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Author: Subject: The true mad science, hydrogen azide distillation
plante1999
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[*] posted on 1-12-2013 at 16:09
The true mad science, hydrogen azide distillation


WARNING
Never ever try this experiment if you want to keep your life expectancy long. The fallowing synthesis deal with EXTREMELY toxic material, similar toxicity to hydrogen cyanide. EXTREMELY sensitive explosive with high power and powerful mucous irritant.

Today I did my most mad project ever, the synthesis of hydrogen azide. During all the synthesis I had two winter coat, a face shield, rubber and leather gloves. There was an acrylic blast shield between me and the reaction most of the time.

8 ml of sulphuric acid and 12 ml of water where mixed, and added to 6 g of sodium azide in 15 ml of water. the mixture was distilled using a short path. The reaction flask was flame heated in a water bath keep at 40-60 C during most of the reaction. At start the mixture that was clear took an orange concentration, the distillation which took about 1 h and half, was kept as low as possible to get the distillate. When the water bath was at 40 I got the first drops in the receiving flask. When distillate stopped to come off at 60 The azide solution was discarded and the hydrazoic acid was measured. The yield was 3 ml of a soft pink liquid with a VERY pungent smell that make someone out of breath the first time he smells it.

I did not test the product yet, however I'm up to take suggestions.


Side point: My apparatus was very improvised if compared to what it should had been, the short path had a teflon tape plug instead of the head thermometer due the lack of one. Since the clamp was very rusted, it was "pressed" in place to keep the apparatus in place. I won't keep the product for long, so if anyone have something that he would like I test, ask for it.

Some detail left behind intentionally.


[Edited on 2-12-2013 by plante1999]

[Edited on 2-12-2013 by plante1999]




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Brain&Force
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[*] posted on 1-12-2013 at 16:25


This is crazy awesome. I wouldn't even think of trying this, even in a well-controlled environment. However Wikipedia says hydrazoic acid is colorless, not light pink. Could you have any sources of contamination in the setup (possibly iron(III) or manganese(II))?

I can't think of any ideas for hydrogen azide use. Perhaps you could make some uncharacterized metal azide salt out of it?

Oh, and happy 1500th post plante1999!




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bismuthate
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[*] posted on 1-12-2013 at 16:30


Well to test it you could mix a mg amout with sodium or NaOH and dissolve that in water then mix with CuSO4 (use conc. solutions) and watch for a brown percpitate. Awesome experiment for your 1500th post!

[Edited on 2-12-2013 by bismuthate]

[Edited on 2-12-2013 by bismuthate]

[Edited on 2-12-2013 by bismuthate]




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[*] posted on 1-12-2013 at 17:28


badass! what about trying to perform a schmidt reaction?
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The_Davster
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[*] posted on 1-12-2013 at 18:21


Do it anhydrous.:D

A very nice way to do this is to warm a mix of dry stearic acid and dry NaN3. The stearic forms a melt and the HN3 distills nicely and if you are crazy you can collect it neat, or it can be distilled into a non-aqueous solvent making it nice for non-aqueous reactions. And only sometimes does the whole apparatus choose to detonate....:o



[Edited on 2-12-13 by The_Davster]
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plante1999
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[*] posted on 1-12-2013 at 18:26


If one donates enough that I can do it safely, I will.

And of course test the undiluted acid.


I have believe in the fact that the orange coloration comes from adole condensation from stabilizer in one or two of the reactants.

Schmidt reaction, I will try to find what I need.

Thanks, it was just a great add-on that it was my 1500th post.

I doubt mixing such a reactive chemical with sodium is a good idea, and I don't own sodium.
[Edited on 2-12-2013 by plante1999]

[Edited on 2-12-2013 by plante1999]

[Edited on 2-12-2013 by plante1999]




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[*] posted on 1-12-2013 at 18:30


Did you measure a concentration from the distillate?
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plante1999
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[*] posted on 1-12-2013 at 18:34


No, but by the smell it should be more then 10%. At the moment I only have access to one of these 10$ cheap Chinese 0.01 g scale, I doubt my measurement will be accurate. I guess a 0.001 cheap one could do the trick.



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[*] posted on 1-12-2013 at 18:36


You could titrate it. Phenolphthalein should be a decent indicator for the endpoint.
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plante1999
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[*] posted on 1-12-2013 at 18:41


I will, I will make stock solutions, and by the end of the week it will be titrated.



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[*] posted on 1-12-2013 at 20:44


Plante... You are absolutely nuts :D. This is pretty awesome though, good on ya!
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[*] posted on 2-12-2013 at 01:00


On another thread, (one I actually started) we discused methods of alkali metal production, where in fact azide production came up. Although, instead of being distilled, the Hydrogen Azide was absorbed into an Etheral layer as soon as it was produced. It gives considerably higher yield of final product, and can be perfomed at quite a low temperature, so it can be done MUCH less dangerous than distillation (considering that very little fumes are present and the risk of spontaneous detonation is almost non existant at low enough temperatures). Not to mention you can calculate precise concentration much easier since the percentage of affinity that Hydrogen Azide has for Ether over water is known to high accuracy. Also, it's very easy to make Etheral Hydrogen Azide ANHYDROUS just by drying it over a simple dessicant followed by filtering.

