megalomania
June 17th, 2003, 08:07 PM
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 05-31-2001 06:46 PM
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How is picramic acid prepared for this stuff? Im thinking about making some sometime, as it seems like it would be pretty good. Improvised Primary Explosives has a way of making it, but im not sure as if that would be the best process for it.
Also, can sulfuric acid be used in megalomania's procedure instead of HCl?
[This message has been edited by FadeToBlackened (edited May 31, 2001).]
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 05-31-2001 06:49 PM
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PICRAMIC???????????
OHHHHH you mean Picric!
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 05-31-2001 07:11 PM
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PREPARATION OF PICRIC ACID FROM ASPIRIN
Picric acid can be used as a booster explosive in detonators, a high explosive charge, or as an intermediate to preparing lead picrate or DDNP.
MATERIALS:
Aspirin tablets (5 grains per tablet)
Alcohol, 95% pure
Sulfuric acid, concentrated(battery acid boiled until white fumes appear).
Potassium nitrate
Water
Paper towels
Canning jar, 1 pint
Rod (glass or wood)
Glass containers
Ceramic or glass dish
Cup
Teaspoon
Tablespoon
Pan
Heat source
Tape
PROCEDURE:
1. Crush 20 aaspirin tablets in a glass container. Add 1 teaspoon of water and work into a paste.
2. Add approximately 1/3 to 1/2 a cup of alcohol (100 militers) to the aspirin paste; stir while pouring.
3. Filter the alcohol- aspirin solution through a paper towel into another glass container. Discard the solid left on the paper towel.
4. Pour the filtered solution into a ceramic or glass dish.
5. Evaporate the alcohol and water from the solution by placing the dish into a pan of hot water. White powder will remain in the dish after evaporation.
NOTE: Water in the pan should be at hot bath temperature, not boiling approximately 160 to 180degrees F. It should not burn the hands.
6. Pour 1/3 cup (80 militers) of concentrated sulfuric acid into a canning jar. Add the white powder to the sulfuric acid.
7. Heat canning jar of sulfuric acid in a pan of simmering hot water bath for 15 minutes; then remove jar from the bath. Solution will turn to a yellow-orange color.
8. Add 3 level teaspoons (15 grams) of potassium nitrate in three portions to the yellow-orange solution; stir vigorously during additions. Solution will turn red, and then back to a yellow-orange color.
9. Allow the solution to cool to ambient or room temperature while stirring occasionally.
10. Slowly pour the solution, while stirring, into 1-1/4 cup(300 militrers) of cold water and allow to cool.
11. Filter the solution through a paper towel into a glass container. Light yellow particles will collect on the paper towel.
12. Wash the light yellow particles with 2 tablespoons (25 militers) of water. Discard the waste liquid in the container.
13. Place particles in ceramic dish and set in a hot water bath, as in step 5, for 2 hours.
ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 05-31-2001 07:15 PM
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No, he meant pircramic acid.
2-amino-4,6-dinitrophenol; 6-amino-2,4-dinitrophenol; dinitroaminophenol; 2,4-dinitro-6-aminophenol; 4,6-dinitro-2-aminophenol; 2-hydroxy-3,5-dinitroaniline; picraminic acid
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 05-31-2001 07:19 PM
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There is no mention of picramic acid,in any of the synthesis for DDNP I have seen. Where can I find more info about Picramic acid??
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 05-31-2001 08:45 PM
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look at megalomania's synthesis..
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 05-31-2001 10:29 PM
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[This message has been edited by 10fingers (edited October 26, 2001).]
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 06-01-2001 12:28 AM
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To synthesize DDNP, it would be best to use these starting materials:
Picric acic/3parts
Sulfur(powdered)/2.5parts
Sodium hydroxide/3parts
Potassium nitrate/1.8parts
Sulfuric acid/2.5parts
Water
Is that right???
