lead azide

[mongo blongo]

i have reciently made some lead azide. this is the only decent explosive i have the required chemicals for. i wish to do something else with it coz its a bit too unstable for my liking. i tryed to plastisize it with petrolium jelly but it diddent work verry well! i was wondering if anyone has any suggestions as to an alternitive plastizer or if anyone can think of doing something more interesting with it? oh yea one more thing when i leave the lead azide to dry it forms an outside layer which is brown! i dont think this is normal! does anyone know what is happening?

[CragHack]

what was your method for making lead azide?

------------------
"If you must, do it with intelligent people, at least they know how to talk to the cops."

[mongo blongo]

i used sodium azide and lead acitate
both dissolved in distilled water
then added to each other while in a hot water bath
a white ppt was formed (lead azide) and was then filtered out and left to dry

[a_bab]

The brown colour is normaly to lead azide especially if you dried at sun light. It is caused because of the lead azide decomposition to a lead oxide called litharge, but it takes place only in a very thin layer. Mine turns usualy in dirty yellow. It must be washed very well, and is preferable to keep it moist. Also, is recomended to use dextrine to avoid formation of big crystals, wich may explode spontaneously. It isn'n recomended to try to plasticise LA, as it isn't very powerfull. Is a very good primer though. In my dreams http://theforum.virtualave.net/ubb/smilies/smile.gif I usualy make batches of 10 grams, enough to take all my palm, but hapily I never had an accident involving lead azide. Beware because LA is very toxic (as all azidic salts, especially the most soluble ones like potassium or sodium azides).

-----------------------------
http://move.to/pyromania

[kingspaz]

i haven't had much luck plasticising primaries either. i think the reason is that a plasticiser slows the reaction rate of the explosive rendering it useless for its purpose - D to D transition. i think maybe nitrocellulose could be a possibility, similar to AP putty.

[mongo blongo]

thanhu evryone for your information ......nitrocellulose is a very good idea (because it is an energetic plastizer and could be made more powerfull with lead azide
and yes it does tend to form that brown layer when in sunlight...
i was also thinking maybey mineral oil may work as a plstizer because i think i could get a higher ammount of la in the mixture... i know la is not meant to be plastized but what the hell it is worth a try? thankue for your data ...all of u it has been a great help!!!!!!

------------------
i like blowing shit up

[mongo blongo]

because of the unstability of la is it wise to store it ? i have been told that in the transport of la they carry it in ethanol( to shorten the drying process?) is this a better way of storage or should it be kept wet?

[Bitter]

Just out of interest where did you get the sodium azide from, air bag inflators ?

[mongo blongo]

no it was from a laboratory

[mongo blongo]

if anyone makes lead azide it might be usefull to know (you might alredy know) that if you do happen to be affected by the accute toxicity of an azide salt (also hydrazide gas (very toxic) can be liberated when in dissolved into soloution(hydrazoic acid), espically sodium azide) that one of the only remidies is ethanol (like a glass of wiskey or something)
ethanol counteracts the brain swelling (LA also affects the nervous system though)
i know someone who has been poisoned when working with sodium azide (from the hydrazide gas from another reaction, not from the reaction with water)!! its nasty shit!!

[mongo blongo]

Just out of interest, i used Megalomania's method of making Lead Azide,(this was not easy) instead of my usual method (above).
The product was a definite crystalline substance. The product i get from my usual method is not crystalline, a powder, about the consistency of flour.
The two look very different!
From messing about with it i found that it is much more sensitive than my usual product!
So i was quite confused!
After a little bit of research, i found out that Lead azide can exist in two allotropic forms; the more stable alpha-form which is orthorhombic, and the beta-form, which is monoclinic. The beta-form had the tendacy to revert to the alpha-form when its crystals are added to a solution containing either the alpha-form crystals or a lead salt. The beta-form will revert to the alpha-form when left in at a temperature of aprox 160 degr. Celcius.

Does anyone know if this is what actually happened?

[wantsomfet]

You said it. If the two solutions are mixed very fast, the alpha-leadazide will form. Mixing slowly (described on Mega's page) yields the beta-form.
Urbanski also refers to BOWDEN & YOFFE, 1958. They say that the beta-form is not as sensitive as the alpha-form.
Leadazide crystals shouldn't exceed the size of 0,1mm to prevent explosions! So if you get a "crystal product" it probably won't be that good...

------------------
for best catfood visit:
kangaroooo.cjb.net (http://kangaroooo.cjb.net)

[cutefix]

There are some primer formulations that encourage the addition of fillers like tapioca starch to make some kind of separation of the explosive crystals.do you think its workable with lead azide in order to minimize the sensitivity variations from polymorphic variation of these material?

[mongo blongo]

I may be wrong but as far as I know it's not the distance between the crystals that makes it so dangerous but the crystal size because the crystals can easily dislocate and this will cause an explosion!
But yes, I think mixing it with tapioca starch would decrease the sensitivity but the particles should be as small as possible.
I find it ok to use it on it's own (but with a booster).

[cutefix]

I think I know the reason now why Lead azide is best used with lead stypnate,especially those primers that use dextrinated lead azide ,where even if the amount of the active ingredient is 95% it is insufficient to initiate the base charge.Having another initiator will enhance its performance.

