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ManyInterests
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Quote: Originally posted by Raid  | | Quote: Originally posted by ManyInterests |
Edit: just some questions about para and ortho-DDNP. Can they be loaded into stainless steel bodies? Also when loaded. How sensitive are they to being
pressed by a vise? I did hear from a user that a few drops of methanol is needed to desensitize them before pressing and allowing them to cure in the
cap before inserting a fuse/electric match. Is this correct?
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I would think that it would be safer to use MeOH or EtOH to desensitize the the DDNP but I have never needed to do this before, The DDNP seems to be
relatively non-sensitive to Newtonian forces. And yes, DDNP can be packed into stainless steel without compatibly issues. Furthermore DDNP is
compatible with almost all transition metals and the DDNP will remain non-effected in contact with these metals for long periods of time.
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OK, so let me see if I understand correctly. Let's say I wanted to make a blasting cap with picric acid as the main charge. If I press the picric acid
into a non-metallic case (like a plastic straw) and then insert that straw into a metal container, I can safely press dry DDNP on top of it with maybe
50kg of pressure (assuming I have a press. The place I wanted to go to buy a cheap C-clamp press no longer carries them) there wouldn't be much danger
of accidental detonation?
Obviously still damping the DDNP before loading and pressing, and then waiting for the methanol/ethanol to evaporate fully before inserting a
fuse/e-match and sealing seems preferable.
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Sir_Gawain
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Using picric acid in a blasting cap might not work well because of its insensitivity. DDNP is fairly safe to press; my crude tests show it to be
slightly more sensitive to impact than NHN, but it's quite a bit more friction sensitive. Dampening it would help. DDNP also needs quite strong
confinement unless in large quantities. 200 mg will not detonate ETN in a thin aluminum tube. I bought some stainless steel tubes for this, then just
switched to NHN because it's safer and easier to work with.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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| Quote: Originally posted by Sir_Gawain | | Using picric acid in a blasting cap might not work well because of its insensitivity. DDNP is fairly safe to press; my crude tests show it to be
slightly more sensitive to impact than NHN, but it's quite a bit more friction sensitive. Dampening it would help. DDNP also needs quite strong
confinement unless in large quantities. 200 mg will not detonate ETN in a thin aluminum tube. I bought some stainless steel tubes for this, then just
switched to NHN because it's safer and easier to work with. |
I'm an NHN guy, too. I made all my caps from NHN so far. It is interesting that you mention that DDNP is only slightly more impact sensitive than NHN.
The reason why I was thinking about making a picric acid/ddnp cap is simply because I want to see how well a cap as described by the Improvised
Munitions Guide works.
The guide calls for 1 gram of a booster (they only list RDX and picric acid as candidates, I guess PETN was harder to make?) and if DDNP is used (they
use the ortho-DDNP, not the para-DDNP) they say that 0.5g is the minimum needed. So I get why you say that you need quite a bit to reliably set off
even a fairly sensitive secondary like ETN.
I might do what some users do and have two separate caps, one with a primary in strong confinement, and the booster in a slightly larger cap which you
insert the first cap into.
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Sir_Gawain
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To test the sensitivity, I built a falling hammer mechanism. From a height that sets off DDNP the first time every time, NHN requires several blows.
For the detonator/booster idea, K&S Precision Metals makes aluminum tubing sizes that fit perfectly into the next size larger.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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fx-991ex
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| Quote: Originally posted by Sir_Gawain | | Using picric acid in a blasting cap might not work well because of its insensitivity. DDNP is fairly safe to press; my crude tests show it to be
slightly more sensitive to impact than NHN, but it's quite a bit more friction sensitive. Dampening it would help. DDNP also needs quite strong
confinement unless in large quantities. 200 mg will not detonate ETN in a thin aluminum tube. I bought some stainless steel tubes for this, then just
switched to NHN because it's safer and easier to work with. |
Did you recrystalise the DDNP from acetone? and for the reduction did you use the dirty method from the military book(sulfur NaOH) or sodium
sulfide/hydrosulfide?(Al2S3+NaOH or dry S+NaOH method or lab grade USP)
Am pretty sure better quality DDNP should definitely set off ETN with around 500mg.
