megalomania
June 21st, 2003, 11:24 AM
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 05:57 AM
--------------------------------------------------------------------------------
this morning, I tried to make RDX by the following method :
Add 35 g of hexamine in 60 mL of red fuming nitric acid ...
I added about 10 g of hexamine when this fucking factor disturd me to sign a package.
this takes me about 2 - 3 min. When I came back, the acid in the beaker was fuming enormously and the temperature was between 50-60°C. I immediately dump the solution in the ice bath but I CANNOT UNDERSTAND WHAT WAS HAPPENED ???!!!
Anyone here can explain to me this strange phenomenon ?
a big thanx...
Tony Montana
Frequent Poster
Posts: 145
From: Australia
Registered: JUN 2001
posted 06-26-2001 06:38 AM
--------------------------------------------------------------------------------
This strange phenomenon be nitration.
When nitration occurs, so does heat. Did you cool the HNO3 to 20 degrees celsius before adding C6H12N4?
Did you very very very slowly add C6H12N4 to HNO3? The temperature is going to rise from reaction, but if it approaches 30 degrees celcuis stop adding C6H12N4 and allow HNO3 to cool to 20 degrees celcius again! After the last of the C6H12N4 has been added continue to stir for 5 minutes watching the temp.
OH YEAH its all got to be done in an ice bath!!!!!!!
As your nitrating something.
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 08:35 AM
--------------------------------------------------------------------------------
thanx
but I have an another question,
in formula i got, the guy says after adding all the hexamine you must heat the solution to 50-60°C during 10 min, is it right ?
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-26-2001 10:04 AM
--------------------------------------------------------------------------------
Not in that process! Runaway can occur and it is what you had!
You also use red nitric...better use white one for that process especially if not cooled as it should.
In the process with NH4NO3 you can heat to 50-60C!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 11:47 AM
--------------------------------------------------------------------------------
thanx again but even on the Megalomania's site, he heats the solution to 50-55°C, why ?
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-26-2001 12:44 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-26-2001 12:48 PM
--------------------------------------------------------------------------------
Are you talking about AN, Ac2O, and (-CH2O-)n, or AN, HNO3 and Hexamine when you talk about the method with ammonium nitrate?
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-26-2001 02:39 PM
--------------------------------------------------------------------------------
I was referring to the process using ammonium nitrate, hexamine and nitric acid.
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 03:38 PM
--------------------------------------------------------------------------------
I produce my own nitric acid by distilling sodium nitrate and sulfuric acid (95%) witout vacuum.
is it concentrated enough ?
thanx
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-26-2001 03:47 PM
--------------------------------------------------------------------------------
Probably not. Do you have a scale to measure the density? Distilling without vacuum means higher temps, which causes some of the nitric acid to break down after formation, the result is NOx and water. The water goes into your receiving flask and lowers the concentration of nitric acid. You can try redistilling this acid with sulfuric acid to remove the water.
a_bab
Frequent Poster
Posts: 55
From: doesn't matter
Registered: MAY 2001
posted 06-26-2001 04:51 PM
--------------------------------------------------------------------------------
The SH-Salz method (hexamine and conc. nitric acid) consist in two phases; the first phase with "dinitrohexamine" formation is when you add hexamine to cooled nitric acid. "Dinitrohexamine" is soluble in nitric acid (and in water). So if you dump this mix in water you'll gonna lose lots of nitric acid and obtain no RDX at all. The drawback of this method is that it needs lots of strong nitric acid (for 10 g of RDX at least 100-150 ml). Most of the cookbookz (including ALL the recipes from the fuckin' site 'tootsie') doesn't even mention about heating the acid/hexamine mix. It must be heated to 55 degrees Celcius for 10 minutes, sometimes for hours, depending of the nitric acid concentration. If you heat the mix to a bigger temp, the RDX yeld will be low. If you don't heat the mix, the RDX will be present only in traces .
(CH2)6N4 + 4HNO3 -> C3H6O6N6 + 3CH2O + NH4NO3
I tryed Sunday to make some RDX with E method using formaline solution instead of parafolmaldehide. Still no result
________________________
http://move.to/pyromania
Jumala
Frequent Poster
Posts: 202
From: Germany
Registered: OCT 2000
posted 06-26-2001 08:59 PM
--------------------------------------------------------------------------------
Here is a good desciption for making RDX
http://huizen.dds.nl/~arcticus/synthesis.htm
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-27-2001 03:18 AM
--------------------------------------------------------------------------------
I only have a 0.1 g precision scale...
