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Author: Subject: 5-ATZ(5-Aminotetrazole), the nitrotetrazolate ion and friends
B(a)P
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[*] posted on 8-12-2022 at 15:47


Some 5,5'-azotetrazolate salts, via double displacement of sodium 5,5'-azotetrazolate.
The cadmium salt was attempted, the reaction failed as the pH of the cadmium nitrate solution was too high or contained too much dissolved NO2 and the 5,5'-azotetrazolate decomposed.
The ammonium salt was attempted, the reaction failed to produce a precipitate and when taken to dryness decomposed.




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[*] posted on 6-2-2024 at 10:38


Is it normal that the wet Ag nitrotetrazolate does not explode from the fire, but only crackles?
Is it permissible to store AgNTz for 1-2 years in direct contact with PETN, ETN, aluminium, NiCr alloy?
Can AgNTz be recrystallized from water ammonia? Will sensitivity decrease after recrystallization?
Is the stability of AgNTz to light lower or higher than that of AgN3?
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[*] posted on 6-2-2024 at 11:18


Quote: Originally posted by Etanol  
Is it normal that the wet Ag nitrotetrazolate does not explode from the fire, but only crackles?

Yes and if you heat it indirectly it will detonate after a short period of time, I guess once it has lost enough water.

Quote: Originally posted by Etanol  
Is it permissible to store AgNTz for 1-2 years in direct contact with PETN, ETN, aluminium, NiCr alloy?

It is storage stable for at least 1 year against copper and aluminium, I have not tried the others you mention.

Quote: Originally posted by Etanol  
Is the stability of AgNTz to light lower or higher than that of AgN3?

I have not tried a comparison to AgN3. It is similar to silver fulminate. In indirect sun light it will decompose within weeks to months.
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[*] posted on 6-2-2024 at 15:27


Quote: Originally posted by B(a)P  

It is storage stable for at least 1 year against copper and aluminium,

Thank you.
More questions.
Is AgNTz stable to hydrolysis in boiling water? In water with a temperature of 80C?
Is the cream color normal for AgNTz?
Which bulk density is normal for AgNTz?
What is the maximum density when pressing with hands?

Quote: Originally posted by Etanol  

Can AgNTz be recrystallized from water ammonia?

Checked: Yes, perhaps.

[Edited on 6-2-2024 by Etanol]
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[*] posted on 7-2-2024 at 02:33


Quote: Originally posted by Etanol  

Is AgNTz stable to hydrolysis in boiling water? In water with a temperature of 80C?

I have not tried, but have seen it reported that it is not susceptible to hydrolysis.

Quote: Originally posted by Etanol  
Is the cream color normal for AgNTz?

Not in my experience, maybe slightly off white though.


Quote: Originally posted by Etanol  
Which bulk density is normal for AgNTz?

I have not measured this nor can I find any reference for it.

Quote: Originally posted by Etanol  
What is the maximum density when pressing with hands?

I have not measured maximum density, but note that using a press it will easily dead press.
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[*] posted on 8-2-2024 at 12:33


More questions
Is it possible to replace CuCl2 => CuSO4 in the synthesis of DBX-1 with ascorbate?
Is it permissible to store DBX-1 for 1-2 years in direct contact with PETN, ETN, aluminium, NiCr alloy?
Can DBX-1 be recrystallized?
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[*] posted on 8-2-2024 at 15:52


You can probably swap CuCl2 for CuSO4, but you need to reduce the active Cu species to Cu 1, not Cu 2 in any case for the synthesis to work.

DBX-1 likely cannot be recrystallized, simply due to its insolubility, same as AgNTz (which isn’t actually soluble in Aq NH3).

It is likely compatible with PETN, less so with ETN (because of ETN’s inherent instability) and I cannot vouch for its compatibility with Al or Ni-Cr.

If you want a good det train, just use loose AgNTz, loose PETN, and slightly pressed PETN in a brass sleeve.

AgNTz IS NOT COMPATIBLE WITH ALUMINUM THOUGH!

[Edited on 8-2-2024 by dettoo456]
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[*] posted on 8-2-2024 at 18:40


Quote: Originally posted by dettoo456  


AgNTz IS NOT COMPATIBLE WITH ALUMINUM THOUGH!



It is interesting that you say this, I have tested this by placing a small sample into an aluminium tube for over 12 months. At the end of the test, there was no obvious mark on the metal or any noticeable change to performance. I note that because the sample was so small I was only able to do limited testing - direct flame test and indirect flame test wrapped in foil.
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[*] posted on 8-2-2024 at 22:37


Quote: Originally posted by dettoo456  
You can probably swap CuCl2 for CuSO4, but you need to reduce the active Cu species to Cu 1, not Cu 2 in any case for the synthesis to work.

Thanks. I'll try it.

Quote: Originally posted by dettoo456  

DBX-1 likely cannot be recrystallized, simply due to its insolubility, same as AgNTz (which isn’t actually soluble in Aq NH3).