[This message has been edited by Mekap (edited June 01, 2001).]
gcic
Frequent Poster
Posts: 80
From: Germany
Registered: OCT 2000
posted 06-01-2001 12:56 AM
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Why should you use sulfur?
picramic acid is synthesized by partial reduction of picric acid or sodium picrate with sodium hydrogen sulfide in a solution of water.
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 06-01-2001 01:18 AM
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In IPE sulfur is heated with NaOH solution to for sodium sulfide (i guess). Im just not sure if that recipe is the best to follow, and I cant figure it out for myself because i dont know how to reaction works...
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 06-01-2001 01:42 AM
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*
[This message has been edited by 10fingers (edited July 19, 2001).]
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 06-01-2001 01:48 AM
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1. Pour 30 parts of warm water into first acid resistant container.
2. Stir 0.5parts of sodium hydroxide into the water in the first container.
3. Stir 3 parts Picric acid into the water/sodium hydroxide mixture. Set this mixture aside.
4. Pour 1 parts water into a heat/acid resistant container.
5. Stir 2.5 parts of powdered sulfur and 2.5 parts of sodium hydroxide into the water in the heat/acid resistant container. Stir for one minute.
6. Place the water/sulfur/sodium hydroxide mixture on a heat source. Gently heat the mixture until it turns a dark red color. Remove the mixture from heat and allow it to cool to room temperature.
7. Slowly stir the red water/sulfur/sodium hydroxide mixture into the water/picric acid/sodium hydroxide mixture from step three. Let this new mixture stand for 30 minures, stirring every 5 minutes.
8. Filter this mixture through filter paper. Reddish crystals will collect on the paper. Keep the crystals and discard the liquid.
9. Thoroughly wash and dry the heat/acid resistant container.
10. Pour 60 parts water into the heat/acid resistant container and heat to a low boil. Turn off heat.
11. Dissolve the red crystals from step 8 in the boiling water.
12. Filter this mixture through filter paper. This time keep the liquid and discard the material that collects on the filter paper. The liquid should now be in the second acid resistant container.
13. Pour 6 parts water into a third acid-resistant container. Slowly stir 3 parts of sulfuric acid into the water. This water acid mixture will be referred to as diluted sulfuric acid.
14. Stir one drop at a time of the diluted sulfuric acid into the liquid in the second acid-resistant container until the liquid turns an orange-brown color. Be sure to add the acid one drop at a time so only the minimum amount necessary to change the liquids color is used. Let this mixture stand for five minutes.
15. Stir in an additional 2.5 parts of diluted sulfuric acid into the above mixture. Let this mixture stand for 30 minutes.
16. Thoroughly wash and dry the first acid resistant container.
17. Pour 80 parts water into the first acid resistant container. Stir 1.75 parts potassium nitrate into the water, stir until all potassium nitrate has dissolved.
18. Stir the potassium nitrate/water mixture into the mixture from step 15. NOTE: The crystals that settle out of this new mixture are DDNP handle with care.
It goes on but I think you get the idea. I am be no means saying this is accurate, I was hoping you could tell me?
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 06-01-2001 02:04 AM
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Ive seen 3 recipes including that one now, and they all use the same proportions of sulfur to NaOH, and PA to NaOH, so im thinking that part is probably ok. I have yet to compare the latter parts of them with megalomanias method. And it is nitrite not nitrate.
Btw anyone know what .1M hydrochloric acid corresponds to in %?
[This message has been edited by FadeToBlackened (edited June 01, 2001).]
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-01-2001 05:17 PM
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FadeToBlackened: 0.1 moles of HCl per litre of water, therefore 3.65 grams of HCl per 1000 grams of water, therefore 0.36% (not very strong!)
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 05-31-2001 06:46 PM
--------------------------------------------------------------------------------
How is picramic acid prepared for this stuff? Im thinking about making some sometime, as it seems like it would be pretty good. Improvised Primary Explosives has a way of making it, but im not sure as if that would be the best process for it.
Also, can sulfuric acid be used in megalomania's procedure instead of HCl?
