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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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wessonsmith
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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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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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