[Kroways]

The reason why they add a small percent lead styphnate to lead azide is bad flammability of the latter. 100% lead azide is quite flammable, but dextrinated material is slightly hygroscopic and if it contains water(~1%) the ignitability goes down rapidly.
And generally, do not try to treat primary explosives like secondary. It is the main source of nasty accidents. To plasticise LA? Bad idea at all - the preparation include friction of very sensitive stuff and the resulting putty is weak, if not dangerous.

[pete]

Were is it possible two get sodium azide from, never seen it personally?

[mongo blongo]

Yes lead styphnate is added to make the Lead azide more sensitive to heat, thus more reliable to initiation from an ignitor wire!
Sodium Azide is almost impossible to get (I was very lucky to get it from a lab)
It can be found in the explosive charge for car air bags!
I have no idea on how much u will get from it but that's the only way i can think of!
U could make it but it is very very difficult!!!!

[cutefix]

Somehow this initiating combination was reliable,and stable if compared with HMTD or Triacetone triperoxide composition which does not have good shelf life compared to the lead azide/styphnate tandem.The only drawback ,I think is difficulty of procuring the precursors for the latter combinations.Indeed I had difficulty in obtaining it also.I was thinking of synthesizing it this way:By reaction of Nitrous Oxide and Hot Sodium Amide-
N2O + NaNH2 => NaN3 + H20
Has anybody done this procedure in the Lab?Does it make good results?
The commercial procedure I think use hydrazine hydrate,which use a different procedure and is more complicated. Check this :
http://www.nrdcindia.com/pages/sodaz.htm


[This message has been edited by cutefix (edited July 29, 2001).]

[This message has been edited by cutefix (edited July 29, 2001).]

[cutefix]

I was also thinking about lead styphnate,somehow Mega,s file did not include the procedure for styphnic acid.(2,4,6 trinitroresorcinol) before being neutralized by a magnesium salt to obtain magnesium styphnate.Because of similarity with phenol but with one more hydroxyl group, resorcinol should be sulfonated first then nitrated to get the final product trinitroresorcinol.What do you think?
So that the tandem can be completed(the combination of lead azide and lead styphnate).by reaction of lead acetate and magnesium styphnate to form the lead styphnate prior to the preparation of the required blends of suitable initiating composition.

[mongo blongo]

For synthesizing Sodium Azide i would go with the reaction N2O + NaNH2 => NaN3 + H20
rather than the commercial procedure with hydrazine hydrate,whichis more complicated.

[PHILOU Zrealone]

NH2-NH2 + butylnitrite + NaOH diluted smooth refluxboiling on water bath.
NH2-NH2-CO-R or like + HCl diluted+ NaNO2 smooth refluxboiling on water bath.
You only need Hydrazine.
While with the sodium amidure process you have to dissolve sodium in liquid NH3 (-33C bp)and add liquid N2O in it (-80C bp) then allow to heat until ambiant temp! A lot of NH3 is evolved.And you have only NaN3 + ice+ NH4OH + NH4N3
If you have acces to Na, liq NH3 and liq N2O OK fine do it in a wel ventilated area.

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Mr Cool]

Dry ice is easy to find and has a temperature of about -79.5*C IIRC. This will liquefy ammonia easily, and if you did it in a closed container then you could bubble in N2O and the increased pressure would cause this to liquefy also. Sodium metal can be bought from chem suppliers or made easily. So this method is a possibility.
But I think the other method (alcohol nitrite + N2H4 + NaOH) would be better. It's only drawback is the toxicity of hydrazine, but this would be comparable with the clouds of ammonia gas in the first reaction.

Does anyone have a synthesis for resorcinol? It is easy to nitrate (same as phenol), but I can't find any sources for it.

[cutefix]

Why not start with sodium amide instead if this material can be commercially obtained,then it will simplify the process?Hydrazine is also a good material to start with,in another process,but I will rather save that to make binary explosives from it, as long as its water content is tolerable....

[Fingerless]

I'm surprised anyone can find Hydrazine. WHere do you get it? Its a strong carcinogen as well as a toxin I believe?

[cutefix]

Hydrazine is not difficult to obtain except the anhydrous one (diamine).I can obtain it from chemical supplier as hydrate.There is a procedure for making it somewhere in this HE section.Indeed it is a dangerous chemical , however excitement about doing experiments with it makes me forget that,and I also exercise more care in handling it.Binary explosives made with it produces virtually no flame and smoke.,.When I made my last explosion with astrolite .Somebody reported the blast to the cops,but they can’t pin anybody who did it besides it did no harm to anybody and they couldn’t find any trace of the main explosive, except remnants of the fuse.,and metal pieces from the blasting cap…

[mongo blongo]

Hi guys I gave up trying to plasticise Lead Azide and yesterday I thought to give it another go using different plasticising agents.
I have succeeded! http://theforum.virtualave.net/ubb/smilies/smile.gif
I tried both motor oil and vegetable oil and there is not much difference between them.
It can be easily be initiated with a simple safety fuse! (no bcap needed!!) http://theforum.virtualave.net/ubb/smilies/smile.gif
The power of it is about the same as straight Lead Azide and it's a little less sensitive!(from observations)
I made a ball the size of a pea and stuck it to the face of a smurf that I found in a cereal packet. For the first split second when the fuse reached the explosive I could hear a small crackling sound. It then it detonated, and well lets say that the smurf no longer has a torso! http://theforum.virtualave.net/ubb/smilies/biggrin.gif
This could also be used as a bodiless detonator.
If anyone is interested I will post ratios next time i make some.
I have no idea on storability yet.
Improvements?
I think it may be necessary to add lecithin to inhibit the formation of large crystals which would especially dangerous with the nature of large Lead Azide crystals.
Maybe mixing in some Lead styphnate to make it a bit more flame sensitive.
What do you guys think?