The AgNTz is perfectly dissolved in water ammonia and settles back when the ammonia is evaporated and neutralize by diluted acetic acid to pH3 approximately.
Similarly, I recrystallized silver azide and silver fulminate.
But I am not sure with copper.

Quote: Originally posted by dettoo456  

It is likely compatible with PETN, less so with ETN (because of ETN’s inherent instability) and I cannot vouch for its compatibility with Al or Ni-Cr.

I find "DBX-1 – A Lead Free Replacement for Lead Azide":

"Compatibility studies of DBX-1 with a variety of output powders, bridgewire materials and component metals were conducted by both metal coupon and DSC test
methods...Coupon metals include 1100 aluminum, 6061-T6 aluminum, 2029-T3 aluminum, 304 stainless steel, brass and a MK107 gilding metal cup (95 % copper and 5 % zinc). Observations made during exposure of up to 1 year demonstrated no reaction or change in the coupons.

Compatibility testing was also done on bridgewire materials including Tophet C (nichrome), Tophet A (StableOhm 650) and EvenOhm (StableOhm 800) via DSC....Analyses of the various spectra indicated no shift or change in the thermal profile for DBX-1 and demonstrated compatibility of DBX-1 with these materials."

Quote: Originally posted by dettoo456  

AgNTz IS NOT COMPATIBLE WITH ALUMINUM THOUGH!

Hmm, I'll clarify it.
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[*] posted on 9-2-2024 at 09:26


If your AgNTz is dissolving in aq NH3 then it might just be disassociating into something weird. It shouldn’t dissolve.

Maybe liq NH3 might dissolve it but even if the AgNTz is exposed to aq NH3, the most it might do is form an ammonia complex which would still be insoluble.

Here’s the link to the Al comparability paper (it was a PDF but the website converted it for some reason, you can CTRL F ‘aluminium’ to find it): https://apps.dtic.mil/sti/citations/ADC001137
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[*] posted on 9-2-2024 at 10:08


Quote: Originally posted by dettoo456  
If your AgNTz is dissolving in aq NH3 then it might just be disassociating into something weird. It shouldn’t dissolve.

Maybe liq NH3 might dissolve it but even if the AgNTz is exposed to aq NH3, the most it might do is form an ammonia complex which would still be insoluble.

This is weird. I do not remember a single insoluble complex of ammonia and silver.

Quote: Originally posted by dettoo456  

Here’s the link to the Al comparability paper (it was a PDF but the website converted it for some reason, you can CTRL F ‘aluminium’ to find it): https://apps.dtic.mil/sti/citations/ADC001137

I find it in webarchive
https://ia801209.us.archive.org/31/items/DTIC_ADC001137/DTIC...
There is metod (c) in this papier: they prepare AgNTz in ammonia solution then add HNO3 to it precipitate.

Is corrosion reaction
Al+3AgNTZ=>Al(NTz)3+3Ag ?
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[*] posted on 9-2-2024 at 12:35


I think the precipitate forms immediately even in the basic solution and the HNO3 is just to balance pH though I might be wrong.
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[*] posted on 10-2-2024 at 01:47


It is known that the solubility of CuCl in an aqueous NaCl solution is several times higher than in pure water. Does it make sense to add NaCl before DBX-1 synthesis to obtain a more complete conversion of CuCl to CuNTz-1?
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[*] posted on 10-2-2024 at 06:15


I would think it likely that AgNTz dissolves in ammonia water, forming the soluble diammine silver complex. This happens with silver chloride. Adding the nitric acid would then bind ammonia as the non-complexing ammonium ion and therefore precipitate the AgNTz by releasing the silver ions from the complex.
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[*] posted on 10-2-2024 at 10:42


Ok, my apologies, I haven’t known the AgNTz to be soluble in anything in my experience but I haven’t tried to recrystallized in NH4OH before.

For me, the ‘crude’ product from metathesis w/ AgNO3 has always been pure enough and fine enough in particle size for any EM use. Though, large crystals of the AgNTz do sound interesting if they can somehow be made.
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[*] posted on 11-2-2024 at 11:18


Once again, I performed 5-ATZ diazoting with hot method, the solution was evaporated and extracted with acetone.
To verify the fullness of extraction, the remainder was acidified with acetic acid, then CuSO4*5H2O, NaCl and ascorbic acid were added and a reaction similar to the preparation of DBX-1 was carried out.
Quite a lot of light brown substance similar to the DBX-1 was distinguished. But the dried substance does not explode and does not burn. What could it be?
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[*] posted on 13-2-2024 at 15:22


Wow! The DBX-1 is oxidized by the oxygen of air into Cu(NTZ)2 and CuO?! Fuck!
Why isn’t any article talk about this problem?
I'm disappointed.