If you're looking to get into energetics, Hydrazanium Azide and Ammonium Azide are pretty interesting.



[Edited on 2-12-2013 by APO]




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[*] posted on 2-12-2013 at 07:20


I Second APOs comments, when I need hydrazoic acid I simply run a sodium azide solution through an Amberlite resin column (H+) form. When I have finished the column can be regenerated with HCl. This off course gives you only dilute aqueous acid but no lost fingers or eyeballs!

The acid then be neutralised with what you want
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plante1999
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[*] posted on 2-12-2013 at 09:20


I do not have a really proper glass set-up, far from having resin column, although it is very viable for low concentration of hydrazoic acid.

APO, Sodium azide will decompose to nitrogen and metallic sodium pretty vigourously when heated in nitrogen.

"Plante... You are absolutely nuts :D. This is pretty awesome though, good on ya!"

Awesome but deadly, had been a while since I had done some mad thing, guess this one is in the top of the mad experiment done by member here ha ha. Absolutly nuts... Maybe a bit.




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[*] posted on 2-12-2013 at 09:23


Quote: Originally posted by plante1999  
Awesome but deadly, had been a while since I had done some mad thing, guess this one is in the top of the mad experiment done by member here ha ha. Absolutly nuts... Maybe a bit.


Just make sure you keep posting- a sudden silence from your end will fill us all with dread.




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plante1999
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[*] posted on 2-12-2013 at 09:27


I'll make sure to post at least time to time for the upcomings years, and since I started chemistry I asked someone I know well to make an account and tell if something happened... Not that a fear it, but it is a possibility.



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[*] posted on 2-12-2013 at 10:45


Deary me... where do I start.

What you have done is very stupid and totally irresponsible. You're too caught up in trying to do the most outrageous/dangerous stuff that you're forgetting to do GOOD science. Not only is this a hazard to yourself, but also those around you, and you have to consider them too.

Before this starts to sound like a brainless rant, lets start with some literature, viz the attached excerpt from Inorganic Syntheses Vol 1. Read the two preparations there, and see where you made the stupid mistakes. I'm not saying you shouldn't have tried to make hydrogen azide solution, but at least do it in as safe a way possible.

If you can't work out what I'm getting at, let me spell it out for you; The experiment you've performed is fairly likely to have generated a very concentrated (and hence explosive) solution of hydrogen azide. It boils at 37 *C. Water doesn't boil until significantly higher. You've collected stuff boiling up to 60 *C. What do you think most of that is..?

They provide a procedure for generating a dilute aqueous solution, and you would have done well to have followed that. It is infinitely safer than what you have done. I think you should consider how badly things could have gone for you; you was lucky this time but maybe not the next.

Quote:
I Second APOs comments, when I need hydrazoic acid I simply run a sodium azide solution through an Amberlite resin column (H+) form. When I have finished the column can be regenerated with HCl. This off course gives you only dilute aqueous acid but no lost fingers or eyeballs!


Actually you can generate 50% HN3 aqueous solutions with IERs. Its not recommended (10-15% is considered safe for freshman labs) but at least possible.

[Edited on 2-12-2013 by DJF90]

Attachment: Hydrogen azide - Inorg Synth Vol 1.pdf (308kB)
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[*] posted on 2-12-2013 at 11:47


Uhhh, and this guy judges me in another thread :D Nice work, but what are you going next with it? I would like to listen on ammonium azide synthesis and properties from you, also could you just for fun take a small drop of it (far from main container) and throw a KMnO4 crystal into it - will it explode or not high enough concentration ? You mentioned it's smell - you're still alive ? :O
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[*] posted on 2-12-2013 at 11:53


Quote: Originally posted by papaya  
Uhhh, and this guy judges me in another thread :D


You suffer from long toe syndrome and of a vindictive kind too.

Stop talking rubbish as you've repeatedly done and people won't treat you as a 'kewl'.

And if you can't take criticism take up knitting: science isn't for you.




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[*] posted on 2-12-2013 at 13:44


Plante, I think you misunderstood me, INSTEAD of being distilled to separate the Hydrogen Azide from the mixture, it is absorbed into a layer of Ether. Thus, it can be cooled as the reaction that forms Hydrogen Azide takes place, since no heating for distillation is needed. Ultimately it is MUCH safer as I described.

Another method that involves a still much safer distillation approach is here.