------------------
I dig explosives
Explosives dig me.....
one day a nice hole 6 ft under.

[Trinitrotoluene]

I was wondering is there a way to prevent the formation of large crystals without using dexterin? I have heard that using dexterin may cause some problems with the final product like if stored under water the bacteria living off the dexterin will cause it to form more senistive azides. Another drawback is dexterin is hard to dry and hygroscopic.So it would make it harder to detonate it under a flame. So any thought?

[mongo blongo]

You are meant to wash the LA very well to get rid of the dextrin. It would be nice though to explore other possibilities. Maybe gelatin?

[bonnsgeo]

hello world !

i just did a search with "dextrin" i didnt found anything. :(

What is precisely dextrin ? i know its not so far from corn flour (its an sugar , same formula) but how do you make dextrin ?? :confused:

thx
bye. :D

[zaibatsu]

Check <a href="http://www.geocities.com/thejuiceuk/dextrin.html" target="_blank">J's page</a> on the subject of dextrin.

[Machiavelli]

Hello bonnsgeo!

I just did a search with "dextrin" on google.com and it gave me ~17500 results, the explanation of what dextrin is was among the first ten and when searched for "+dextrin +make" I got 2 preparations among the first 3 hits.

You might want to practice your searching a bit <img border="0" title="" alt="[Wink]" src="wink.gif" />

<small>[ January 23, 2003, 01:37 PM: Message edited by: Machiavelli ]</small>

[nbk2000]

Anyone who uses the 'net for more than IM or AOhelL chatrooms NEEDS good search skills.

When searching for something pyro related, search here first. Most likely, it's already been discussed to death, you just need to find it.

If you can't find it here, then a Google search will most likely uncover it, but you need to know HOW to find things. A broad vocabulary, logical thinking, relational association, and the ability to construct a proper query, are all very neccessary.

I fear, though, that the lack of librarial skills being taught to the current generation, is going to come back to bite us in the ass. How many of todays youngsters would know how to do a card stack search at a library? Computers are a poor substitute for the use of your own "supercomputer" (the human brain).

[stanfield]

What are the stoechiometric proportions (or the new equation) to use with lead acetate ? I usually make LA with lead nitrate and I would like to change because of the pH problem...

thanx !

[PEROMAN]

Is it so difficult to count ?
The reaction is 2NaN3 + Pb(CH3COO)2 = Pb(N3)2 + 2CH3COONa
You need 130g NaN3 per 325g of lead acetate
Use not concentrated solutions ! (no more then 10%)

[stanfield]

To count what ?
I know NO equation on lead azide ! Even the one with lead nitrate !
so, please, apologize my stupidity... And don't be agressive like this, it's very unpleasant !

[PEROMAN]

... Maybe i dont understand you because i'm silly , or i dont know english enough .

The reaction is:
Pb(CH3COO)2 + 2NaN3 = Pb(N3)2 + 2CH3COONa
For getting 1 mole of lead azide(291gr = 207 + 6*14) , you need :
2 moles of sonium azide ( 130g = 2*(23 + 3*14) ) and
1 mole of lead acetate . I think you have not unhydrous salt ,
but Pb(CH3COO)2*3H2O (379g = 207 + (12 + 3 + 12 + 16*2)*2 + 3*18)

Dissolve 13 grams of sodium azide in about 150ml of water(better distilled) ,
dissolve 37.9gr of lead acetate in about 150ml of water(better distilled).
and them mix the solutions. Some people advice to keep the mix in a hot bath for few hours
You should get about 25-29gr of lead azide
Attention! Some peoble say that mixing the solutions can be dangerous!

Did you learn chemistry at school ?
What are the formulas of lead azide , lead acetate , sodium azide?
What is "periodic tabble of elements?" , what is "molar mass " ?

[PEROMAN]

Sorry .. instead of written "and them mix " you should read
"and then mix"

You don't need to make a new post to make minor corrections to a post, you can use the "edit" feature to change the original post.

<small>[ February 03, 2003, 07:22 PM: Message edited by: Anthony ]</small>

[stanfield]

I needed this fucking equation to calculate ! WITHOUT this equation, it's hard to make calculations !
You understood ? I just need this new equation and now I know it, thanx.

Ofcourse I learnt chemistry at school, but I've learnt too it's difficult to calculate something without an equation...

