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Author: Subject: ANGN ever made on SM ?
underground
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[*] posted on 23-5-2019 at 14:46


Wow Great job Boffis and really nice photoes!! Can you try out the nitrate salt too ? :D The hcl salt looks like fibers, just like nitroguanidine. If the nitrate salt would be the same, i really doubt if high density can be achieved

[Edited on 23-5-2019 by underground]
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Microtek
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[*] posted on 24-5-2019 at 03:21


The nitrate does not form fibers, but rather cubic crystals that are very similar to ordinary granular sugar. Recently, I took another look at the sample of ANQN that had decomposed on standing about one month in the open. I dissolved it in warm 65% HNO3 and upon cooling, crystals that are visually identical to those originally prepared formed. I think this is a strong indication that the decomposition I have observed is in fact (primarily) loss of weakly bound nitric acid.
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[*] posted on 24-5-2019 at 11:21


Yea. Maybe at lower temps without light it could stay more. Have you ever try the clo4 salt? It may be more stable. Did u try to detonate it ?
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[*] posted on 28-5-2019 at 03:15


No, I haven't tried detonating it, but I do agree that the low vapour pressure of perchloric acid would tend to make the salt more stable (and also the lower pKa of HClO4 relative to HNO3 of course).
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[*] posted on 29-5-2019 at 20:35


I thought the chlorite salt lost all elite VOD, and P and sensitivity traits. Why not just shoot for the best and accept stability issues. Such as coating with an oil or a wax.
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[*] posted on 30-5-2019 at 09:58


OK I have had a go at preparing the nitrate and the perchlorate salts of aminonitroguanidine today. The nitrate salt is currently drying over CaO to remove the excess water and nitric acid since it is difficult to wash without loss of nitric acid and the perchlorate hasn't started to crystallise yet.

Nitrate: 2.7ml of 68% nitric acid was diluted to 5ml and 1.5g of aminonitroguanidine was added and the mixture warmed (very) gently :). I actually weighed out 2.3g which is still less than the Fischer et al paper calls for but after I struggled to get 1.5g todissolve I chicken out and reweighed the weighing boat at this point and I had added slightly less than 1.5g; enough I thought! The clear faintly yellow solution was left to crystallise slow. The crystals were broken up and filtered to yield colourless, dense, blocky crystals up to about 0.4 to 0.7mm, like granulated sugar in appearance as Microtek says.

Perchlorate: This compound is reportedly much more sensetive and I am much less happy about handling it so I initially used on 0.81g in 15ml of 1M perchloric acid but this crystallised too quickly so I redissolved it and added an extra 5ml of acid and left it to cool slowly. The crystals are not as dense and granular as those of the nitrate salt.
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[*] posted on 31-5-2019 at 12:51


Quote: Originally posted by Boffis  
OK I have had a go at preparing the nitrate and the perchlorate salts of aminonitroguanidine today. The nitrate salt is currently drying over CaO to remove the excess water and nitric acid since it is difficult to wash without loss of nitric acid and the perchlorate hasn't started to crystallise yet.

Nitrate: 2.7ml of 68% nitric acid was diluted to 5ml and 1.5g of aminonitroguanidine was added and the mixture warmed (very) gently :). I actually weighed out 2.3g which is still less than the Fischer et al paper calls for but after I struggled to get 1.5g todissolve I chicken out and reweighed the weighing boat at this point and I had added slightly less than 1.5g; enough I thought! The clear faintly yellow solution was left to crystallise slow. The crystals were broken up and filtered to yield colourless, dense, blocky crystals up to about 0.4 to 0.7mm, like granulated sugar in appearance as Microtek says.

Perchlorate: This compound is reportedly much more sensetive and I am much less happy about handling it so I initially used on 0.81g in 15ml of 1M perchloric acid but this crystallised too quickly so I redissolved it and added an extra 5ml of acid and left it to cool slowly. The crystals are not as dense and granular as those of the nitrate salt.