2. DBX-1 is soluble in water. Bad, but soluble. It does not settle all even at 10°C.

[Edited on 13-2-2024 by Etanol]
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[*] posted on 15-2-2024 at 00:26


upd...
Inaccuracy
The DBX-1 is soluble in solution after the reaction.
It is insoluble in distilled water. But it is hydrolyzed in boiling distilled water.
Hydrolysis proceeds faster in NaCl solution. DBX-1 is hydrolyzed completely within 2-3 hours in boiling NaCl solution into a black-green non-explosive solid substance.
foto: hydrolyzation product of DBX-1 in NaCl solution
DBX1hydr.png - 367kB

Water ammoia on air decomposes DBX-1 into black CuO and blue solution.
It seems DBX-1 is soluble in hot DMSO with partial decomposition.

Quote: Originally posted by dettoo456  

AgNTz IS NOT COMPATIBLE WITH ALUMINUM THOUGH!
[Edited on 8-2-2024 by dettoo456]

I read that nitrotetrazolates are reduced by Mg,Zn,Al into aminotetrazolates. I mix recrystallized AgNTZ, Al and dist water at room temperature but I did not see a sign of the reaction within 2 day. Maybe this reaction is very slow or requires impurities.

Is it true that BNCP loses NH3 during long storage in wet air?

[Edited on 16-2-2024 by Etanol]
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[*] posted on 16-2-2024 at 12:22


If you bring the flame to the (NH4)4[Cu(NT)6], does it fully detonate or is there microdetonation with partial spraying of the powder?

Has anyone prepared MTX-1?
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[*] posted on 16-2-2024 at 20:45


MTX-1 is fine. The prep is easy and gives good yield of product, it does stick on glassware though - during the synthesis.

It forms salts, but the pure MTX-1 on its own is weak, and the salts (Ag & NH4) don’t seem to perform much better.

I’d say it’s not worth your Aminoguanidine; 5-NTz or even 5-ATz complexes perform far better. Plus, MTX-1 doesn’t detonate reliably and has a low Tdecomp.
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[*] posted on 18-2-2024 at 07:33


Is diazodinitrophenol chemically compatible with AgNT? It attracts its low ignition temperature compared to AgNT.
And MTX-1 + AgNT?

[Edited on 18-2-2024 by Etanol]
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[*] posted on 19-2-2024 at 08:24


I read somewhere that tetrazene & MTX-1 are not compatible with AgNTz, though I don’t remember where (somewhere in some military report).

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.

AgNTz is fine on its own in a detonator. It’s relatively heat stable, storage stable, and its only main drawback is ESD sensitivity. You should want a detonator to be as insensitive as possible, until you send 250V or 1/4” fuse into it, that’s the point.
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[*] posted on 20-2-2024 at 13:02


Is it possible not to separate the 5-aminotetrazole from the reaction mixture, but immediately diazotize it into 5-nitrotetrazole?

aminoguanidine sulphate+H2SO4+NaNO2=>guanilazide
guanilazide+Na2CO3=(reflux)=>5-aminotetrazole
5-aminotetrazole+H2SO4+2NaNO2=>5-nitrotetrazole
5-nitrotetrazole+Na2CO3 or NH3 =>NaNT or NH4NT
in situ all

[Edited on 20-2-2024 by Etanol]
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[*] posted on 20-2-2024 at 13:57


Yes it’s possible but you’d be reacting a strongly diluted mixture of 5-ATz & Na2SO4 with nitrous acid and even more Na2SO4. Plus, you wouldn’t be able to quantify the yield of your 5-ATz yield to calculate req’d reactant amounts, unless you had a very expensive rxn monitoring setup.

The 5-ATz workup should cost too much in yield, and it’s pretty straightforward. If you are really concerned with yield, just dry out the solids from a 5-ATz synthesis and reflux in anhydrous EtOH for an hour or two to completely extract any available 5-ATz. In my experience though, the crystallization of 5-ATz is consistent enough to disregard a different extraction method.

Or just buy the 5-ATz. Thermo sells it at a pretty reasonable price.
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[*] posted on 20-2-2024 at 21:36


Quote: Originally posted by dettoo456  
Yes it’s possible but you’d be reacting a strongly diluted mixture of 5-ATz & Na2SO4 with nitrous acid and even more Na2SO4.

It's even good. In the diluted solution, the risk of detonation of diazotetrazole in the second stage is less.

Quote: Originally posted by dettoo456  
Plus, you wouldn’t be able to quantify the yield of your 5-ATz yield to calculate req’d reactant amounts, unless you had a very expensive rxn monitoring setup.

Is it important to determine the yield of 5-ATz? Then an excess of acid and NaNO2 is used to diazotation. I can determine the yield of the final product (5-NTz salt) after aceton extraction.
I am concerned about possible organic impurities after the first stage.

Quote: Originally posted by dettoo456  

If you are really concerned with yield, just dry out the solids from a 5-ATz synthesis and reflux in anhydrous EtOH for an hour or two to completely extract any available 5-ATz. In my experience though, the crystallization of 5-ATz is consistent enough to disregard a different extraction method.

Thanks

[Edited on 21-2-2024 by Etanol]
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