[PEROMAN]

Remember ! Probobly you have Pb(CH3COO)2*3H2O (not unhydrous)!
so the equatiun is
Pb(CH3COO)2*3H2O + 2NaN3 = Pb(N3)2 + 2CH3COONa + 3H2O

[bonnsgeo]

hmmm ...
i just want to answer : 1) i did a search on google but i didnt find anything cause i did it very quickly.
2) And i think its better there is a question/answer on this forum for all the persons after me who will want to make dextrin.

and ..oh yes : i have just made some lead azide ...and i'm deaf ! what a sh*t !! <img border="0" title="" alt="[Wink]" src="wink.gif" />
more seriously there is still some LA on my filter in a shape of "sheet" or "plate" (i used my dictionnary sorry) , do you think i can break this sheets in security ?

bye
bonnsgeo

[stanfield]

yes, I have Pb(CH3COO)2,3H2O but water is a byproduct so, it's not a problem ? Am I right ?

bonnsgeo : ofcourse you can ! I usually do it at hand with gloves very slowy !
Yeah, this explosive is very good but it forms "lump" when dry... That's a problem. Maybe the industry have an anti-caking agent ?

thanx :)

[PEROMAN]

Yes , water is not a problem .. you just should take 379g of
Pb(CH3COO)2*3H2O instead of 325g of Pb(CH3COO)2 per 130g of sodium azide

[stanfield]

yeah, that's what I thought...

What about my idea of "anti-caking agent" ? it sounds interesting...
How can we stop LA from caking ?

[bonnsgeo]

when you make LA do u obtain a powder or a big cake of La ?

how do u proceed to reduce your LA in powder ?

thx

[Mr Cool]

It is produced as a powder, which may cake together. To uncake it all you have to do is very gently crush the lumps (crush, not grind or scrape).
This is one potential benefit that silver azide has; it can be recrystalised from ammonia into coarser crystals, which do not cake as much. I did this for a while, but then decided against it because it seems to me that there might be a risk of producing fulminating silver, which is very sensitive indeed. Also, occaisionally a few larger crystals (the largest that I saw must have been almost 3mm long) could be seen in the finished product which I didn't like.

[bonnsgeo]

ok.

i had this idea to put directly the LA (not completely dry) in a detonator , and let it dry inside the detonator.

it s easy to place in because its a paste and its safer because it s wet ...

do u think it s a good idea?

bye
thx

[Mr Cool]

It would work, but might not be as good as drying it first and then pressing it.

1) You will either need to put the wet LA on top of your fuse/igniter, which could harm it, or on top of your base charge, which could possibly cause problems.
2) It will take a long time to dry when enclosed in a small space.
3) After drying it will not be at the highest possible density, because as the water evapourates it will leave air spaces behind.

Also, I think I should clarify something. When I said it's best to crush the lumps, you must avoid actually crushing the crystals if you see what I mean. You're just trying to break up the clumps, and should try to avoid putting any significant force on the actual crystals.

And you may remember that I was looking for a way to destroy silver azide a while ago... I've found that the best method is simply to put it into 5% NaOCl bleach and leave it overnight.

2 AgN₃ + NaOCl --&gt; Ag₂O + NaCl + 3 N₂

You need to leave it overnight because the Ag₂O coats the AgN₃, slowing the reaction.
Then the Ag₂O can be recycled back into AgNO₃.

[bonnsgeo]

cool ... thx u for the reaction of destruction of silver azide.... is it working for lead ?

2 other questions:

1) do you have a "device" (a "machine") to press your LA in detonator in safety ?

2) i know that LA is better than AP (more powerful and safer) if we consider the temperature but about friction and shock ...is it safer ?

the problem of this *shit* of LA is that explode even it s not confined.

[Mr Cool]

I haven't tried using bleach to destroy LA yet, because I only wanted to get rid of the SA because of the large crystals in it, and the possibility of fulminating silver.
But I'm sure it would work with LA too if you ever needed to do it. It's oxidising the azide ion, which is the same in both cases.
Edit: to my surprise, SA is also very soluble in sodium thiosulphate solution. I'm not sure if it could be recovered from it, there was no sign of a reaction and I can't think of one that might take place, but you never know...

"1) do you have a "device" (a "machine") to press your LA in detonator in safety ?"

Personally, at the moment I'm using nothing more technical than a long wooden stick and a big block of polystyrene to press detonators. And big safety glasses, ear defenders and thick gloves.
MHN is my base charge, which seems to press to a high density without very great pressures, so I have no need for a machine with levers etc to get the pressure.

"2) i know that LA is better than AP (more powerful and safer) if we consider the temperature but about friction and shock ...is it safer?"

IIRC LA is slightly more sensitive, but it depends greatly on crystal size. I'll try to dig up some figures for you.

<small>[ February 10, 2003, 04:45 PM: Message edited by: Mr Cool ]</small>

[stanfield]

During the production, some of you advised me not to use a magnetic stirrer, ok, I understand why, but couldn't this be possible a very low "velocity" (dunno how to say) ? Teflon (PTFE), has a very low "friction coefficient" (again, are they the correct words ?)

My second question, all patent on Lead Azide relate that the addition must be done between 70°C and 90°C, why ? I always done LA at room temperature and it works pretty well...

thanx !

[Hystrix]

Mr. Cool: i'm afraid that treating of azide with hypochlorite can produce very dangerous chloroazide ClN3. Are you sure your method is safe? AFAIK for LA destruction this reaction is employed:
2Pb(N3)2 + 6HNO3 + 2NaNO2 --&gt; 2Pb(NO3)2 + 2NaNO3 + N2O + 3H2O + 6N2
(nitrite is added to prevent HN3 formation).