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plante1999
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[*] posted on 2-12-2013 at 13:52




"What you have done is very stupid and totally irresponsible. You're too caught up in trying to do the most outrageous/dangerous stuff that you're forgetting to do GOOD science."

Stupid, I would not say so, totally irresponsible, probably. I have done good science for a while... Trying to do the most dangerous/outrageous stuff I can, Totally agreed, and you already know the reason why, and this is why you are involving yourself into this.


"If you can't work out what I'm getting at, let me spell it out for you"

I may be mad, but not stupid, far from that, you know me better then that.

" I think you should consider how badly things could have gone for you; you was lucky this time but maybe not the next. "

I, honestly considered it before doing the experiment.


I read your reply before you edited it, and I had in fact read a few reference, such as Brauer preparation, Ullmann's encyclopedia, and inorganic syntheses, the same you provided me in another time.


Please, do not make this thread derail and go to detritus by arguing with each others.

[Edited on 2-12-2013 by plante1999]




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[*] posted on 2-12-2013 at 14:24


Quote: Originally posted by plante1999  


I have done good science for a while... Trying to do the most dangerous/outrageous stuff I can, Totally agreed, and you already know the reason why, and this is why you are involving yourself into this.


Agreed, you generally do good science. But not this. Far from it. I am involving myself in this because it is an excessively dangereous method and I'd like to try and prevent yourself and others foolish enough to follow in these footsteps from a serious accident. Theres only one of you, and if you get seriously damaged, not even the best surgeon may be of help.

If you were doing good science you would have read the references and taken note of the following line (which appears in both!):
Quote:
The contents of the flask are heated to boiling (very important!), and 90 ml. of 40% H2SO4 is added dropwise.
.

You see... I don't have a problem with you preparing HN3, but not if you're going to ignore important instructions such as these. Doing so is negligent. These experienced chemists do not make such comments for the fun of it.

Quote: Originally posted by plante1999  

I may be mad, but not stupid, far from that, you know me better then that.

" I think you should consider how badly things could have gone for you; you was lucky this time but maybe not the next. "

I, honestly considered it before doing the experiment.


If you had honestly considered it, you would have followed the literature method to the letter. You did not. These seemingly small details could mean the difference between death and performing a successful synthesis. Perhaps you will re-evaluate your risk assessment next time.

Quote: Originally posted by plante1999  

I read your reply before you edited it, and I had in fact read a few reference, such as Brauer preparation, Ullmann's encyclopedia, and inorganic syntheses, the same you provided me in another time.


I only edited my post to include the attachment which I had forgotten. You already have the Inorg Synth prep, and that tallies against you once again on the negligence front. You had access to two preps that both tell you to heat before dropwise addition of acid, yet you did not. I'm starting to feel like a broken record...
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plante1999
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[*] posted on 2-12-2013 at 14:45


"I'm starting to feel like a broken record..."

You are not. I made a variation of the first Brauer preparation.




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[*] posted on 2-12-2013 at 14:47


Quote: Originally posted by plante1999  

I may be mad, but not stupid, far from that, you know me better then that.


Apparently not, if you are willing to attempt this experiment using your "improvised" equipment and comparative minimal experience. I would not even consider this preparation without significantly longer periods of training and outside of a proper laboratory using proper equipment.

Quote: Originally posted by plante1999  


" I think you should consider how badly things could have gone for you; you was lucky this time but maybe not the next. "

I, honestly considered it before doing the experiment.


Again, apparently not, if you prepared a significantly more concentrated, and extremely dangerous, solution of this compound than you had intended.

Quote: Originally posted by plante1999  


I read your reply before you edited it, and I had in fact read a few reference, such as Brauer preparation, Ullmann's encyclopedia, and inorganic syntheses, the same you provided me in another time.


Reading a few references is not sufficient for synthetic chemistry, least not for compounds of this nature. You must look at each one critically, appreciate and evaluate its content, and design your own experiment accordingly. I feel that your attitude towards your work is too laid back, arrogant and simply not acceptable, if you choose to work with these kinds of compounds. You claim to have done proper science, but your attitude here strongly shows otherwise.

To summarise, do not attempt experiments that are clearly too dangerous for someone of your experience, skill level and equipment availability, and do not show your arrogance. I've learnt this lesson myself, and it's done me a world of good.


[Edited on 2-12-2013 by Hexavalent]




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plante1999
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[*] posted on 2-12-2013 at 14:52


"Again, apparently not, if you prepared a significantly more concentrated, and extremely dangerous, solution of this compound than you had intended."

It was intended to be concentrated, read Brauer prep. one.

"To summarise, do not attempt experiments that are clearly too dangerous for someone of your experience, skill level and equipment availability, and do not show your arrogance. I've learnt this lesson myself, and its done me a world of good."

Equipment availability, agreed it was far from required, as for skill and experience, from someone saying that I'm arrogant, show your not fully maturity.




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