nitroglycerin (Stranger)
05-26-03 15:31
No 435713
      sodium azide  Bookmark   

Sorry fucked up on the first post, didin't even know what a digest was. Anyways SWIM had found some supplyer in another country that sells sodium azide, SWIM wanted to order some. Do anyone think it will get past inspection? After 9-11 that had been a watched chemical.
 
 
 
 
    rudebwoy
(Hive Bee)
05-26-03 15:41
No 435715
      What do you think?  Bookmark   

"After 9-11 that had been a watched chemical"

What do you think?

If you don't have a valid reason then it won't.

Just work it baby!
 
 
 
 
    Nick_J
(Stranger)
05-27-03 04:07
No 435840
      It was fine for me.  Bookmark   

I got a multi-kilogram amount through (UK) customs after 11/09, and jackbooted thugs haven't kicked my door down and busted me, not even once.
I wasn't aware it had any uses for making candy though... I've tried reducing things with it but it only seems to reduce things that I would consider oxidisers, like hypochlorites. It doesn't reduce anything organic, as far as I'm aware. I suppose an azide group could itself be reduced to an amine though. I'll have to UTFSE about it...

I was a bit nervous about getting it due to its obvious use in many primary explosives, but to be honest, it's not as dodgy as you would think at first. Terrorists aren't going to be getting any sent over, since it's a lot less legally risky to make organic peroxides for their detonators, for example. And it's not a very common reactant in drug synthesis, it seems.
Basically, customs think that no-one who is doing anything illegal with it would be stupid enough to order any wink.

It's synthesis is easy though. Bleach and urea, or ammonia, are used to produce hydrazine, which is reacted with a nitrite ester and NaOH in alcoholic solution to ppte NaN3. A google search will give you a method to follow.

Edit: airbags are a good source too, if you can get any. Some Daewoo airbags that I had each contained ~100g, as brown disc-like pellets. The other constituents are iron oxide and silica. They can be crushed up under warm water (slightly basified, just in case...) and stirred to dissolve all the azide. Then let most of the sediment settle, and pour off the solution through a filter paper to yield practically pure sodium azide solution. Somewhere round here I have my notes, telling me what purity the azide pellets were... IIRC it was about 75%, I'll post the exact figure if I can find it.

Another edit: http://www.geocities.com/eawfuk/sodium_azide_from_airbag.htm
An illustrated guide on butchering an airbag. It is the same as the type that I got, although I did not write this. The pellets are insensitive to friction, but still, be careful with that saw...

"Simplicity is the ultimate sophistication."
 
 
 
 
    Barium
(Hive Addict)
05-27-03 04:50
No 435851
      Azides  Bookmark   

Yes azides are very useful in amine chemistry but you should know what you are doing before using them. Otherwise nasty things will most likely happen. Sodium azide is not at all explosive but it is a nasty poison if ingested. The azide ion from sodium azide is as unhealthy as the cyanide ion, if not even a bit more. Heavy metal azides and many organic azides on the other hand are, beside being very poisonus, a bit shock sensitive.

Freaky
 
 
 
 
    Nick_J
(Stranger)
05-27-03 08:00
No 435882
      Well...  Bookmark   

You are right that sodium azide is not explosive as such, but it can certainly decompose/burn rather vigorously when prompted to, making sodium oxide smoke, which ain't good...

As for toxicity, that is a very real danger. That is why I recommended to crush airbag pellets up under basified water, to avoid any dry dust (inhalation hazard) and also to avoid the possibility of hydrogen azide being formed, an explosive, toxic gas that'll kill you just as well as hydrogen cyanide.
Other than that, the only other very important thing is to remember not to mix it with any heavy metal salts or organic halides. Both can form sensitive/spontaneously explosive compounds. Also be careful when disposing of excess, it is probably a good idea to destry the azide ion before disposal.

"Simplicity is the ultimate sophistication."
 