70 mL of my nitric acid weigh 250.8 g
is it concentrated enough ?
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 04:44 AM
--------------------------------------------------------------------------------
Impossible! There is a mistake here. 250g for 70ml means a density of 3.57g/ccm...Are you living on Jupiter to reach such a high density for nitric acid what can only reach approx 1.65 g/ccm? Even conc sulfuric doesn't reach such a density.
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 04:46 AM
--------------------------------------------------------------------------------
I guess you have forgotten to set the scale to zero with the container on it before incorporating your 70ml of NA.
I think also that the container weight approx 150g...right?
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-27-2001 04:53 AM
--------------------------------------------------------------------------------
really sorry...
the acid weigh 113.3 g
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 05:43 AM
--------------------------------------------------------------------------------
Then it is 113.3g for 70ml this means 113.3/70 = 1.617-1.620g/ccm (considering the error that might come from your scale to be +/- 0.1g and that the Volume is near 100% correct thus 70.00 ml.
I think your acid is thus near 97.5-98%...quite good.
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
goiterjoe
New Member
Posts: 10
From:
Registered: JUN 2001
posted 06-29-2001 01:02 PM
--------------------------------------------------------------------------------
cooking up shit when the Fed-Ex guy shows up is a really easy way to get caught for shit. and be careful ordering hexamine, as it is heavily watched due to it's use in making methylamine. the DEA is all over this one, and if they see it ordered in conjunction with substances such as aluminum powder or mercury salts or borohydrides, it might be your ass.
goiterjoe
New Member
Posts: 10
From:
Registered: JUN 2001
posted 06-29-2001 01:07 PM
--------------------------------------------------------------------------------
guess I should mention that methylamine, sodium borohydride, aluminum, etc. are used to manufacture methamphetamine and exstacy.
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-29-2001 04:00 PM
--------------------------------------------------------------------------------
YEAAAAAAAH !
this morning, I succeeded to make RDX ! but now I know how to make it, i got some new questions, here they are :
- The nitric acid became greenish after the addition of the hexamine, at this point, I stop adding hexamine, is it the good way or do I need to add more hexamine ?
- After that, I boil the solution to 50-60°C for 10 min, the solution changed color to yellowish but why do I need to boil the solution ?
any replies are more than appreciated
mongo blongo
Frequent Poster
Posts: 175
From: I live in a Creosote Bush!
Registered: JUN 2001
posted 07-04-2001 02:49 PM
--------------------------------------------------------------------------------
To PHILOU Zrealone.]
i know ihis is an old topic but it was the only topic i have seen this being talked about in.
looking at above you somehow calculated the %concentration of hno3 from the density.
i have been having problems doing this!
since i have never worked in percentages when working out concs of soloutions. i am probably approaching this the wrong way. i usually work in moles!
this is what i have come up with so far (to show u i have been trying!):
nitric acid (white) is a mixture of hno3 and h20
The Mr of hno3 = 63
Mr of h2o = 18
what is the molar strength of eg. 98% hno3%?
when i know this:
you need 63g hno3 to make 1dm3 of a 1mol soloution.
so then for 98% soloution u nees 63*(molar strength for 98% hno3)
so weight of hno3 per cm3 is (above)/1000
but u need to take the 2%h20 into concideration.
FUCK THIS!!!!
There must be a better way?
how did u do it?
it's probably something really simple! im a dumass!!
please help!
thanx!!
c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 07-05-2001 01:25 AM
--------------------------------------------------------------------------------
mongo blongo: It could probably be calculated mathematically, but why bother? Every decent Chemistry Handbook has a section on the Densities of Aqueous Solutions, where the specific gravities of most common chemicals in solution are shown, as empirically determined and agreed to by international convention.
In the meantime, bookmark this very useful reference page - it gives EVERYTHING you ever wanted to know about nitric acid:
http://www.efma.org/publications/NitricAcid/Section15.asp
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 05:57 AM
--------------------------------------------------------------------------------
this morning, I tried to make RDX by the following method :
Add 35 g of hexamine in 60 mL of red fuming nitric acid ...
