrator
Posts: 751
From: USA
Registered: SEP 2000
posted 02-06-2001 08:48 AM
--------------------------------------------------------------------------------
You can try to concentrate nitric acid by decomposing a batch. If you add copper metal to dilute nitric acid you will get NO, which combines with air to form NO2. If you add copper to conc nitric acid you get NO2 fumes. These fumes could be channeled into another batch of nitric to concentrate it, but this would be kinda wasteful, what with copper nitrate formation and all.
------------------
For the most comprehensive and informative web site on explosives and related topics, go to Megalomania's Explosives and Stuff at http://surf.to/megalomania
Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-01-2001 04:01 PM
--------------------------------------------------------------------------------
SHIT ! My goose was nearly cooked just now.
I tried to make RDX using 50cc 70% nitric acid and 200cc of sulphuric acid. I let it cool down and put the mix in an ice bath. I put the hexamine in slowly, but then I accidently screwed up and dropped a load in.
Along came the brown fumes accompanied by a sort of a 'mini-detonation' similar to what happens when you set light a small amount of unconfined AP.
It's a good job I was wearing 'the suit' when this happened- it could have been nasty had the lot gone off.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-03-2001 08:54 AM
--------------------------------------------------------------------------------
Yes it was 1/2O2!
N2O--> N2 + 1/2O2 (sometimes I forget to take may finger off that shift button and then numbers becomes arrows....happens sometimes when I type fast and when I'm tired).
Hey bitter! When will you learn to follow recipes!!!! Never add H2SO4 in a RDX process!
RDX is unstable/decompose in conc H2SO4 medium so does most nitramines.Yield 0% and useless risks of explosions!!!!!
Read twice before acting or learn to read!
It is hexamine + conc HNO3 ALONE!
Other processes uses H2SO4 conc but via methylenesulfamate of K!!!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-03-2001 09:39 AM
--------------------------------------------------------------------------------
Sorry, Philou, but it was only an experiment...which, as you say didn't work. Plus, there is so much bullshit posted about this subject that it's hard to differentiate the right from the wrong anymore. Speaking of which, it's about time we all tried to make a definitive info collection on this subject rather than the 'mixture' we have at present.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-04-2001 07:19 AM
--------------------------------------------------------------------------------
OK but be careful next time and use less quantity as a first shot! Never use more than what is necessary to generate 2g-just to see how it behaves...! I suspect you have tried to make like 30g of RDX...right?Even if it goes wel for 2g then scale up slowly!
Usually, scientist make a thermic study on 5g reactant mix by putting it in an uncooled insulated reactor (frigolite is OK); just to let you see what can happen on runaway or when scaling up (since then heat dissipates much slower; that equals to an insulation towards cooling!).
Usually recipes on Mega's site are OK; also it is a good idea to ask here before acting on something new..it can spare your time, money, lungs, eyes, hands, life!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Bitter
Frequent Poster
Posts: 290
From: 11 Downing Street, London, England
Registered: SEP 2000
posted 05-04-2001 11:31 AM
--------------------------------------------------------------------------------
Don't worry, all of the stuff was 'free' and I was heavily protected.
Come to think of it, I don't think it was actually the nitration process that caused that 'pop' at all...probably a slight crust of KClO3 residue that I hadn't managed to clean off the bottom of the fume cupboard. It was probably the sulphuric acid that did it. I just noticed a bit after cleaning up yesterday's mess.