 
 
 
    nitroglycerin
(Stranger)
05-27-03 21:07
No 436001
      well....  Bookmark   

swim had not atempted to go to a junkyard to ask for airbags. If they ask a question about it swim coulden't find a answer. So the problem is fear..
 
 
 
 
    blaaky
(Hive Bee)
05-28-03 17:57
No 436199
      one more thing....  Bookmark   

One more thing... I've used sodium azide to make Lead Azide, which is a shock/friction sensitive explosive.

DO NOT DUMP ANY sodium azide or solution containing sodium azide down your drain or toilet. If you have Lead (i hope not) or steel water pipes it can form explosive azide salts!!! bee safe!

-blaaky

If you want divine justice, die.
 
 
 
 
    nitroglycerin
(Stranger)
05-28-03 20:36
No 436228
      Chemical method toward NaN3  Bookmark   

The chemical method is too dangerous. 2NH3+NaOCl=N2H4+H2O+NaCl. Hydrazine is extreamly explosive when distilled to a high concentration in air it will EXPLODE! its also extreamly toxic. A few breaths of fumes will kill you, and in lower concentrations will give you cancer.Any advice on handleing hydrazine?
Yea the reaction N2H4+NaNO2=NaN3+2 H2O.
Also discussed in the E&W forum the NaN3 will react very slowly with lead to produce lead azide. You need lead acetate or lead nitrate to prepear NaN3 for a primary.
 
 
 
 
    ClearLight
(Hive Addict)
05-29-03 11:37
No 436380
      Lead azide warning!  Bookmark   

Lead Azide, unless prepared with an appropriate conditioning agent in the crystallization phase will produce shock sensitive crystals, that when large enough( hence conditioner) will spotaneously detonate due to crystal strain!

  Not a good idea..

Infinite Radiant Light - THKRA
 
 
 
 
    Nick_J
(Newbee)
05-29-03 13:15
No 436403
      Hydrazine.  Bookmark   

Hydrazine isn't too bad. Remember that you're goal is an azide... that's like complaining about the toxicity of carbon monoxide and chlorine if you're trying to make phosgene wink.
Anyway, you do not need to distil hydrazine, isolate it as the sulphate (which isn't volatile, thus the risk is greatly reduced), make a solution of it, add that to an appropriate amount of a calcium nitrate solution, filter out and wash the calcium sulphate ppte, leaving hydrazine nitrate in solution. This is interesting stuff, it's the basis of the astrolite explosives, its VoD is around 8km/sec. Anyway, crystalise out the nitrate salt and dry it. This can then be used to prepare sodium azide by adding more sodium hydroxide to the alcohol/nitrite ester/sodium hydroxide mixture, in order to deprotonate the hydrazinium ion to freebase hydrazine. Sodium nitrate will also be formed in the solution, as will water. This might make pptation of the azide a bit less high-yielding, but not much I wouldn't think. It's best to use hydrazine nitrate rather than sulphate, since if you're using it for lead azide or other heavy-metal azides (as your name kinda suggests, as does the fact that you've visited the E&W Forum) you won't ppte any metal sulphate which would dilute your primary's power, and also sodium sulphate is not soluble in alcohols, whereas IIRC sodium nitrate is, or at least, I believe it is more soluble in alcohols than is the sulphate. You'd have to check that though. But this should make purification of the sodium azide a lot simpler.

A few breaths of fumes will kill you, and in lower concentrations will give you cancer.Any advice on handleing hydrazine?

The first statement is a total lie, the second is exagerated. It is a carcinogen, but not a spectacularly powerful one. Saying it "will" give you cancer is perhaps misleading... Advice on handling? Store it as a salt, use it in a dilute solution. Never powder dried salts. That way any risk is very small indeed.

Hydrazine is extreamly explosive when distilled to a high concentration in air

Yes, that's why you don't distil it in air wink. An inert atmosphere is used, such as argon or nitrogen.

Or you could be adventurous and try the sodium amide route, but I think you will find that even less appealing to you tongue.