PEROMAN: </font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> Did you learn chemistry at school ? etc. etc.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I didn't think you can be so angry, Labean :D

[Mr Cool]

2 AgN₃ + 2 NaOCl + H₂O --&gt; 2 ClN₃ + Ag₂O + 2 NaOH
??
Hmm... I never considered that. Thanks for the warning!
I haven't died yet, but maybe I should change my method! D'oh! And it was so nice and simple! <img border="0" title="" alt="[Frown]" src="frown.gif" />

[VasiaPupkin]

By the way LA from Pb(NO3)2 is some safer than Pb(CH3COO)2 LA at the whole (Sure in same conditions).
Many scientist's has this observation. Interesting, what is the nature of this appearance?!

Methods with Pb-acetate is not used now. Maybe for this cause.
You can use some additives for dextrine to improve colloidal ability.
For example Na- tartrate, oxalate or ferrocyanide.
In England there was a some LA sort with gelatine using instead dextrine...

__________________________________________________ ____________________
all patent on Lead Azide relate that the addition must be done between 70°C and 90°C, why?
__________________________________________________ ____________________

- Its one of the ways to prevent beta-LA impurity forming.

[bonnsgeo]

hi all !

lot of questions :

1)could u finish the equations for me please :
H2O + NaN3 =&gt; ??
H2O + PB(NO3)2 =&gt; ??

its not so difficult but i found different equations on Internet so i d like to be sure.

2) what is the pH of the solution of NaN3 (i found it s around 9 with a concentration of 3 %..is it right ?)
3) what is the pH of the solution of Pb(NO3)2 (around 3 or 4 IIRC)
4) what is the action of dextrin in the reaction ? is it a pH regulator ? or is it just a phlegmatizer for LA ? (i know it s usefull for the alpha form appears)

5)... hmm.. i forgot it .. ..it was about a patent for LA wich use sodium citrate ... i ll search.

thx
bye

<small>[ February 12, 2003, 08:54 AM: Message edited by: bonnsgeo ]</small>

[VasiaPupkin]

I have found info that acetate presence tend to crystal structure distortion of LA.
Therefore LA from Pb(CH3COO)2 more dangerous and more tend to explode when crystallized.

little of answers: :)

1) 8% Pb(NO3)2 solution (10-15% molar excess)
5% dextrine sol-n (~0.2% when all solutions are mixed)
3% NaN3 sol-n
Be sure concentralions may be different... a little.
To prepare 1kg LA they use 0.45kg NaN3, 1.40 kg Pb(NO3)2,
0.041kg dextrine and 0.02 kg NaOH.
I think its not so difficult to calculate water amount? <img border="0" title="" alt="[Wink]" src="wink.gif" />

2) NaN3 solution is always a little basic pH.
3) I know only that desirable pH of Pb(NO3)2/dextrine is ~7 (neutral). ~8%Pb(NO3)2 sol-n usually has pH 4.2-4.4 for hydrolysis. And they use a small amount of NaOH to make pH=7. I think the better choise to add NaOH into NaN3 solution. But its not so important... This measure only to prevent HN3 forming - its forming may be dangerous in industry, but not so dangerous when you operate with small quantities.
4) Colloidal dextrine particles adsorb LA microcrystalls and make it spheoidal and very small. Its only prevent of dangerous large and needle crystall forming. But dextrine addition dont effect on alpha or beta-LA relative yeild. Take in mind that large alpha crystalls is also very dangerous.

Dextrine is sure has own little phlegmatize action. At the same time dextrinated LA has a good pouring. - Its a very important property because industry use not mass but volume dosing in detonators.
Nowadays they use polyvinyl spirit and Na-salt of carboxymethylcellylose instead of dextrine. Because dextrinated LA is hydroscopic and has some lower initial properties than Na-CMC LA.

[bonnsgeo]

ok thx u.

today i have made LA (with dextrin at 70 degrés). perfect...but the only problem is that at the bottom of my erlenmeyer some LA stay. How can i remove it ?

i need a solvent..but what ?

i have put in some water for avoid all risk of explosion.... but i really would like to clean my erlen...could u give me advice please ?

thx
bye

EDIT: shit ...my LA was in the solution (it was all white like milk) but when i tried to filter the liquid did nt want to go down (a little liquid passed through the filter but it was white too)... the LA stay with the water.
how can i extract the LA without a buchner ?

last time i did LA without heating ..the crystals went on the bottom and i hadnt any problem to filter it ...

why it did nt work this time ?
thx

<small>[ February 13, 2003, 11:55 AM: Message edited by: bonnsgeo ]</small>

[stanfield]

Hey, bonns, do you use my magnetic stirrer for LA synthesis ?
If yes, I guess you never had a problem... otherwise, you couldn't be there today <img border="0" title="" alt="[Wink]" src="wink.gif" />

[bonnsgeo]

hmm ...
no i didnt use your magnetic stirrer !! i m not stupid ! for LA <img border="0" title="" alt="[Wink]" src="wink.gif" /> i love life !

but i dont know why i could nt filtered it.

bye

[stanfield]

I'm pretty sure that a magnetic stirrer could be used with a low "velocity" as I said earlier. Teflon has a low coefficient friction...

