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Author: Subject: 5-ATZ(5-Aminotetrazole), the nitrotetrazolate ion and friends
MineMan
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[*] posted on 19-12-2018 at 21:52


Why so much love for DBX-1? It’s VOD is high, it’s lead free but is it not still pretty sensitive?
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snooby
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[*] posted on 20-12-2018 at 03:25


https://www.researchgate.net/publication/288871303_Recent_Ad...

This article include some detailed info about impurities in raw nantz.
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[*] posted on 29-6-2019 at 10:03


Quote: Originally posted by MineMan  
Why so much love for DBX-1? It’s VOD is high, it’s lead free but is it not still pretty sensitive?


Yeah, I agree. I have made some of the nitrotetrazole salts, silver(AgNTz), copper(DBX-1), and Sodium(NaNTz). I have even made the Nickel salt from NaNTz. The Nickel looks very similar to NHN in color but will not separate out into a fine powder when suction filtered.

They are all very sensitive with NaNTz being the exception. NaNTz can't be used by itself in the Dihydtare form, it's too difficult to set off.

The nitrotetrazole salts are more stable and less reactive then Lead Azide but just as sensitive. So for those companies who use LA, DBX-1 is a direct replacement, and no machinery changes are necessary. For the rest of us, they still don't offer any advantage over primaries like NHN and are more expensive to manufacture.
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wessonsmith
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[*] posted on 29-6-2019 at 10:11


Quote: Originally posted by snooby  
https://www.researchgate.net/publication/288871303_Recent_Ad...

This article includes some detailed info about impurities in raw NaNTz.


This doesn't apply to those who are manufacturing NaNTz using the 2017 Batch Method patent.
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Microtek
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[*] posted on 29-6-2019 at 10:55


I have experimented with the complexes in the "Green primaries" paper (transition metal complexes with nitrotetrazole amine and water). They are about equivalent with NHN in sensitivity and power, but makes DDT more reliably.
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Mychemlife
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[*] posted on 21-7-2019 at 09:09


Has anyone ever crystalized out any Na,(NTZ)

Screenshot_20190720-213531.png - 1.1MB
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snooby
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[*] posted on 4-11-2019 at 09:47


Since there are sooo many synths about nant, what is your favoriete? The facile methode give me a very yellow end product. Still kt works, but not like this: https://youtu.be/U-1bNouTHhQ

My solution Just turns green.
Edit: i usde this one: https://patents.google.com/patent/US9598380B2/en

I notice a lot of red Times, no maybe to fast addition rate waht explanins the color.

[Edited on 4-11-2019 by snooby]
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fusso
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[*] posted on 4-11-2019 at 10:47


Great crystals!!!



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snooby
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[*] posted on 4-11-2019 at 11:00


Whats your method of maling the nantz and het the clear crystals?
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B.D.E
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[*] posted on 14-3-2020 at 13:39


nevermind, please delete.
apologies.

[Edited on 14-3-2020 by B.D.E]
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Etanol
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[*] posted on 13-4-2020 at 13:04


How to prepare the NH4-nitrotetrazole from Na-nitrotertazole?
Na-NTz+H2SO4=>NTz ?
NTz+NH3 (water)=>NH4NTz ?
Is exist the short way?
I wish green primaryes)
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[*] posted on 21-4-2020 at 08:00


Quote: Originally posted by Mychemlife  
Has anyone ever crystalized out any Na,(NTZ)


Sure have. But via recrystallising crude product in minimal Water first and second from Acetone. The greenish tint was replaced by Snow White colour.
These crystals you have look very nice and quite well formed. Nice job.




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there is a way.

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B(a)P
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[*] posted on 18-5-2020 at 16:21


Yesterday I conducted a synthesis of 5-ATZ. I have done this reaction 3 other times, always following the Engager method, starting with aminoguanidine bicarbonate, presented earlier in this thread. The only way I deviate from Engagers write up is to add sodium carbonate until my solution is at pH 5.5 rather than adding the exact mass presented in the paper. Each time my yield of 5-ATZ has been around 70 to 80% based on aminoguanidine bicarbonate.
This time the changes in colour that I noted on my previous attempts did not quite match up. I also needed less sodium carbonate than I had previously used. I didn't question this as much as I should have.
At the completion of reflux I adjusted the pH to 3 and left the solution to cool.
After cooling no product was visible, which is normal given 5-ATZ readily produces supersaturated solutions. I tried agitating, but this did not work. I drew off 3 mls and warmed it on an evaporating dish to produce a seed crystal then inserted that into the main solution. After about 8 hours a small mass of needle like crystals precipitated. At this point I stopped and reviewed what I had done. I reviewed my notes and other than the differences mentioned above I couldn't see where I had gone wrong. I tried checking my pH and my meter was toast. I checked it with indicator paper and found it to be at around 1! It seems my pH meter was on its last legs during the synthesis and so I likely refluxed at a less than optimal pH. The crystallisation would also have occurred at a pH that was sub-optimal, though I understand this is not so critical as the pH for the reflux.
My question is what have I ended up with? I have done some research and can't find much on side products that might dominate at lower temperates. Yield is very low. My crystalline product is transparent, colourless and needle like to 10 mm in length. For scale the stir bar is 25 mm in length. The melting point of the product seems about right for 5-ATZ and it decomposes at about the right temperature in a way I would expect it to. My thoughts are a very low yield and as a result the product has crystallised very slowly. Does anyone have any resources that go into depth on the side reactions that occur for this reaction? Thanks in advance for any assistance!