I added about 10 g of hexamine when this fucking factor disturd me to sign a package.
this takes me about 2 - 3 min. When I came back, the acid in the beaker was fuming enormously and the temperature was between 50-60°C. I immediately dump the solution in the ice bath but I CANNOT UNDERSTAND WHAT WAS HAPPENED ???!!!
Anyone here can explain to me this strange phenomenon ?
a big thanx...
Tony Montana
Frequent Poster
Posts: 145
From: Australia
Registered: JUN 2001
posted 06-26-2001 06:38 AM
--------------------------------------------------------------------------------
This strange phenomenon be nitration.
When nitration occurs, so does heat. Did you cool the HNO3 to 20 degrees celsius before adding C6H12N4?
Did you very very very slowly add C6H12N4 to HNO3? The temperature is going to rise from reaction, but if it approaches 30 degrees celcuis stop adding C6H12N4 and allow HNO3 to cool to 20 degrees celcius again! After the last of the C6H12N4 has been added continue to stir for 5 minutes watching the temp.
OH YEAH its all got to be done in an ice bath!!!!!!!
As your nitrating something.
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 08:35 AM
--------------------------------------------------------------------------------
thanx
but I have an another question,
in formula i got, the guy says after adding all the hexamine you must heat the solution to 50-60°C during 10 min, is it right ?
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-26-2001 10:04 AM
--------------------------------------------------------------------------------
Not in that process! Runaway can occur and it is what you had!
You also use red nitric...better use white one for that process especially if not cooled as it should.
In the process with NH4NO3 you can heat to 50-60C!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 11:47 AM
--------------------------------------------------------------------------------
thanx again but even on the Megalomania's site, he heats the solution to 50-55°C, why ?
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-26-2001 12:44 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-26-2001 12:48 PM
--------------------------------------------------------------------------------
Are you talking about AN, Ac2O, and (-CH2O-)n, or AN, HNO3 and Hexamine when you talk about the method with ammonium nitrate?
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-26-2001 02:39 PM
--------------------------------------------------------------------------------
I was referring to the process using ammonium nitrate, hexamine and nitric acid.
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-26-2001 03:38 PM
--------------------------------------------------------------------------------
I produce my own nitric acid by distilling sodium nitrate and sulfuric acid (95%) witout vacuum.
is it concentrated enough ?
thanx
10fingers
Frequent Poster
Posts: 415
From: USA
Registered: SEP 2000
posted 06-26-2001 03:47 PM
--------------------------------------------------------------------------------
Probably not. Do you have a scale to measure the density? Distilling without vacuum means higher temps, which causes some of the nitric acid to break down after formation, the result is NOx and water. The water goes into your receiving flask and lowers the concentration of nitric acid. You can try redistilling this acid with sulfuric acid to remove the water.
a_bab
Frequent Poster
Posts: 55
From: doesn't matter
Registered: MAY 2001
posted 06-26-2001 04:51 PM
--------------------------------------------------------------------------------
The SH-Salz method (hexamine and conc. nitric acid) consist in two phases; the first phase with "dinitrohexamine" formation is when you add hexamine to cooled nitric acid. "Dinitrohexamine" is soluble in nitric acid (and in water). So if you dump this mix in water you'll gonna lose lots of nitric acid and obtain no RDX at all. The drawback of this method is that it needs lots of strong nitric acid (for 10 g of RDX at least 100-150 ml). Most of the cookbookz (including ALL the recipes from the fuckin' site 'tootsie') doesn't even mention about heating the acid/hexamine mix. It must be heated to 55 degrees Celcius for 10 minutes, sometimes for hours, depending of the nitric acid concentration. If you heat the mix to a bigger temp, the RDX yeld will be low. If you don't heat the mix, the RDX will be present only in traces .
(CH2)6N4 + 4HNO3 -> C3H6O6N6 + 3CH2O + NH4NO3
I tryed Sunday to make some RDX with E method using formaline solution instead of parafolmaldehide. Still no result
________________________
http://move.to/pyromania
Jumala
Frequent Poster
Posts: 202
From: Germany
Registered: OCT 2000
posted 06-26-2001 08:59 PM
--------------------------------------------------------------------------------
Here is a good desciption for making RDX
http://huizen.dds.nl/~arcticus/synthesis.htm
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-27-2001 03:18 AM
--------------------------------------------------------------------------------
I only have a 0.1 g precision scale...
