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Author: Subject: TNP Purification
freedompyro
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[*] posted on 27-1-2012 at 23:50
TNP Purification


TNP manages to stand up to hot H2SO4 quite well... Is a water wash and storing it under water good enough or should it be recrystallized somehow?

This synthesis right here works very well and has good yields.


TNP (7480m/s) Note: Toxic! Do not breathe dust or handle without gloves.
183g H2SO4 (98%)
20g ASA (Purified Asprin)
35g KNO3

1. Mix ASA into H2SO4 in a heat safe flask and heat to 90C to dissolve. You should have a black solution at this point.

2. Cool solution to 50C and begin slow additions of KNO3. Keep under 80C. The solution will begin bubble and NOX with each addition. Swirl and let bubbles subside after each addition. Use a fan to suck the NOX away and use a mask. You should have a red solution at this point.

3. Heat the solution to 120C. The solution will turn black again. Five minutes after it turns black it's done. It should take around 10 minutes total.

4. Decant the solution into a measuring cup once it cools to around 65C. If using pyrex you can do it immediately as the glass will not shatter from sudden heat. Cool the solution to around 5C then scoop/pour into cold water with stirring.

5. Filter, wash with water, and collect the TNP.
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freedompyro
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[*] posted on 28-1-2012 at 00:02


I'm not sure this is outside the acceptable scope of scimad... But does anyone know if any of the picrate salts are sensitive enough to be used for pop-its? Maybe potassium picrate. I am talking about the little novelty throwing fireworks you can get on the 4th of july... And the pull string ones.

iI would like to be able to take 3-5mg of a picrate metal salt and place it in 250mg of sand inside thin hobby paper and twist it closed... Throwing it hard at the ground would cause a "POP" sound and it's not powerful enough to cause injury if exploded in hand in such small amounts. As far as I know the pop-its you buy in stores are made with fulminates by hand one at a time in china by workers on a factory line.

You might try to recommend me to use KClO3/Antimony Trisulfide but that is far too insensitive for this... Red phosphorous is not available.


This brings new meaning to the word "yellowcake"... :D That is a 100% stainless steel dehydrator.


[Edited on 28-1-2012 by freedompyro]
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quicksilver
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[*] posted on 28-1-2012 at 12:10


If your interested in the little novelty "cracker-balls" that kids would throw upon the sidewalk, it's actually the construction more that the material(s) that yield the toy. I believe Davis may have some information there. -- Look around page(s) 105 + and there's your information.
In his pyrotechnic section the item was make with washed quartz aquarium gravel and rice-paper covering placed within a Sweety barrel utilizing a mild glue to produce a sphere. The energetic contents would be most materials that provide a small noise from impact and friction. So a few Mg of many materials would function. Obviously the construct must maintain a very low level of energetic so that only noise is produced and no hard matter is in any manner propelled from the little cracker-ball.




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dangerous amateur
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[*] posted on 29-1-2012 at 06:05


How do you know it's TNP?
Couldn't that be just DNP?


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[*] posted on 29-1-2012 at 08:21


Quote: Originally posted by dangerous amateur  
How do you know it's TNP?
Couldn't that be just DNP?




The simplest method if you do not have a melting-point test method that is accurate is the following -
A small milligram level sample is struck between two steel surfaces. Only TNP will "pop". Wrap a tiny "match-head" size sample in aluminum foil and place on a anvil. A hammer blow will created a tiny "cap-like" explosion. Most TNP has SOME DNP in it. But if the level of DNP is too high or if the synthesis has not been carried out fully, the sample will not explode. DNP can create picrate salts however.




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[*] posted on 29-1-2012 at 10:32


" So a few Mg of many materials would function. "
preparation of mega gram amounts of explosives should only be undertaken by professionals.
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[*] posted on 29-1-2012 at 11:02


If you need really pure TNP, perhaps try re-sulfonating/nitrating the TNP/DNP to convert any remaining DNP to TNP?

@ unionised - Good luck throwing a snapper weighing a couple thousand kilos. :D

Be careful though. I get goosebumps thinking about giving kids high explosives. I don't think I'd trust myself to make them with such consistency as to ALWAYS be safe.




Victor Grignard is a methylated spirit.
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