Well I have tried an ignition test on each of the compounds and they both deflagrate vigorously but nothing special; the perchlorate seems a little more vigorous. When heated on foil they both melt before deflagrating, the nitrate leaves practically no residue.
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[*] posted on 31-5-2019 at 13:29


I have done some tests on the supposed reconstituted nitrate salt. On ignition it deflagrates quite vigorously and it can be set off by hammer blows (but not very easily; I definitely wouldn't worry about accidental explosion from ordinary handling). I think it is likely that this substance is in fact ANQN.
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[*] posted on 1-6-2019 at 11:05


The best think it would be to see both salts at what max density can be pressed (1) and detonate 3-4gr into a steel plate and compare them to PETN, ETN or RDX (2)

[Edited on 1-6-2019 by underground]
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[*] posted on 1-6-2019 at 21:17


That is some burning quickly is nice, but main is how is behavior of material in cavity at high density. What described underground. Thus for example 1g ANQN (high pressed) against steel plate 3 mm. With some primary 0,2 g. If is it necessary ever. In plate should by hole. In plate 2 mm of thickness should by hole as same diameter a like diameter of pressed charge. At 1 g and diameter 8 mm. Or even bigger hole...:cool:...LL



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[*] posted on 2-6-2019 at 23:51


Mineman commands these test be done!!! Listen to the mind of mineman.
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[*] posted on 8-1-2021 at 15:19


Here is my synthesis and testing of ANQN:
https://www.youtube.com/watch?v=vTrBWW_fqe8




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[*] posted on 8-1-2021 at 15:28


Mine man happy. Next test DBX is to mix with 10-15 percent aluminum powder and test DDT in copper tube. 1 gram
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[*] posted on 8-1-2021 at 16:22


Yeah I can try that sometime tomorrow. 3 micron flake Al.



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[*] posted on 8-1-2021 at 17:14


Quote: Originally posted by DBX Labs  
Yeah I can try that sometime tomorrow. 3 micron flake Al.


Perfect! Follow the compression instructions of LL if possible. If this DDTs, you got the best.

If AL does not work I have other ideas.
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[*] posted on 8-1-2021 at 18:04


Quote: Originally posted by MineMan  
Quote: Originally posted by DBX Labs  
Yeah I can try that sometime tomorrow. 3 micron flake Al.


Perfect! Follow the compression instructions of LL if possible. If this DDTs, you got the best.

If AL does not work I have other ideas.


Wait, are you proposing that I attempt to initiate with a fuse? I was going to be using one of my BNCP bridgewire detonators




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[*] posted on 10-1-2021 at 12:51


This should make MineMan happy.

I tested the 15:85 Al to ANQN composition out both with fuse ignition and through BNCP bridge wire initiation.
To start, this mix burns quite vigorously, I'd compare it to a slower TACP but brighter due to Al. (I used 3-micron flake).

Fuse Ignition:
I lightly ground the mix with a mortar and pestle and compressed a 0.5-gram charge into plastic housing. Density was calculated to be >1.4 grams/cc. When the fuse reached the compressed mix, it burned like a rocket motor; fast, but doesn't look like a potential DDT primer.

BNCP Bridgewire Initiation:
1 gram of fine 15:85 powder was loaded and compressed inside plastic housing to >1.4 grams/cc. 0.05 grams of loose ETN filled gaps between BNCP bridgewire detonator and compressed mix.
Holy shit.
It was loud and powerful. By far more of a bang than any other secondary, I've yet to work with.
Looking through the slo-mo, it DEFINITELY went thermobaric. That fireball is unmistakenly the near-instantaneous combustion of the AL powder.
The pan hole is much bigger than either of the test pans produced in my video on the ANQN.

With MineMan's consent, I plan to make a short video on this mix (including the thread) as well as the bis-aminonitroguanidinocopper ii nitrate perfect OB complex that I've made.

Attachment: IMG_7206.MOV_Trim mega.mp4 (6.5MB)
This file has been downloaded 485 times





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[*] posted on 10-1-2021 at 13:14


Mad substance from .MOV. Great work. And fire effect with secondary spark from cables.....:cool:



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[*] posted on 10-1-2021 at 22:27


Good work! Try uncompressed for DDT. Yes. Aluminum will increase the power substantially. Should DDT in aluminum or copper casing with LLs CHP method of compression.
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[*] posted on 12-1-2021 at 08:40


CHP was tested in pretty thin cavity 7mm/8 mm from brass. Wall only 0.5 mm. And works also. But for best reliability is better steel or copper wall 1 mm. For ANQN shlould by thin brass enough I estimate. However with classic ignition hot wire. Using high huge electric shock generator is not practical.
For example in forrest. For laboratory testing is it great. But in fight not....:cool:

[Edited on 12-1-2021 by Laboratory of Liptakov]




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[*] posted on 12-1-2021 at 22:17


Yeah, I exhausted my 10 grams of ANQN in recent tests with the Al so I’ll have to make some more to record with. I’ve reached out to a local university energetics group which has forwarded the crude data I collected to local military research establishments. Hopefully something will come of it.
I just am personally ecstatic seeing the clear thermobaric detonation on the film I took. Everything works out in theory, and testing confirms it both visually, and quantitatively.
Big thanks to MineMan for idea.

