| Pages:
1
2
3 |
underground
National Hazard
Posts: 703
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
Wow Great job Boffis and really nice photoes!! Can you try out the nitrate salt too ?  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]
|
|
|
Microtek
National Hazard
Posts: 871
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
underground
National Hazard
Posts: 703
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
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 ?
|
|
|
Microtek
National Hazard
Posts: 871
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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).
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
Boffis
International Hazard
Posts: 1868
Registered: 1-5-2011
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
Boffis
International Hazard
Posts: 1868
Registered: 1-5-2011
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
Microtek
National Hazard
Posts: 871
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
underground
National Hazard
Posts: 703
Registered: 10-10-2013
Location: Europe
Member Is Offline
|
|
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]
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1397
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
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... ...LL
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
Mineman commands these test be done!!! Listen to the mind of mineman.
|
|
|
DBX Labs
Hazard to Self
Posts: 57
Registered: 24-12-2020
Member Is Offline
|
|
Here is my synthesis and testing of ANQN:
https://www.youtube.com/watch?v=vTrBWW_fqe8
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
Mine man happy. Next test DBX is to mix with 10-15 percent aluminum powder and test DDT in copper tube. 1 gram
|
|
|
DBX Labs
Hazard to Self
Posts: 57
Registered: 24-12-2020
Member Is Offline
|
|
Yeah I can try that sometime tomorrow. 3 micron flake Al.
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
DBX Labs
Hazard to Self
Posts: 57
Registered: 24-12-2020
Member Is Offline
|
|
| Quote: Originally posted by MineMan |
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
|
|
|
DBX Labs
Hazard to Self
Posts: 57
Registered: 24-12-2020
Member Is Offline
|
|
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 580 times
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1397
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
Mad substance from .MOV. Great work. And fire effect with secondary spark from cables.....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1397
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
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....
[Edited on 12-1-2021 by Laboratory of Liptakov]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
DBX Labs
Hazard to Self
Posts: 57
Registered: 24-12-2020
Member Is Offline
|
|
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]
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1397
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
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.
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
MineMan
International Hazard
Posts: 1004
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
Looking forward to your aluminized test video
|
|
|
Hey Buddy
Hazard to Others
Posts: 434
Registered: 3-11-2020
Location: Bushwhacker Country
Member Is Online
|
|
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]
|
|
|
| Pages:
1
2
3 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
