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Author: Subject: Lead azide synthesis
NeonPulse
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[*] posted on 24-6-2014 at 22:50


I was just curious to know a little more on the sensitivity of lead azide and have a couple of questions about it.
I have synthesized this compound a few times now and each time has produced great results and it is a brilliant primary explosive.
the synthesis i used was as follows:
2.33g sodium azide dissolved in to 70ml dist water, and 6.9g lead nitrate+ 0.35g dextrin in 90ml dist water in another plastic beaker.
3 or 4 drops of a 10% sodium hydroxide solution added to the lead nitrate sol to raise the PH to 5.
I then heated the nitrate sol on a hot water bath to 63c and stir while dropwise adding the azide solution to the nitrate/dextrin solution. immediate precipitation of the desired product was apparent.
taking around 10-15mins to complete the addition, the mix was removed form the water bath and allowed to cool to room temp with continued stirring. it was then filtered, washed and dried. Yeild was 5g probably a tiny bit more as some small losses from the filtering and crystals deposited on the walls of the beaker, which i was NOT going to attempt to scrape off...

The only differences with this latest synthesis was the stirring. I made an electric overhead stirrer similar to what Ral123 made. Its very efficient. the last times were stirred by hand. Could this stirring have made a product even less flame sensitive than hand stirring?
The reason i ask is this particular batch doesn't seem to want to detonate in small piles lit with a flame splint. It only ignites very quickly like mercury fulminate with a small pop and flash even with piles around 100mg (not weighed- just guessing). With a previous synthesis it was able to DDT in small amounts detonating violently. this latest batch will detonate but only with confinement, a solid whack with a hammer or a small amount heated in foil. I knew lead azide to not be particularly flame sensitive but not to the point it wont detonate in a small pile. is this normal behaviour for lead azide?



Hmmm, I see. Simple mistake. I did mean increase, and not really paying attention to detail. if I took the time to proof read my post before posting I wouldn't have made that mistake.oops.

[Edited on 25-6-2014 by NeonPulse]




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[*] posted on 25-6-2014 at 06:27


Quote: Originally posted by NeonPulse  

3 or 4 drops of a 10% sodium hydroxide solution added to the lead nitrate sol to reduce the PH to 5.


Adding bases increases pH.




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[*] posted on 15-7-2014 at 19:45


People have used sugar to reduce crystal size in LA synths .... Can glucose be used ... Is it critical ?
Glucose isn't as deliquescent and I have lots.




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[*] posted on 14-8-2014 at 08:41


Quote: Originally posted by Motherload  
People have used sugar to reduce crystal size in LA synths.


Is it necessary to do this, or can I just handle the LA after with a normal crystal size?
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[*] posted on 14-8-2014 at 08:54


Quote: Originally posted by Energetic Einstein  
Quote: Originally posted by Motherload  
People have used sugar to reduce crystal size in LA synths.


Is it necessary to do this, or can I just handle the LA after with a normal crystal size?


Is this related to the use of dextrin in LA (dextrinated lead azide)?
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[*] posted on 14-8-2014 at 13:54


Quote: Originally posted by Loptr  
Is this related to the use of dextrin in LA (dextrinated lead azide)?


Yes it is.

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[*] posted on 15-9-2014 at 15:35


Hello Nerds!

I've made Lead Azide several times with a supply of Sodium Azide that I've had for quite some time; however, my Sodium Azide supply is running low. Therefore, I've been trying to synthesis Sodium Azide from Hydrazine Sulfate; Isopropyl nitrite; and sodium hydroxide. Unfortunately I can't quite seem to get the end product (some documents refer using ethyl nitrite instead, but I think either will work please correct me if I am wrong). The documentation is not entirely clear, but the reaction doesn't seem to work or go to completion. I also know its possible to make Lead Azide directly from the Hydrazine Sulfate, but I'm not sure if I feel comfortable making it directly, but at this point I would be happy with any successful product.
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[*] posted on 15-9-2014 at 17:35


Please describe the procedure you use in more detail. In my experience, you need to prepare hydrazine hydrate (be careful!) before reacting it with the isopropyl nitrite and sodium hydroxide.

[Edited on 16-9-2014 by Cheddite Cheese]




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[*] posted on 23-9-2014 at 17:54


As a general question, how do you all feel about the toxicity of the azide family? I've read a couple precautions about it so I'm appropriately concerned. I know most all EM are toxic but there is a difference between the liver toxicity of TNT and the pulmonary edema of NOx. While I'm not planning to eat it, what sorts of behaviors are peculiar in handling these materials and the hydrazine precursors?
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[*] posted on 23-9-2014 at 22:04


Quote: Originally posted by roXefeller  
As a general question, how do you all feel about the toxicity of the azide family?


Similar to my feelings about the cyanide family?

Plus the whole primary explosive issue...

If you ingest, or expose azides to an acidic environment without a proper air handling scheme/respiratory protection in place... Expect to stop breathing soon after. Add to this an alarming tendency for random explosions of Hydrazoic acid, vapors of same and various materials exposed to these.

[Edited on 24-9-2014 by Bert]




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[*] posted on 25-9-2014 at 13:49


It says the video is private for me; link?



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[*] posted on 28-9-2014 at 12:18


I'm very sorry for the video, I assure you it's value is almost entirely entertainment. Some TV has used material from the channel, let's say for their own frame of things :/
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