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Ral123
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Lead azide synthesis
Here's how I see a generic azide synth. A lot of people ask me and I decided to make a video:
http://www.youtube.com/watch?v=xRGJdbenK1c
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chemcam
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Wow, that seems very straight forward and simple. I have yet to experiment with any azides, I am hesitant to do a hydrazine synthesis without a
stronger fume hood.
I would like to compliment you on your overhead stirring apparatus, It would seem to me that we both are very mechanically inclined people. That
talent seems to be declining, most homemade things I have seen lately look like something from a horror film that will fail just by looking at it. I
wish people would take the time to properly design and build what they need rather than buying from a large corporation. Everyone will be coming to us
when some disaster happens and no stores are available.
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Ral123
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Wow, thanks. Addition of the solution drop by drop takes quite a while. Manual stir will make your hand hurt and you can hit the wall or bottom of the
vessel. For micro experimentation lead azide is great. For big AN based charges all azide can offer is marginal safety.
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chemcam
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Yeah all my energetic experiments are small scale so this would be ideal. I just need to further educate myself with hydrazine.
The overhead stirring device I made looks similar to yours but it mounts on my metal ring stand pole. I took a 12" 5mm glass tube and made it into an
upside down T, sealed the ends and attached the other end to the motor shaft. I wired it to a variable resistor so I can control the speed.
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Ral123
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These polypropylene pudding cups can withstand nitrating mixture. I've made MN and NG in these. It feels quite safe.
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Finnnicus
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Love the video. You are incredibly shakey though! Use a longer splint for comfort purposes 
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Ral123
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Imagine if I had to do the synth. in glass and stir manually 
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Fantasma4500
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can lead azide go off by just striking a tiny wet particle in between plastic??
also to solve this for ppl without such fancy gear a erlenmeyer flask might come in handy, filling it less than half for easier swirling ^^
swirling a erlenmeyer flask is the feeling of science. (=
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Ral123
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Not that it's likely, but if a small plastic cup with azide synth. explodes and you are with safety glasses you wont be hurt at all. It wont even be
loud. The glass however can be nasty. AP feels kinda stable when is drowned in water. Azide is known to be quite potent and sensitive, even when wet.
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Bot0nist
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Your right about using the thin plastic reaction vessels when you can. I used small, HDPE test tubes when I made M.E.K.P. and other sensitive
primaries, when it was possible.
Yes, the plastic can still fragment and produce shrapnel, but it is of much less density, so it travles slower and less distance. A rigged up blast
shield or fumehood curtian is a great idea. Or a face shield. At the very leas, goggles.
You took into account the extreme toxicity of the sodium azide as well, I assume.
Nice video. Thanks Ral.
edit: spelling.
I am sorry to everyone for the spelling as of late from me. My only connected device at the moment is a crappy "blackberry, style cheap phone. The
buttons are tiny, my thumbs large and insensitive and weathered from manual labor. The browser also lack a spellchecker or auto correct feature, and
the built in predictive text feature is so difficult to work that it ends up making things worse, when coupled with the prevously mentioned thumb
hinderance. And, I am just a terrible speller, and have been known to abuse commas, also. I will try and upgrade soon.
[Edited on 22-4-2013 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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Motherload
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Sorry to bring up an old thread but ..... This the most relevant place to ask.
I recently acquired 500 gms of NaN3 but the shitty part is I had spent sooo
much time making Hydrazine Sulfate and after making about 200 gms of it I had the opportunity to buy the NaN3 but regardless I want to make some
Pb(N3)2 now.
Would it be dangerous to mix dilute solutions of Azide and Nitrate and dextrin in a polypropylene beaker with a Teflon coated stir bar ?
Would there be a possibility of detonation from friction ?
I do notice the the stir bar typically pushes the sediment outward and away from its centre.
Ral123 I see you use a overhead mixer.
"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
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Ral123
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According to the literature the stir bar is very inadvisable as water doesn't desensitize LA that much.
My NaN3 was more then 50 years old, I guess if pure, yours can wait too.
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Trinitrophenol
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Hey anyone know about azides (sodium/lead azide) compatibility with stainless steel?
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Dany
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Lead azide is compatible with stainless stell.
here's a quote from [1]:
"...It is therefore necessary to prevent lead azide coming into contact with copper in its applications. Aluminum, stainless
steel, tin, and lead do not react with lead azide even in presence of water. The preferred material for applications containing LA is
therefore aluminum."
Reference:
[1] Robert Matyas & Jiri Pachman, Primary Explosives (Springer 2013)
Dany.
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Ral123
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Does copper case offer any advantage over brittle aluminium or thin stainless steel? Only that it looks old school.
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Dany
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Ral123, what do you mean by this question? what advantage?
Dany.
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Ral123
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The brittle aluminum will provide a little faster shock wave and allow the hot gases to contact the main material, unlike the copper witch may
balloon.
Also if we try to set off anfo: Imagine these 1000m/s+ fast hot pulverised aluminum particles in the centre of your charge.
The only advantage of copper I can see is it's less reactive toward some things and it can be shaped and soldered.
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Dany
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Quote: Originally posted by Ral123  | The brittle aluminum will provide a little faster shock wave and allow the hot gases to contact the main material, unlike the copper witch may
balloon.