[This message has been edited by FadeToBlackened (edited May 31, 2001).]
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 05-31-2001 06:49 PM
--------------------------------------------------------------------------------
PICRAMIC???????????
OHHHHH you mean Picric!
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 05-31-2001 07:11 PM
--------------------------------------------------------------------------------
PREPARATION OF PICRIC ACID FROM ASPIRIN
Picric acid can be used as a booster explosive in detonators, a high explosive charge, or as an intermediate to preparing lead picrate or DDNP.
MATERIALS:
Aspirin tablets (5 grains per tablet)
Alcohol, 95% pure
Sulfuric acid, concentrated(battery acid boiled until white fumes appear).
Potassium nitrate
Water
Paper towels
Canning jar, 1 pint
Rod (glass or wood)
Glass containers
Ceramic or glass dish
Cup
Teaspoon
Tablespoon
Pan
Heat source
Tape
PROCEDURE:
1. Crush 20 aaspirin tablets in a glass container. Add 1 teaspoon of water and work into a paste.
2. Add approximately 1/3 to 1/2 a cup of alcohol (100 militers) to the aspirin paste; stir while pouring.
3. Filter the alcohol- aspirin solution through a paper towel into another glass container. Discard the solid left on the paper towel.
4. Pour the filtered solution into a ceramic or glass dish.
5. Evaporate the alcohol and water from the solution by placing the dish into a pan of hot water. White powder will remain in the dish after evaporation.
NOTE: Water in the pan should be at hot bath temperature, not boiling approximately 160 to 180degrees F. It should not burn the hands.
6. Pour 1/3 cup (80 militers) of concentrated sulfuric acid into a canning jar. Add the white powder to the sulfuric acid.
7. Heat canning jar of sulfuric acid in a pan of simmering hot water bath for 15 minutes; then remove jar from the bath. Solution will turn to a yellow-orange color.
8. Add 3 level teaspoons (15 grams) of potassium nitrate in three portions to the yellow-orange solution; stir vigorously during additions. Solution will turn red, and then back to a yellow-orange color.
9. Allow the solution to cool to ambient or room temperature while stirring occasionally.
10. Slowly pour the solution, while stirring, into 1-1/4 cup(300 militrers) of cold water and allow to cool.
11. Filter the solution through a paper towel into a glass container. Light yellow particles will collect on the paper towel.
12. Wash the light yellow particles with 2 tablespoons (25 militers) of water. Discard the waste liquid in the container.
13. Place particles in ceramic dish and set in a hot water bath, as in step 5, for 2 hours.
ALENGOSVIG1
Moderator
Posts: 766
From: Vancouver, Canada
Registered: NOV 2000
posted 05-31-2001 07:15 PM
--------------------------------------------------------------------------------
No, he meant pircramic acid.
2-amino-4,6-dinitrophenol; 6-amino-2,4-dinitrophenol; dinitroaminophenol; 2,4-dinitro-6-aminophenol; 4,6-dinitro-2-aminophenol; 2-hydroxy-3,5-dinitroaniline; picraminic acid
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 05-31-2001 07:19 PM
--------------------------------------------------------------------------------
There is no mention of picramic acid,in any of the synthesis for DDNP I have seen. Where can I find more info about Picramic acid??
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 05-31-2001 08:45 PM
--------------------------------------------------------------------------------
look at megalomania's synthesis..
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 05-31-2001 10:29 PM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited October 26, 2001).]
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 06-01-2001 12:28 AM
--------------------------------------------------------------------------------
To synthesize DDNP, it would be best to use these starting materials:
Picric acic/3parts
Sulfur(powdered)/2.5parts
Sodium hydroxide/3parts
Potassium nitrate/1.8parts
Sulfuric acid/2.5parts
Water
Is that right???