[Edited on 23-6-2023 by fx-991ex]
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Sir_Gawain
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Yes, I recrystallized it. For the reduction I used the improved NaOH/S method from here(scroll down). The problem is not lack of power, it's that small amounts of DDNP (<200 mg) need quite strong confinement to DDT.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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| Quote: Originally posted by fx-991ex | | Quote: Originally posted by Sir_Gawain | | Using picric acid in a blasting cap might not work well because of its insensitivity. DDNP is fairly safe to press; my crude tests show it to be
slightly more sensitive to impact than NHN, but it's quite a bit more friction sensitive. Dampening it would help. DDNP also needs quite strong
confinement unless in large quantities. 200 mg will not detonate ETN in a thin aluminum tube. I bought some stainless steel tubes for this, then just
switched to NHN because it's safer and easier to work with. |
Did you recrystalise the DDNP from acetone? and for the reduction did you use the dirty method from the military book(sulfur NaOH) or sodium
sulfide/hydrosulfide?(Al2S3+NaOH or dry S+NaOH method or lab grade USP)
Am pretty sure better quality DDNP should definitely set off ETN with around 500mg.
[Edited on 23-6-2023 by fx-991ex] |
I actually didn't think to think of recrystalizing DDNP! That would definitely make it more reliable. Also I was not aware that sodium sulfide can
used in the place of sulfur powder. But it has been a long time since I thought about making DDNP.
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Sir_Gawain
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The sulfur/NaOH mixture reacts to form sodium sulfide and polysulfides. Pure sodium sulfide works better but is hard to buy or make (it is extremely
hygroscopic and reacts with moisture to form H2S).
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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Ahh, that makes sense.
Also after looking at sodium sulfide and the price seems high for this project. At any rate, I am seeing the PDF by Rosco about para-DDNP via turning
Tylenol into it. I heard the P-DDNP is less sensitive and more stable than the ortho variant that is described in the improvised munitions guide.
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Sir_Gawain
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Extractions&Ire has a series on both DDNP's. Here's the one on p-DDNP.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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fx-991ex
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https://www.sciencemadness.org/whisper/viewthread.php?tid=63...
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ManyInterests
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Yeah I downloaded both of them years ago. Sometimes I forget I even have those videos! 
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Cubane538
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Hi guys,
Since many days I'm trying to make DDNP but it fails again and again I don't know why...
I took 3g Picric acid and dissolved it in 30ml of hot boiling water.
Then I mixed 2.5g of NaOH with 2.5g sulphur with few drops of water.
And then I added the sodium sulfide mixture to picric acid solution.
After that I filtered the picramic acid.
Everything was fine till i added Picramic acid to hot water.
But after adding 2-3 mls of concentrated sulphuric acid it's colour changed to reddish-orange not brown.
Then I cool down the reddish-orange solution and added 80ml of sodium nitrite solution to it.
And nothing changed!!!
Please guide...
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
 
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
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B(a)P
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| Quote: Originally posted by Cubane538 |
Hi guys,
Since many days I'm trying to make DDNP but it fails again and again I don't know why...
I took 3g Picric acid and dissolved it in 30ml of hot boiling water.
Then I mixed 2.5g of NaOH with 2.5g sulphur with few drops of water.
And then I added the sodium sulfide mixture to picric acid solution.
After that I filtered the picramic acid.
Everything was fine till i added Picramic acid to hot water.
But after adding 2-3 mls of concentrated sulphuric acid it's colour changed to reddish-orange not brown.
Then I cool down the reddish-orange solution and added 80ml of sodium nitrite solution to it.
And nothing changed!!!
Please guide...
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538] |
How sure are you that you have picramic acid and not sodium picrate?