[Microtek]

Maybe you should do an experiment:
Put a little ( 0.01 g ) lead azide into a cheap mortar or other container along with 50 mL water. Then grind the LA with a pestle or similar instrument, starting with gentle mixing, then moving on to more harsh strokes. If you get a detonation at any point, I wouldn't use a magnetic stirrer.
If you really want to stir it with something else than hand-power, it must be easy to construct a container that can rotate at a slight angle to vertical ( like a cement mixer ).

[Mr Cool]

You could rig up a propeller-style stirrer, using a drill with variable speed control in a clamp above your reaction vessel, and use that to stir your reaction with a bent piece of plastic or something. It wouldn't be as efficient as a prop., but it should work just as well as a mag stirrer.

[bonnsgeo]

somebody can explain me why my LA stayed in suspension in water and never settle ?

and why my LA solution wich passed through the filter stayed white ? (the LA was so litlle particles that the filter didnt stop it ????????!)

bye

<small>[ February 14, 2003, 01:28 PM: Message edited by: bonnsgeo ]</small>

[Anthony]

If the suspension is passing through your filter paper, you could try using multiple layers of filter paper, if a finer one isn't available to you.

[Hystrix]

bonnsgeo: perhaps that's colloidal solution (you could reach it if one of reactives was in surplus). You can preciptate your LA if you'll add the second reactive to solution (for example, you have lead salt in surplus so you need to add NaN3 solution to colloid)

<small>[ February 14, 2003, 04:55 PM: Message edited by: Hystrix ]</small>

[Scorpion]

Hi there!!

After 5 years having my Lead Azide keeped closed in plastic containers and away from any kind of light, I found many grams of it the other day inside a cardboard box. So, I decided to try its strenght after all this time taking a very few miligrams and putting them on a metal spoon in direct fire!!! Almost instantaneously it made a big BANG and no traces of it were left on the spoon!!
So I must conclude that the substance seems to keep very well over the years and it is really stable. I just found a very little part having the brown-yellow layer because of the light it must have caught the first time when I prepared the substance in 1998.

I think the key to preserve the substance is keeping it in a cool dark place and if possible wet with ethyl alcohol so it does not crystalize itself nor letting any bactery decompose LA.

[rooster]

I have recently aquired some chemicals for making LA. However, I haven't got a normal, soluble lead salt. What I have is called "basic lead acetate", and the formula is Pb(CH3COO)2*H2O2. I suppose it will be soluble in water, but will the H2O2 trapped inside the crystal structure interfere with the reaction? I thought that I might get out Lead Peroxide? Or will I just get the Pb(N3)2?

Also, Is it possible to use a Pb(4+) salt to make LA? Like Lead tetraazide?

[Mr Cool]

Pb(4+) isn't as stable as Pb(2+), so if you did get some to form then it might be quite dangerous... I've been wondering about using N3(-) as a ligand in complex salts, it might work. Something like (NH4)2[Cu(N3)4], although I'm not entirely happy about NH4(+) with N3(-), --> NH3 + HN3.

If I were you rooster, I'd ppte Pb(OH)2 using your lead compound and NaOH (assuming that what you have is soluble in water), collect and wash that, and then dissolve it in nitric acid to make a lead nitrate solution. You will have to crystalise that out and recrystalise it to remove acid traces befoe use.

[rooster]

Sure kingspaz - that would work.
But what i have is a pure lead compound, with almost no impurities(analytical grade). My nitric is only 62%, most of the rest is water, but there is probably some other stuff too. I would not like having for example 0,1% copper azide in my LA. Just to be on the safe side, you know.

Also, I heard someone saying that Lead Acetate is preferable in front of Lead Nitrate. The nitrate made the soln. more acidic or something (I thought it was the acetate that made the soln. basic?). Which is best? I will do some tests...

EDIT: I tested the lead salt, it didn't dissolve in water. Hell, it didn't even dissolve in 60% nitrric acid! What the fuck is wrong? My PbO doesn't want to dissolve in the same nitric either. Do I have to heat it on a boiling water bath?

[Kerrupt]

<- *Dreams of 70 something grams of sodium azide in his lab*

I have lead acetate also, but i want more, i have some pure lead, can that be reacted with glacial acetic acid to form lead acetate?

[vulture]

I think you need slightly diluted GAA, because pure will cause passivation IIRC.
Anyways, it's going to take a while to react.
I would advise using a stronger acid.

[Mr Cool]

I'm sure it'd work if you're not in a hurry. Just cut up the lead into little bits and chuck it into some strong acetic acid for a while.

I happen to have a rather huge block of lead, and I was thinking about making some more lead nitrate. BUT, I am not sure of the purity of the lead, and if I was making azide I'd want to be very sure that I didn't have any other metal azides in it, just in case. The lead was removed from a very old, bulky computer or some other big electronic thing. I'm not sure, I wasn't the one who removed it. It was basically ballast to stop this big, top-heavy piece of equipment from falling over. So, although I am sure that it was not alloyed with anything deliberately, it also seems likely that they would not have bothered to purify it very much.