In response to LL, I haven’t been able to get it to DDT from ignition; rather, it burns like a high grade propellant. I can pretty much say with certainty that I don’t have the testing materials required to contain a compressed sample for hot-wire ignition of that sort. Not to say it shouldn’t be tested. What you bring up likely holds great potential.
My ultimate safe go-to primer has rapidly become my BNCP detonators which for my purposes, have little area for improvement.

[Edited on 13-1-2021 by DBX Labs]




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[*] posted on 12-1-2021 at 23:39


Great job! DDT testing would be easy. Copper tubing from hardware store and a wooden dowel. Use a fuse.

Yes. Of course the aluminum worked. 15 percent is usually the optimal amount for explosive power which is the heat times volume of gas. Being an OB explosive makes this perfect. Although some explosives perform higher at OB- because of CO.
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[*] posted on 14-1-2021 at 08:08


I also recommend classic ignition method. According MineMan descriptions. It would be great, if worked it. With an fuse. Metal cavity is important for easy manipulation. For example easy penetration into plastic secondary. With thin plast tube is it difficulty.



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[*] posted on 21-1-2021 at 13:50


Looking forward to your aluminized test video :)
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[*] posted on 10-4-2023 at 07:45
ANQ Preparation Issue


This thread is on ANQN, but ANQ is entroute to ANQN and I have been having issues with ANQ. I was hoping someone else may have seen these issues and be familiar with remedy.

The hang up for me is at the point when the yellow solution of dissolved NQ and hydrazine is either cooled or buffered down to 7 pH with HCl. I have tried both the method of cooling and also tried to reduce pH prior to cooling. I have also attempted to shoot the pH way down to ~2 and brought it back up to ~7-8 with NH4OH. All of this was just attempting to figure out what is going on, but I'm left a little confused. In all attempts the NQ used here is double recrystallized neutral NQ and the hydrazine is from Hydrazine sulfate freebased from NaOH in denatured alcohol.

The NQ dissolves, the solution changes yellow during addition of hydrazine over 15 minutes, then the color strengthens after continued stirring for 15 minutes all at 55 C. The solution does not turn the darker orange that is reported by others. Upon removing from heat to cool, light yellow material precipitates out of solution at around 35 C. The material does not seem to be ANQ as the mp is above 240 C. Its a little fibrous so it appears to be NQ although its form has changed somewhat. In other experiment, after cooling failed during the prior experiment, pH was reduced with HCl while still around 40C, this did not change the precipitation of NQ from happening at lower temp ~35 C. This was repeated again but this time pH was reduced to around 2-3, the material precipitated again on pH reduction and the color of yellow was entirely removed leaving a white mass in clear solution. NH4OH was added and at around pH of 7, the yellow color returns and the mass of precipitated nitroguanidine remains. At no time does the solution turn orange and in all attempts a material precipitates that seems to be nitroguanidine. The material remains and the solution does not redissolve the mass on standing overnight at neutral pH or darken or change color. I believe this nitroguanidine could be recrystallized and used again.

Does anyone know what is going wrong here? The hydrazine is already in slight excess, is it possible that the hydrazine should be in even greater excess?

Or perhaps longer reaction time?

Im not sure why it changes from yellow to white and back to yellow with pH adjustment. ANQ*Cl has a low mp and ANQ also has a low mp. This materials mp is around what NQ would be.

[Edited on 10-4-2023 by Hey Buddy]

I should also mention, I have tried the reaction without any buffering and just allowing it to cool. After around 24 hours the solution becomes more amber in color but there isnt really much precipitate formed at all. This is all at the native reaction pH around 11.


[Edited on 10-4-2023 by Hey Buddy]
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