Edit: I think junkyards are instructed to dispose of airbags when they arrive, or they send them away to be disposed of. I was lucky enough to know someone who was asked to dispose of some smile. Try looking for an abandonned car with one. I think my car has four, dotted about in various places. So if you find a good car, you could get several hundred grams.

So, you're at the junkyard...

"Can I have some airbags please?"
"Why do you want them?"
"Why do you want them??"
"I don't, but--"
"Well then, give them to me!" smile

Or maybe the owner just wont care and will give you them.

I have a few times deliberately tried to grow large crystals of lead azide to see if they explode, so far, they have not. I think the risk is small (yet the hazard is great).

"Simplicity is the ultimate sophistication."
 
 
 
 
    nitroglycerin
(Stranger)
05-29-03 17:17
No 436424
      large crystals problem and amide method  Bookmark   

Acually the addition of dexterin whick is made by baking starches in the oven in a extended amount of time. The dexterin added while synthesizing lead azide will prevent the formation of large crystals.
Anyways what about the sodium method? SWIM had planned to make sodium via electrolysis of NaOH 2NaOH>>>>2 Na+H2+O2.
Molten Na react with dry ammonia gas to form sodium amide NaNH3. That is melted then reacted with N2O to form sodium azide.
So heres the equation NaNH3+N2O=NaN3+H2O some the water can be evaporated off.
 
 
 
 
    Daphuk_up
(Hive Bee)
05-29-03 20:38
No 436458
      with the amide method...  Bookmark   

What would you use for a container?  My understanding is that molten sodium amide acts as a solvent for a variety of materials, including glass, tungsten, magnesium and others.  Is there a specific stainless steel that is appropriate for this reaction?

Regal Sir Palladium and the Harlot Chlorine...they make such a cute couple. ^_^
 
 
 
 
    Nick_J
(Newbee)
05-30-03 03:28
No 436548
      Sodium amide method.  Bookmark   

2 Na + 2 NH3 --> 2 NaNH2 + H2
NaNH2 + N2O --> NaN3 + H2O
H2O + NaNH2 --> NaOH + NH3

Thus, overall, it is
2 Na + NH3 + N2O --> NaN3 + NaOH + H2

Sodium amide is exceedingly basic and reactive, and also very toxic. It can not come into contact with water. Sodium is harder to make than you might think if you have not tried before. A common problem is that sodium is soluble in fused sodium salts. You will need huge quantities of ammonia, and a safe way to vent the excess. Then you will need a dry N2O source, and again, you will need a lot of it and a good way to vent it from your lab. I know in some places 12g N2O cylinders can be bought, these could be used. Larger cylinders are expensive, and I don't think the method from NH4NO3 is very good. Others may have had more success with it, but yields are not good when I try it. It is not a method without risk, and the N2O will be very damp and will need cleaning and drying. And then at the end you will need to seperate the NaN3 from the NaOH before you use it for anything.

Well, try it, you might like it. But if I were you I would not use that method. Too complicated, and too many dangers. 

If lithium could be used instead of sodium then it would make it simpler, lithium being in batteries. I don't know what the stability of lithium azide is like though.

"Simplicity is the ultimate sophistication."
 
 
 
 
    nitroglycerin
(Stranger)
05-30-03 23:45
No 436737
      SWIM tried to electrolysis NaOH today but the...  Bookmark   

SWIM tried to electrolysis NaOH today but the molten NaOH burned through the pyrex beaker. This failure to create Na metal means SWIM will look towared the N2H4 method. Again SWIM is afriad on the N2H4 explosion hazard.SWIM does't have vacumm distillation, and he's still a very young person.
Speaking of the N2H4 method thers one where N2H4 is reacted with ethyl nitrate to yield NaN3. Any insights?
 