So, any ideas on lead purification? I was thinking about dissolving it in nitric acid, ppting PbCl2 (since most other chlorides are more soluble), and then maybe electrolysis of a PbCl2 melt. What do you think?

[Kerrupt]

I think the insoluable salt idea (PbCl2) would work great as long as there aren't any other heavy metals that form insoluable salts you should be ok. You might want to check the density for shits and giggles.

So the lead + acetic acid should work? I imagine increasing surface area of the lead would speed up the process but i do have plenty of lab grade lead acetate at the moment so i have time to spare. I don't think lead purity for me is an issue :) The source has taken care to only possess the purist of lead for neutron stops :)

[The_Rsert]

Would this work for preparation/synthesis of lead azide?
http://www.infernolabs.co.uk/filehost/Synthesis_of_azides_without_hydrazine.gif
http://www.infernolabs.co.uk/filehost/file-list.php?dir=&file=Synthesis_of_azides_without_hydrazine.gif&PHPSESSID=b330e212daea7ae480c5f1a58739631f
Mirror: http://www.infernolabs.co.uk/filehost/Synthesis_of_azides_without_hydrazine.gif

[nbk2000]

Fusing nitrate and urea at 150&deg;-200&deg; results in an azide salt? Hmmm....

BTW, you have to copy/paste the links to see the files.

[The_Rsert]

Yes!?
In a little chemistry book "Gefährliche Reaktionen" (English="Dangerous reactions") it said, that urea can react with nitrates to produce toxic azides.

I think sodium azide will be only produced as a byproduct.
But it can purified by making HN3, which can destilled at about 50°C.
I have not tried it yet. They said, that it will react with nitrate. Maybe it will work only with ammonium nitrate!? Or another nitrate?!

It the book it also said, that the power of AP can increased by mixing it with potassium permangante (losing of stability). And some other interesting things...

Maybe I can get another look in the book (it's not my book, I found the on my "intership" at a lab (I hope it's the right word) at a lunch break; they have some interesting chemicals in the lab, heheheeeee: nicotine, benzoyl peroxide,...)

[Myrol]

The_Rsert, have you tested the reaction for his usefulness? It sounds very intresting for me because I just love Lead Azide, especially as a Primary!

I saw some time ago an Explosion of 30g Lead Azide (Brainiac) where they attached the charge to the feet of a fibre-glass puppet.

I don't cheat you but the puppet was entirely destroyed and even a short flame was visible wich wasn't ever usually to me!

The synthesis (if it works) had to be improved a little, I would never purify my Sodium Azide via adding a diluted acid to produce Hydroazoic Acid. That could be a fatal error, Hydroazoic Acid is a little more toxic than Hydrogen Cyanide! Only a little but it's true! Not to mention the huge explosion risk of pure gaseus HN3.

So I thought: let the Urea and the NaONO2 react (I would prefer at 150°C for a little more time as at 200°C really short because Urea decomposes at 150°C not to much but at 200°C a lot!) and dilute it with some organic solvents wich are able to extract especially Urea and his derivates (Biuret and some cyclic's etc.), dissolve all organics out and let the crude Azide dry. Dissolve it in Water and filter all impurties with a normal coffeefilter out. Add some Dextrin, and then precipipate your Lead Azide wich should be nicely pure if you DON't crystallize ALL PB(N3)2 out. 90% total should be enough. Main impurties like Lead Nitrate, Sodium Nitrate etc. stay in the solution wich will be easily filtered off to give a nice pure Azide.

I'll test this method after it's gettin' a little warmer here. Actually it snow's in Germany and we have -6°C outside....my poor hotplate isn't prepared for such conditions :p so I have to wait!

[The_Rsert]

Myrol, I have also seen the explosion of 30g lead azide on the German TV-Show "VIVA-Brainiac".

I'm not sure with the synthesis... maybe only a decomposition product of urea will react with the NaNO3 to sodium azide...(?)
Or maybe there's another nitrate (for example NH4NO3) needed for the reaction.
All what I know is that in the little German book "Gefährliche Reaktionen" (English="Dangerous reactions") it is written that nitrate can react with urea to form toxical azide.
I don't know more about it. Maybe a catalyst, more heat, or something else is needed. Maybe small amounts of sodium hydroxide, HCL, or sodium nitrite are needed to form stable azide.
You can try it but be careful!

You can contact me at the_rsert@arcor.de

Don't forget: If you use any acids HN3 can be produced. HN3 is extremely dangerous! It is more poisoness than prussic acid!

[Sundried]

This is my first post outside of the Water Cooler...It's good to be here. I'm working on a small booster to initiate a small ANFO (Prilled, activated, AN, AL, and NM race fuel) charge.

I've searched around extensively and haven't found any info on compositions containing PbN6/KNO3. Will 10% Lead Azide be adequate to sensitize the KNO3 booster? I'm using a homemade pressed lead azide detonator in a plastic tube 15mm x 3mm.

Thanks,


"It is not answers you seek, rather more questions."

[Sundried]

This is my first post outside of the Water Cooler...It's good to be here. I'm working on a small booster to initiate a small ANFO (Prilled, activated, AN, AL, and NM race fuel) charge.

