Lead Azide

[stanfield]

Ok, I just received 100 g of Soium Azide 99% and I would like to make some Lead Azide (ofcourse !)

Firstly, when you're adding the 2 solutions (of sodium azide and lead nitrate), can I use a magnetic stirrer (low stirring...) or will I detonate some crystals ?

Secondly, why are they so many differences between these two pages :
<a href="http://edetonator.hyperlink.cz/Azidy.htm" target="_blank">http://edetonator.hyperlink.cz/Azidy.htm</a>
<a href="http://roguesci.org/megalomania/explo/lead_azide.html" target="_blank">http://roguesci.org/megalomania/explo/lead_azide.html</a>

Will the "Czech" method work efficiently ? Megalomania preconizes a slow adding instead of the czech who add the solution in one time !
Furthermore, Mega introduce sodium hydroxide in his synthesis and the szech no ! what the pH do in this reaction ?

plz, give me your opinion before loosing my fingers ! :)

a big thanx...

<small>[ June 15, 2002, 10:50 AM: Message edited by: stanfield ]</small>

[mongo blongo]

The best method I have ever tried is adding a solution of warm conc Lead Acitate to a conc solution of Sodium Azide. You can also use Lead Nitrate but it's very poisonous. I think NaOH is added to prevent hydrazide gas (VERY toxic) being evolved from NaN3 solution. I have never had this problem.
You add dextrin to make the crystal size small (less sensitive) but in the method that I use I get a very fine ppt of crystals so I don't use dextrin.

[Phoenix]

well just make a solution of sodium azid + a few drops of NaOH
and a second solution of lead salt (no mater what ) calculate how much you need to get a complete reaktion
AND NEVER FOGET DEXTRIN to the lead solution
then pour the 2 solutions together and i wthite priticipate will fall out filter and dry and thats it the best and most easy to make initiating explosiv :)
dont care for heatign the solution it dont make any differences as far as i observed
and remember that both leadsalts and sodiumazid are highly toxic

[mongo blongo]

I add excess Lead Acitate untill Lead Azide stops precibitating. I use warm soloutions because it's quicker to filter.

[stanfield]

The czech page use 14%-15% excess of Pb(NO3)2, as well as megalomania if I remember correctly...

Could a magnetic stirrer be used ?

thanx !

[mongo blongo]

A magnetic stirer? It would work but it could be dangerous! From my experiences I would not recomend it!

[inferno]

Err, i can never get to any of the edetonator sites! It always says either "You are unauthorized to view this page" or "page cannot be displayed" - its really annoying as ive seen many links to it

Im not very experienced but you would probably be better not to use a magnetic stirrer to be on the safe side. "Always err on the side of caution"

[stanfield]

ok, this will be "manual strirrer" :)

Could it be pressed in a cap ? I ask this 'cause I really don't like this idea...

see ya !

[stanfield]

ok, I just made Lead azide ! this is filtering...
I made a mix of megalomania's and the czech's method...
An observation : Pb(NO3)2 is a bitch to dissolve in water ! it took me 10 min !

When your adding the solution of sodium azide, the solution of lead nitrate become milky... I felt no toxic gas were produced by the reaction but I had my mask and maybe the NaOH destroyed them...

During the strirring, I touched many times to beaker and nothing happened so it isn't as sensitive as mega and the czech said...

When the filtering will be done, could it be dried at direct sunlight ? And, how could I "unstick" it from the filter paper without blowing up my face ? usually, I scrape the paper to unstick the filtrate but this explosives is "very sensitive to shock and friction", so, what's the tips ?

thanx !

[nbk2000]

Turn the filter paper upside down over a plate and use a squirt bottle to spray distilled water through the filter paper and on the azide. This will dislodge the precipitate.

Don't dry in direct sunlight! Just use a fan or warm air.

[stanfield]

MUHAHAHAHAHA !!! I just tested out a little wet portion of lead azide : the sound was impresive for the amount there was !!! I think I ignited 1 mg of lead azide, this made the "bang" of a middle firecracker ! impresive !

Thanx NBK !

see ya !

[Microtek]

I think a bit of perspective is needed here. Lead azide is used commercially and militarily and while it may be very sensitive, it is nowhere near as sensitive as acetone peroxide or some of the other primaries that have been used here. My point is that I don't think you need to be overly concerned.
BTW, I strongly recommend that you compress the lead azide when making detonators; that way you will need far less primary and once the pressing is done, you will have a safer detonator.

[stanfield]

ok but if it's as sensitive as aceton peroxyde, this will be a hard task, no ? this frighten me a bit... sorry !

[stanfield]

maybe is there way to desensibilize this explosive ?

[kingspaz]

stanfield he said it is NOT as sensitive as acentone peroxide :)
if you are unsure then press it slightly damp to reduce friction sensitivity.

[stanfield]

oups, you'r right...

What's the composition of a military Bcap ?

[mongo blongo]

Stanfield- Good stuff isn't it! :)
In military Bcap the Lead Azide is mixed with a bit of Lead Styphnate to give it better flame sensitivity. About 5% AL powder is also added to increase it's initiation ability. This is usually used with PETN as a booster.
I can't see much danger with drying it in sunlight but it will then form some PbO in a very thin layer around the Lead Azide. I dry mine with the filter paper on some tissue on a hot water bottle.

[stanfield]

I will soon receive some Mg, could it be substitued to Al ?
Lead styphnate is harder to make...shit !

I don't understand why must I press the Lead azide to be a safe detonator ?, by vibrations or something like that who may occurs in the transport, this will "unpress" it, no ?

thanx !