 
 
 
    Nick_J
(Newbee)
05-31-03 07:27
No 436779
      No,  Bookmark   

It is reacted with ethyl nitrite. It must be a nitrite. Basically there is some hydrolysis of the nitrite ester, forming nitrous acid. Then there is a diazotisation reaction, N2H4 + HONO --> H2N3(+) + H2O + OH(-), then the protonated hydrogen azide rapidly kicks off its extra hydrogen atom, along with the positive charge, thus giving N2H4 + HONO --> HN3 + 2 H2O. And since we have NaOH in the solution, HN3 + NaOH --> NaN3 + H2O, and the NaN3 pptes because of its low solubility in alcohol.
A nitrate ester will not work, because it is unable to form the required nitrous acid.
Aqueous hydrazine is not an explosion hazard, don't worry about it. I will repeat: you do not need to work with concentrated hydrazine. Only salts and dilute solutions.

"Simplicity is the ultimate sophistication."
 
 
 
 
    foxy2
(Distinctive Doe)
05-31-03 11:35
No 436824
      SWIM tried to electrolysis NaOH today but the...  Bookmark   

SWIM tried to electrolysis NaOH today but the molten NaOH burned through the pyrex beaker.


I think they use cast iron for that.
 
 
 
 
    nitroglycerin
(Stranger)
06-01-03 18:25
No 437089
      Another try  Bookmark   

SWIM had tried to do electrolysis of NaOH again this time with a copper crucible. The NaOH was melted SWIM inserted the electrodes. SWIM then touched two elcetrodes 12V 7 AMPS the worse electric shock SWIM had experenced in his life. SWIm tried again attaching the - to the copper and the + carbon electrode into the molten soloution, blak some molten stuff shot up and hit SWIM in the arm, it burns like hell, so painful, SWIM will try again another day.
 
 
 
 
    Barium
(Hive Addict)
06-02-03 02:18
No 437171
      For christ sake  Bookmark   

You want to make sodium by electrolysis of sodium hydroxide. This is a industrial method and needs special equipment. Sodium hydroxide melts at 318C and you just assume you can somehow collect the liberated, unprotected sodium at this temperature? Do you perhaps have a vauge memory from highschool chemistry that sodium is a tad reactive towards water and oxygen at room temp? Then what do you think the reactivness will be at around 320C? Less, perhaps?

Freaky
 
 
 
 
    raffike
(Hive Addict)
06-02-03 03:24
No 437183
      For what do you need sodium azide ...  Bookmark   

For what do you need sodium azide afterall,maybe there's some other way around.It's not very expensive(150$/500 grams at Fluka) but it's very unlikely you can manufacture it at home.

For those about to synth,we salute you
 
 
 
 
    nitroglycerin
(Stranger)
06-02-03 16:27
No 437339
      I'm in alot of pain now!  Bookmark   

Damit it hurts, SWIM is wraped up in bandages now. And yea SWIM had just compleated almost 2 semister of highschool chemistry. SWIM's not going to be a freshman for long. getting tossed in the trashcan.
 
 
 
 
    Bumpz
(Stranger)
06-02-03 22:01
No 437395
      better preparation method  Bookmark   

Sciencemadness.org has a few posts detailing a slightly more OTC preparation of azides.  There are a few posts by a "Mr. Anonymous" which were emailed to both Polverone and PHILOU Zrealone.  In these posts he details a technique to produce hydrazine sulfate.  Search for "hydrazine sulfate OTC optimized synthesis" to find this procedure.  IIRC he continues in another post to describe how to produce sodium azide from the hydrazine sulfate with important details like color changes and reaction times.  Mr. Anonymous also contributed some very interesting procedures for other OTC preparations which may be very useful to the home chemist.

About the only difficult chemical to find IIRC is sodium nitrite.
 
 
 
 
    foxy2
(Distinctive Doe)
06-02-03 22:37
No 437407
      Search under my name here and Hydrazine, I...  Bookmark   

Search under my name here and Hydrazine, I think I posted alot of stuff

But by the sound of your dabbleing with sodium I think maybee you should leave these hazardous chems alone until you develop more lab skills and common chemistry sense.wink