I've searched around extensively and haven't found any info on compositions containing PbN6/KNO3. Will 10% Lead Azide be adequate to sensitize the KNO3 booster? I'm using a homemade pressed lead azide detonator in a plastic tube 15mm x 3mm.

Thanks,


"It is not answers you seek, rather more questions."

[Sundried]

This is my first post outside of the Water Cooler...It's good to be here. I'm working on a small booster to initiate a small ANFO (Prilled, activated, AN, AL, and NM race fuel) charge.

I've searched around extensively and haven't found any info on compositions containing PbN6/KNO3. Will 10% Lead Azide be adequate to sensitize the KNO3 booster? I'm using a homemade pressed lead azide detonator in a plastic tube 15mm x 3mm.

Thanks,


"It is not answers you seek, rather more questions."

[Myrol]

Hello to all! Umm, because I wanna order some chemicals over the University I've made a practice (very long ago) in and trough this I have really good connections to the Professor there (Master of the Martin-Luther University for Catalyst Chemistry) I asked him if I can order some Sodium Azide (500g) for my "own" experiments.

Well, he know what I do with Sodium Azide and he also know the risks with that stuff. But he trusts me and know that I dont do serious shit with Explosives or generally with Chemistry.

Now, I have to give him "some Reasons" why I need Sodium Azide.

He want to see some good preferable Scientific Videos of Lead Azide going off and some pictures wich effects Lead Azide do on Target X etc.

I searched a while via googling but ended up with almost nothing. If somebody of you have a good Video or pictures that I could show him, please let me know this. 500g NaN3 is a lot. But I would say my problem with good Detonators is then solved.

[Myrol]

Hello to all! Umm, because I wanna order some chemicals over the University I've made a practice (very long ago) in and trough this I have really good connections to the Professor there (Master of the Martin-Luther University for Catalyst Chemistry) I asked him if I can order some Sodium Azide (500g) for my "own" experiments.

Well, he know what I do with Sodium Azide and he also know the risks with that stuff. But he trusts me and know that I dont do serious shit with Explosives or generally with Chemistry.

Now, I have to give him "some Reasons" why I need Sodium Azide.

He want to see some good preferable Scientific Videos of Lead Azide going off and some pictures wich effects Lead Azide do on Target X etc.

I searched a while via googling but ended up with almost nothing. If somebody of you have a good Video or pictures that I could show him, please let me know this. 500g NaN3 is a lot. But I would say my problem with good Detonators is then solved.

[Myrol]

Hello to all! Umm, because I wanna order some chemicals over the University I've made a practice (very long ago) in and trough this I have really good connections to the Professor there (Master of the Martin-Luther University for Catalyst Chemistry) I asked him if I can order some Sodium Azide (500g) for my "own" experiments.

Well, he know what I do with Sodium Azide and he also know the risks with that stuff. But he trusts me and know that I dont do serious shit with Explosives or generally with Chemistry.

Now, I have to give him "some Reasons" why I need Sodium Azide.

He want to see some good preferable Scientific Videos of Lead Azide going off and some pictures wich effects Lead Azide do on Target X etc.

I searched a while via googling but ended up with almost nothing. If somebody of you have a good Video or pictures that I could show him, please let me know this. 500g NaN3 is a lot. But I would say my problem with good Detonators is then solved.

[The_Rsert]

Another Idea for Myrol:

Mix sodium hypochlorite with urea in destilled water to get hydrazine.
Take some sodium nitrite and add some HCL (7%) in steuchometric amounts to get HNO2.
Mix it together with a big excess of the hydrazine solution.
Some HN3 should be formed which could be destilled under vakuum!?
Right? Does it work?

Look at the attachment....

[The_Rsert]

Another Idea for Myrol:

Mix sodium hypochlorite with urea in destilled water to get hydrazine.
Take some sodium nitrite and add some HCL (7%) in steuchometric amounts to get HNO2.
Mix it together with a big excess of the hydrazine solution.
Some HN3 should be formed which could be destilled under vakuum!?
Right? Does it work?

Look at the attachment....

[The_Rsert]

Another Idea for Myrol:

Mix sodium hypochlorite with urea in destilled water to get hydrazine.
Take some sodium nitrite and add some HCL (7%) in steuchometric amounts to get HNO2.
Mix it together with a big excess of the hydrazine solution.
Some HN3 should be formed which could be destilled under vakuum!?
Right? Does it work?

Look at the attachment....

[VasiaPupkin]

:eek: Distilling of HN3 is a very,very dangerous process. My friend was carefull but got a hospital when trying to distill HN3 from water solution. It may explode without causes when keeping. And this thing is so toxic that 1-2 breath of its fumes is enough to fall on floor. I would be carry out reactions without HN3 forming.

[VasiaPupkin]

:eek: Distilling of HN3 is a very,very dangerous process. My friend was carefull but got a hospital when trying to distill HN3 from water solution. It may explode without causes when keeping. And this thing is so toxic that 1-2 breath of its fumes is enough to fall on floor. I would be carry out reactions without HN3 forming.

[VasiaPupkin]

:eek: Distilling of HN3 is a very,very dangerous process. My friend was carefull but got a hospital when trying to distill HN3 from water solution. It may explode without causes when keeping. And this thing is so toxic that 1-2 breath of its fumes is enough to fall on floor. I would be carry out reactions without HN3 forming.