5ATZ_2.jpg - 2.6MB 5ATZ_1.jpg - 1.8MB
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B(a)P
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[*] posted on 19-9-2020 at 01:36


Cadmium nitrotetrazole
0.5 g of cadmium was dissolved in 1.5 g of 70 percent HNO3 and a little dH2O
The cadmium nitrate was added to a solution of 0.5 g of nitrotetrazole in 2 ml dH2O.
A white precipitate of cadmium nitrotetrazole (CdNTZ) formed immediately with a slight exotherm.
On drying the precipitate shrunk in size considerably.
The CdNTZ was readily soluble in water.
CdNTZ is slightly friction sensitive and moderately impact sensitive.
CdNTZ is sensitive to direct and indirect heating and donates before melting in amounts almost too small to see.
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pdb
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[*] posted on 6-5-2021 at 23:01
Question about NaNT purification


I refer to "Facile method for preparation of NaNT" (US9,598,380). It works well and is indeed very easy. But I am intrigued by the 1:2 molar ratio of 5-AT to NaNO2: this means that if one mole of Na gives NaNT, another mole of Na goes into the solution and pollutes it. But in what form? NaNO3, or an excess of NaNO2, or what else? We should know this before trying to find a method to purify NaNT. Does anyone know how to write the reaction between 5-AT, NaNO2 and HNO3?


[Edited on 7-5-21 by pdb]
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pdb
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[*] posted on 11-5-2021 at 05:30
Advice from someone who has successfully prepared crystalline DBX-1


I have prepared DBX-1 according to Fronabarger twice, with similar results. I have no doubt about the nature of the product, which deflagrates on contact with flame and detonates on heat or under light confinement. On the other hand, I observe that the product, when dried on a filter, appears as lumps, which leave a fine sticky dust on the finger when touched. Under the microscope, this powder appears amorphous. Moreover, its density is low, and even under high pressure it is difficult to reduce its volume: for the same weight, it is 4 to 5 times more voluminous when pressed than AgN3 for example. Also, I wonder if I missed the crystallisation step: according to Fronabarger, at about one third of the addition of the ascorbate, the product starts to precipitate and the solution takes on a rusty colour within a few minutes. I have observed these changes, but still my DBX-1 appears amorphous, and in this form I do not see how it could replace Pb(N3)2 according to the drop-in replacement principle.

Also, I would be interested in having someone who has obtained DBX-1 in crystalline form look at the attached photos to tell me if any differ from their own experience. Thank you!

(sorry, the pictures are in reverse order)
(the microscope pics are 1 mm in lenth)



DBX-1 1.jpg - 43kB DBX-1 2.jpg - 38kB 20210510_120622.jpg - 604kB 20210507_190039.jpg - 535kB 20210510_151550.jpg - 323kB 20210507_165210.jpg - 333kB 20210507_163520.jpg - 337kB 20210507_161754.jpg - 357kB 20210507_160910.jpg - 373kB 20210507_160643.jpg - 448kB

[Edited on 11-5-21 by pdb]
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DBX Labs
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[*] posted on 21-5-2021 at 14:39


From my experience making DBX-1, I'll get a near identical amorphous brown sludge most every time I run from scratch. The sludge dries into chunks just like yours that are flame sensitive and detonate when confined and heated. However, I have never been able to get this first product to detonate confined with a fuse, even as a powder.
What I've found and and have yet to publish in a video is that when I've taken a small amount (~2-3 grams) of this amorphous product and fed it into a repeated synthesis from scratch, the impure DBX-1 present in the first product catalyzes the formation of much more visible DBX-1 crystals that are red rather than brown. Additionally, it appears much less gelatinous sludge remains intermixed with the product in this case.
Hope this helps.




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pdb
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[*] posted on 22-5-2021 at 06:18


Quote: Originally posted by DBX Labs  
the impure DBX-1 present in the first product catalyzes the formation of much more visible DBX-1 crystals that are red rather than brown. Additionally, it appears much less gelatinous sludge remains intermixed with the product in this case.


This effect is reported by Ford (from line 46). I'll give it a try myself.



Attachment: 2015 DBX-1-Ford.pdf (929kB)
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