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Cubane538
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| Quote: Originally posted by B(a)P | | Quote: Originally posted by Cubane538 |
Hi guys,
Since many days I'm trying to make DDNP but it fails again and again I don't know why...
I took 3g Picric acid and dissolved it in 30ml of hot boiling water.
Then I mixed 2.5g of NaOH with 2.5g sulphur with few drops of water.
And then I added the sodium sulfide mixture to picric acid solution.
After that I filtered the picramic acid.
Everything was fine till i added Picramic acid to hot water.
But after adding 2-3 mls of concentrated sulphuric acid it's colour changed to reddish-orange not brown.
Then I cool down the reddish-orange solution and added 80ml of sodium nitrite solution to it.
And nothing changed!!!
Please guide...
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538]
[Edited on 19-8-2023 by Cubane538] |
How sure are you that you have picramic acid and not sodium picrate? |
I'm not sure why it's giving sodium picramate.
Although it was my 3rd attempt to make DDNP and this was 3rd time I got this red-orange precipitate..
I'm taking guide from "1969 us army improvised munitions handbook".
I still have that precipitate.
What should I do now?
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fx-991ex
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Dont you have to neutralize the picric acid with NaOH to sodium picrate before processing with the reduction with the sulfide?
That should give you the sodium picramate, that you reacidify to picramic acid before the diazotization with the nitrite.
Am pretty sure that reducing the picric acid will yield H2S gas and sodium picrate.
[Edited on 20-8-2023 by fx-991ex]
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B(a)P
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| Quote: Originally posted by fx-991ex | Dont you have to neutralize the picric acid with NaOH to sodium picrate before processing with the reduction with the sulfide?
That should give you the sodium picramate, that you reacidify to picramic acid before the diazotization with the nitrite.
Am pretty sure that reducing the picric acid will yield H2S gas and sodium picrate.
[Edited on 20-8-2023 by fx-991ex] |
You are correct, that is why I think Cubane538 has sodium picrate. From what is written sodium sulfide has been added directly to picric acid. I would
also add that the method used to generate sodium sulfide is a little unreliable and is likely that it contains a mixture of reactants, products and
some polysulfide compounds. In my opinion a better approach would be to convert the picric acid to sodium picrate using sodium hydroxide. Prepare
sodium sulfide by another method or purify it first. Once you have pure sodium sulfide use it to reduce the sodium picrate to sodium picramate.
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Etanol
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| Quote: Originally posted by dettoo456 |
As for DDNP, it may be compatible but it isnt a great primary on its own. It’s unstable in humid and/or hot environments and too sensitive to
ignition.
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Hmm. Where does such information come from?
The "Diazodinitropheno1, a Detonating Explosive" says that DDNP does not change properties and does not evaporate when heated to 60C, is resistant to
the dispersion light, but was noticeably weaken after 3-5 hours in the direct sunlight.
In addition, it does not change the properties up to 45 days of storage in distilled water at room temperature.
I need high sensitivity to heating so that the electric detonator works from a low energy capacitator and good storage stability.
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dettoo456
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Even though it might be stable at 60C, it doesn’t mean it won’t outgas or react in some manner at any temperatures above that. The tetrazoles
generally won’t react in any way until they detonate, and in such cases, they detonate reliably.
Also, generally, any organic diazo compound comes with its own inherent instability. The same thing goes for organic azides, which is why I would
advise against them too.
If you need higher heat sensitivity in your priming mix, you should try to see how compatible something like Sb2S3 and/or Ba(NO3)2 are with it. Or,
mix a stable but flame sensitive EM like PETN in with your primary.
https://www.mdpi.com/2073-4352/6/1/5
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Etanol
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Is 2,4-dinitrophenyldiazonium perchlorate stable for long storage under the influence of light, wet air and carbon dioxide? Is it possible to prepare
it from Diazodinitrophenol?
[Edited on 1-9-2024 by Etanol]
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