Also if we try to set off anfo: Imagine these 1000m/s+ fast hot pulverised aluminum particles in the centre of your charge.
The only advantage of copper I can see is it's less reactive toward some things and it can be shaped and soldered. |
What is the connection between the incompressible story that you are telling me and the subject of the thread???
Dany.
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PHILOU Zrealone
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| Quote: Originally posted by Dany | | Quote: Originally posted by Ral123 |
Does copper case offer any advantage over brittle aluminium or thin stainless steel? Only that it looks old school.
The brittle aluminum will provide a little faster shock wave and allow the hot gases to contact the main material, unlike the copper witch may
balloon.
Also if we try to set off anfo: Imagine these 1000m/s+ fast hot pulverised aluminum particles in the centre of your charge.
The only advantage of copper I can see is it's less reactive toward some things and it can be shaped and soldered.
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What is the connection between the incompressible story that you are telling me and the subject of the thread???
Dany. |
He apparently tries to give his 50 cents on your data.
But he misses the point that copper is not compatible with lead azide.
Copper can be "cooked" and becomes then harder than aluminium at equivalent thickness (it becomes also much more brittle). Stainless steel is even
harder. Usually when one tends to push the VOD/density of the primary, he needs the stronger material. So stainless steel > hard copper > soft
copper > lead; and iron > glass > hard plastic > paper > rubber.
Here I think that in your reference they go for aluminium over stainless steel because of price reasons.
@Ral123,
The statement that Copper will "inflate like a balloon" is not possible at the speed, overpressure and heat of the detonic process inside the cap...it
will be fragmented or reduced to copper dust.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Trinitrophenol
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Thanks a lot for you answer Dany! Very much appreciated 
But when you make lead (II) azide do you need commercial/pyro grade dextrin or would just home baked corn starch do the job?
After my experience homemade dextrin won´t dissolve that easily in water and might not dissolve completely.
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Motherload
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Also, I have seen glucose refered to as dextrin. Normally as dextrose.
So the " impurity " we add in to prevent the crystals from getting to big ..... Is it regular corn starch ? I can't seem to find any starches labeled
dextrin.
I am going to buy one of those cheapo personal coffee/drink whisks and turn down the rpm and use to stir.
"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
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Ral123
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In my experiments adding very little sugar reduces the size of the crystals. It also makes the product much less flame sensitive. I don't know if it's
because it attracts water.
@PHILOU Zrealone
Why would case hardness matter so much for the velocity. My foil(bad idea) and straw detonators work fine. May be case hardness contributes to DDT and
case weight and density to velocity.
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Bert
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| Quote: Originally posted by Motherload | Also, I have seen glucose refered to as dextrin. Normally as dextrose.
So the " impurity " we add in to prevent the crystals from getting to big ..... Is it regular corn starch ? I can't seem to find any starches labeled
dextrin. |
Dextrin can be made FROM corn starch, by roasting it carefully with frequent stirring in your kitchen oven.
Or you could toast some bread, scrape off the brown surface, and dissolve the dextrin in water. Filter the water and dry the filtrate to recover
dextrin.
Wichita buggy whip-Dextrin procedure
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PHILOU Zrealone
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| Quote: Originally posted by Ral123 | In my experiments adding very little sugar reduces the size of the crystals. It also makes the product much less flame sensitive. I don't know if it's
because it attracts water.
@PHILOU Zrealone
Why would case hardness matter so much for the velocity. My foil(bad idea) and straw detonators work fine. May be case hardness contributes to DDT and
case weight and density to velocity. |
Suggar catch indeed more water from the air than dextrin would; in moist weather your Lead di-azide will be harder to ignite.
Hardness matters apparently.
For a given explosive material, at an equivalent density and internal diameter; tubes of different materials do detonate at different VOD. So the
casing is important.
With a harder casing, you can press harder (for primaries that allow this) and increase the weight of primary per volume (thus the density).
Hardness (non deformability) of the casing increases the shockwave confinement, but explanation is probably also partly due to the speed of sound
propagation into the casing material (?)... there seems to be a correlation between this and the VOD as a function of the casing material.
Speed of sound into materials
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Dany
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| Quote: Originally posted by PHILOU Zrealone | Hardness matters apparently.
For a given explosive material, at an equivalent density and internal diameter; tubes of different materials do detonate at different VOD. So the
casing is important.
With a harder casing, you can press harder (for primaries that allow this) and increase the weight of primary per volume (thus the density).
Hardness (non deformability) of the casing increases the shockwave confinement, but explanation is probably also partly due to the speed of sound
propagation into the casing material (?)... there seems to be a correlation between this and the VOD as a function of the casing material.
Speed of sound into materials |
A heavily confined explosives is equivalent to a large diameter charge and as detonation velocity depend on charge diameter a harder confinement will
help the achievement of maximum detonation velocity at the density of the explosive under test. The sound speed of the casing has no effect unless in
some cases like a liquid explosive detonated with a weak iniator or a liquid explosive which detonate near its critical diameter. The sound speed of
the casing play a role in what is called low velocity detonation for more on this read this old comment and reference therein. For more on detonation initiation and parameter affecting this initiation read this report.
Dany.
[Edited on 6-5-2014 by Dany]
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