[Anthony]

A pressed cap will be safer because it will contain less explosive than an unpressed cap to do the same job. Unpressed is less efficient so you need more explosive. A pressed cap is not necessarily safer because it is less sensitive, but because it doesn't contain much explosive, if it does go off, it can only do limited damage.

A question of my own: how bad is the problem of low flame sensitivity of LA? Would a thin layer of BP or other ignition mixture pressed onto the LA ensure ignition?

[a_bab]

It would for sure. Though there might be some chances to get a dull blasting cap. From my experience, if you heat the LA slowly in a teaspoon, it'll turn yellow due to it's decomposition (in litharge- the lead will get oxydized by the air) and it won't detonate. The yellow color is a characteristic of LA; it'll occure especially if the LA is exposed to light, in a very thin layer.

It's also very insensitive to hit. Actually, it'll be unusefull in a primer. And is moderatly sensitive to fricition (rubbing), but only between hard surfaces (metal, rock). Is by far the most unsensitive primer I know. I heard about the "internal stress in crystals", but I never had problems with that (yet :( )

I don't think that it could be dangerous to take the LA out of the filter paper; it stiks very well though. But is is throughly dryed it should be easy to remove it.

[mongo blongo]

I never have any problems with it's flame sensitivity.I am using pure chems though.

[Microtek]

If worried about flame sensitivity, a thin layer of double salts is useful. Lead styphnate synthesis is indeed causing me a lot of grief at the moment; the styphnic acid is not difficult to make from resorcinol but converting it to its lead salt just won't work. I've had the same problem when making lead picrate, I wonder why.
Anyway, pressing both the base charge and the primary will improve safety both because of the smaller amount of explosive, but more substancially because the solid pellet of primary does not leave room for the crystals to rub against each other either when subjected to impact or when shaken.

[stanfield]

ok, I just separated lead azide from filter paper and I didn't loose a finger :) ! so it isn't as sensible to friction like that... but I was prudent !

But I have a little problem, the lead azide powder is "glued" so I have big pieces of lead azide, how to make a fine powder ?
hehehe, I don't want to test with a mixer... muhahahaha !

thanx !

[da man]

Did you add dextrin to the solution? If you don't add dextrin to the solution the lead azide forms large crystals which can be very sensitive and dangerous, because of inner tension i think? So you should always add dextrin!

[stanfield]

Don't worry, I added (homemade) dextrin...
The lead azide is "caking"... and he's not as sensitive as you said so I think I don't have very large crystals...

[Microtek]

I know what you mean. Lots of things aglomerate in this manner when drying on the filter paper. If I'm dealing with a sensitive substance, I usually use a razor blade to divide the mass to finer particles. It should preferably be done when damp, but using a very sharp instrument minimizes the risk of explosion.

[xoo1246]

I would dampen it again, then remove it. I wouldn't like to have small pieces of razor blade in my face, use shielding.

[Mr Cool]

If you can make silver azide, then I strongly recommend that you do. Not only is it more powerful, but it can also be made in a form which does not stick together in a big clump. Instead it is a free-flowing powder.
IIRC, the process involved adding NaN3 soln to a soln of AgNO3 in conc. NH3 (aq). This I suppose formed diaminesilver azide, which was ppted as the NH3 was driven off by heating. I think there's a patent about it in the knowledge section.

[mongo blongo]

Yes I also posted the patent in a thread "Silver Azide" a while back.

[stanfield]

I got a last question :
when you're finishing to filter the lead azide cristals, what's the liquid in the receiving flask ? I'm vey worried when I throw away this liquid in the sink...
If, it's dangerous to environement, how could I neutralize this liquid ?

thanx !

[mongo blongo]

Sodium Nitrate if you are using Lead Nitrate.

Edit: I just realized that I use Lead Acetate so I will end up with Sodium Acetate which can be used to make Glacial Acetic acid.
Also you can use your NaNO3 to make HNO3.
Of course you will have to evaporate the soloutions first. Waste not want not. :)

<small>[ June 24, 2002, 10:55 AM: Message edited by: mongo blongo ]</small>

[stanfield]

ok, thanx ! so, this isn't bad for environment ! even good since sodium nitrate is a fertilizer :)
It will be hard to make HNO3 whit so little sodium nitrate ! Further more, I can legaly buy sodium nitrate in garden store so : no problemo ! :)

see ya !

What's the equation for the reaction ? I saw it somwhere but can't remember...

<small>[ June 24, 2002, 01:07 PM: Message edited by: stanfield ]</small>

[mongo blongo]

It could be harmfull if you used an excess of any of the precursors! You could have a bit of Lead Nitrate or Sodium Azide left which are both very toxic!

[stanfield]

shit, yes, I have 10-15% excess of lead nitrate but when I throw this liquid in the sink, I add lot of water too...

<small>[ June 24, 2002, 04:06 PM: Message edited by: stanfield ]</small>

[mongo blongo]

When I filter, the filtrate goes directly into a soda bottle. Then I dilute it with more water (just incase) and chuck it in the bin. Let the dustmen deal with it. :D
I use Lead Acetate (excess) so there is no cause for concern really.

<small>[ June 24, 2002, 08:34 PM: Message edited by: mongo blongo ]</small>

[stanfield]

Lead acetate isn't as toxic as lead nitrate ?
otherwise, is there a way to neutralize the lead nitrate solution ?

[Polverone]

There are many lead salts of low solubility. Convert your leftover nitrate to one of them. Add HCl to get lead chloride, or Na2CO3 to get the carbonate. Then save them until such time as you could use them for something useful, or until you can dispose of them at a proper facilty.