70 mL of my nitric acid weigh 250.8 g
is it concentrated enough ?
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 04:44 AM
--------------------------------------------------------------------------------
Impossible! There is a mistake here. 250g for 70ml means a density of 3.57g/ccm...Are you living on Jupiter to reach such a high density for nitric acid what can only reach approx 1.65 g/ccm? Even conc sulfuric doesn't reach such a density.
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 04:46 AM
--------------------------------------------------------------------------------
I guess you have forgotten to set the scale to zero with the container on it before incorporating your 70ml of NA.
I think also that the container weight approx 150g...right?
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-27-2001 04:53 AM
--------------------------------------------------------------------------------
really sorry...
the acid weigh 113.3 g
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-27-2001 05:43 AM
--------------------------------------------------------------------------------
Then it is 113.3g for 70ml this means 113.3/70 = 1.617-1.620g/ccm (considering the error that might come from your scale to be +/- 0.1g and that the Volume is near 100% correct thus 70.00 ml.
I think your acid is thus near 97.5-98%...quite good.
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
goiterjoe
New Member
Posts: 10
From:
Registered: JUN 2001
posted 06-29-2001 01:02 PM
--------------------------------------------------------------------------------
cooking up shit when the Fed-Ex guy shows up is a really easy way to get caught for shit. and be careful ordering hexamine, as it is heavily watched due to it's use in making methylamine. the DEA is all over this one, and if they see it ordered in conjunction with substances such as aluminum powder or mercury salts or borohydrides, it might be your ass.
goiterjoe
New Member
Posts: 10
From:
Registered: JUN 2001
posted 06-29-2001 01:07 PM
--------------------------------------------------------------------------------
guess I should mention that methylamine, sodium borohydride, aluminum, etc. are used to manufacture methamphetamine and exstacy.
stanfield
Frequent Poster
Posts: 176
From: FRANCE
Registered: MAY 2001
posted 06-29-2001 04:00 PM
--------------------------------------------------------------------------------
YEAAAAAAAH !
this morning, I succeeded to make RDX ! but now I know how to make it, i got some new questions, here they are :
- The nitric acid became greenish after the addition of the hexamine, at this point, I stop adding hexamine, is it the good way or do I need to add more hexamine ?
- After that, I boil the solution to 50-60°C for 10 min, the solution changed color to yellowish but why do I need to boil the solution ?
any replies are more than appreciated
mongo blongo
Frequent Poster
Posts: 175
From: I live in a Creosote Bush!
Registered: JUN 2001
posted 07-04-2001 02:49 PM
--------------------------------------------------------------------------------
To PHILOU Zrealone.]
i know ihis is an old topic but it was the only topic i have seen this being talked about in.
looking at above you somehow calculated the %concentration of hno3 from the density.
i have been having problems doing this!
since i have never worked in percentages when working out concs of soloutions. i am probably approaching this the wrong way. i usually work in moles!
this is what i have come up with so far (to show u i have been trying!):
nitric acid (white) is a mixture of hno3 and h20
The Mr of hno3 = 63
Mr of h2o = 18
what is the molar strength of eg. 98% hno3%?
when i know this:
you need 63g hno3 to make 1dm3 of a 1mol soloution.
so then for 98% soloution u nees 63*(molar strength for 98% hno3)
so weight of hno3 per cm3 is (above)/1000
but u need to take the 2%h20 into concideration.
FUCK THIS!!!!
There must be a better way?
how did u do it?
it's probably something really simple! im a dumass!!
please help!
thanx!!
c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 07-05-2001 01:25 AM
--------------------------------------------------------------------------------
mongo blongo: It could probably be calculated mathematically, but why bother? Every decent Chemistry Handbook has a section on the Densities of Aqueous Solutions, where the specific gravities of most common chemicals in solution are shown, as empirically determined and agreed to by international convention.
In the meantime, bookmark this very useful reference page - it gives EVERYTHING you ever wanted to know about nitric acid:
http://www.efma.org/publications/NitricAcid/Section15.asp