[This message has been edited by Mekap (edited June 01, 2001).]
gcic
Frequent Poster
Posts: 80
From: Germany
Registered: OCT 2000
posted 06-01-2001 12:56 AM
--------------------------------------------------------------------------------
Why should you use sulfur?
picramic acid is synthesized by partial reduction of picric acid or sodium picrate with sodium hydrogen sulfide in a solution of water.
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 06-01-2001 01:18 AM
--------------------------------------------------------------------------------
In IPE sulfur is heated with NaOH solution to for sodium sulfide (i guess). Im just not sure if that recipe is the best to follow, and I cant figure it out for myself because i dont know how to reaction works...
10fingers
Frequent Poster
Posts: 411
From: USA
Registered: SEP 2000
posted 06-01-2001 01:42 AM
--------------------------------------------------------------------------------
*
[This message has been edited by 10fingers (edited July 19, 2001).]
Mekap
New Member
Posts: 37
From: Australia
Registered: MAY 2001
posted 06-01-2001 01:48 AM
--------------------------------------------------------------------------------
1. Pour 30 parts of warm water into first acid resistant container.
2. Stir 0.5parts of sodium hydroxide into the water in the first container.
3. Stir 3 parts Picric acid into the water/sodium hydroxide mixture. Set this mixture aside.
4. Pour 1 parts water into a heat/acid resistant container.
5. Stir 2.5 parts of powdered sulfur and 2.5 parts of sodium hydroxide into the water in the heat/acid resistant container. Stir for one minute.
6. Place the water/sulfur/sodium hydroxide mixture on a heat source. Gently heat the mixture until it turns a dark red color. Remove the mixture from heat and allow it to cool to room temperature.
7. Slowly stir the red water/sulfur/sodium hydroxide mixture into the water/picric acid/sodium hydroxide mixture from step three. Let this new mixture stand for 30 minures, stirring every 5 minutes.
8. Filter this mixture through filter paper. Reddish crystals will collect on the paper. Keep the crystals and discard the liquid.
9. Thoroughly wash and dry the heat/acid resistant container.
10. Pour 60 parts water into the heat/acid resistant container and heat to a low boil. Turn off heat.
11. Dissolve the red crystals from step 8 in the boiling water.
12. Filter this mixture through filter paper. This time keep the liquid and discard the material that collects on the filter paper. The liquid should now be in the second acid resistant container.
13. Pour 6 parts water into a third acid-resistant container. Slowly stir 3 parts of sulfuric acid into the water. This water acid mixture will be referred to as diluted sulfuric acid.
14. Stir one drop at a time of the diluted sulfuric acid into the liquid in the second acid-resistant container until the liquid turns an orange-brown color. Be sure to add the acid one drop at a time so only the minimum amount necessary to change the liquids color is used. Let this mixture stand for five minutes.
15. Stir in an additional 2.5 parts of diluted sulfuric acid into the above mixture. Let this mixture stand for 30 minutes.
16. Thoroughly wash and dry the first acid resistant container.
17. Pour 80 parts water into the first acid resistant container. Stir 1.75 parts potassium nitrate into the water, stir until all potassium nitrate has dissolved.
18. Stir the potassium nitrate/water mixture into the mixture from step 15. NOTE: The crystals that settle out of this new mixture are DDNP handle with care.
It goes on but I think you get the idea. I am be no means saying this is accurate, I was hoping you could tell me?
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 06-01-2001 02:04 AM
--------------------------------------------------------------------------------
Ive seen 3 recipes including that one now, and they all use the same proportions of sulfur to NaOH, and PA to NaOH, so im thinking that part is probably ok. I have yet to compare the latter parts of them with megalomanias method. And it is nitrite not nitrate.
Btw anyone know what .1M hydrochloric acid corresponds to in %?
[This message has been edited by FadeToBlackened (edited June 01, 2001).]
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-01-2001 05:17 PM
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FadeToBlackened: 0.1 moles of HCl per litre of water, therefore 3.65 grams of HCl per 1000 grams of water, therefore 0.36% (not very strong!)