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Author: Subject: The true mad science, hydrogen azide distillation
DJF90
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[*] posted on 2-12-2013 at 15:13


Brauer does indeed give instructions along these lines, but they mention it is dangerous and that the liquid obtained is potentially explosive. The synthesis in that case is intended for chemists wanting to study the properties of the pure comound HN3. From an amatuer chemistry perspective, we're more interested in utilising the acid for reactions and salt formations, any improvement on safety at the expense of concentration should be taken.

You did not need to prepare such a concentrated form, and if it really was necessary, ion exchange resin would probably be the best way to go. A dilute 3% solution obtained from the Inorg Synth prep would have served your needs, but you're too cavalier to settle for that. I'm hoping you'll wise up sooner than later, or it may cost you dearly.

Don't take this as an attack; like I mentioned previously I think its good you're following your interests ,but please do it safely. I'd recommend that you start making risk assessments before doing practical work.
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Random
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[*] posted on 2-12-2013 at 15:23


Extremly dangerous chemical. There is description on rhodium mirror that after preparation of it the chemist had a very strong headache even while using fume hood and all safety equipment. Personally I would have to think more than twice to attempt this.


I have the feeling that you don't value your life enough plante.. It is not always a matter or life or death to deal with but also a matter of staying phiyically handicapped from your mistakes and having to continue to live.

Very strong acute toxins are pretty straightforward but then again life should be respected and strong explosives in small amounts won't kill you but leave you as a handicap.
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plante1999
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[*] posted on 2-12-2013 at 20:37


Well it seams I was doing it safer then him as after the synthesis I only had very very slight headache. I was washing the exit gas in Basic solution. The worst time was when I dismantled the apparatus.

Handicapped or really badly hurt would mess my life so much that I would probably finish myself honestly, in this case a tablespoon of azide should had done the trick, and it was near...

"You did not need to prepare such a concentrated form, and if it really was necessary, ion exchange resin would probably be the best way to go. A dilute 3% solution obtained from the Inorg Synth prep would have served your needs, but you're too cavalier to settle for that"

True, true and True.

"Don't take this as an attack"

I never did, I take theses as advises.


Next time I will make a table for the pros and the cons of my synthesis/madness ha ha.

-----------------------------

I was not obligated at all to make it that concentrated, nor to make it all. It was overly dangerous but well though contrary to the popular believe. I am someone generally quite wise for my age but there is stuff I have hard time to, especially when I got nothing else then my own intelligence to provide reflections. I do not pretend that it was intelligent, the synthesis was definitely not, but the chemist however is not slow or stupid, at all. I could have done something else, but I did not as I was looking for something, something I am looking all day long, and you know what it is DJF90.




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quantumchromodynamics
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[*] posted on 3-12-2013 at 01:17
science takes balls


I realize that I am a nobody with no posts; however, I congratulate the experimental science and sheer balls it took to attempt this reaction, let alone submit it for review! New experience has created new shared knowledge. Certainly there are more standard and less suicidal ways this particular reaction could have been done, but that was not the point. To me, the point was to push a boundary and learn from experience. Bravo! Real scientists are voraciously curious. Curiosity drives us. Sometimes curiosity makes us do stupid things. Ask any cat. It takes balls to be truly and experimentally curious. Imagine the first Vikings striking out on shitty rafts just to see what the hell was in the West. The list of stupid things people have done just out of curiosity is endless. Frankly, I would rather blow myself up in some chemistry experiment, or get sucked into an electromagnetic space/time vortex, or mind wiped by a rail gun capacitor EMP, than die old and bored, whining about my fair share of government cheese.
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[*] posted on 3-12-2013 at 12:43


If you are seeking to risk your life or health with your experiments, at least do something that counts. Not just in our little mad scientist community, but preferably to humanity at large. Come with something monumental or you will just be another Darwin award.

e.g. sign up for the One way trip to mars, a scientist could be useful.

Top 10 Scientists Killed or Injured by Their Experiments




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"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer
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[*] posted on 3-12-2013 at 13:46


I'm taken aback by the negative responses in this thread.


Quote:

If you are seeking to risk your life or health with your experiments, at least do something that counts. Not just in our little mad scientist community, but preferably to humanity at large. Come with something monumental or you will just be another Darwin award.


Get off your high horse. When is the last time you did something monumental?

I don't understand how people can chastise plante for not doing proper research while at the same time expressing concern that others might get hurt trying to replicate what he did. Clearly you don't hold others up to the same standard.

Yes, this experiment is dangerous. But as long as you're not endangering others and are fully aware of the danger to yourself, I see no harm. What happened to complaining about the nanny state?





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[*] posted on 3-12-2013 at 15:14


I agree with vulture. Knowing the danger and not putting other people at risk is all that the experimenter needs to do.

Fantastic but dangerous experiment. Good work.




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[*] posted on 3-12-2013 at 17:41


Quote: Originally posted by vulture  
I'm taken aback by the negative responses in this thread.


Quote:

If you are seeking to risk your life or health with your experiments, at least do something that counts. Not just in our little mad scientist community, but preferably to humanity at large. Come with something monumental or you will just be another Darwin award.


Get off your high horse. When is the last time you did something monumental?

I don't understand how people can chastise plante for not doing proper research while at the same time expressing concern that others might get hurt trying to replicate what he did. Clearly you don't hold others up to the same standard.

Yes, this experiment is dangerous. But as long as you're not endangering others and are fully aware of the danger to yourself, I see no harm. What happened to complaining about the nanny state?




100% agreed.

Lets not turn into chemicalforums where when someone uses nitric acid at home, the board collectively wets itself.
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plante1999
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[*] posted on 3-12-2013 at 19:22


Especially since the name of the forum is science madness. So, anyone got something he would want I try?



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blogfast25
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[*] posted on 4-12-2013 at 06:46


Quote: Originally posted by vulture  
What happened to complaining about the nanny state?



DOWN with the nanny state!




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[*] posted on 4-12-2013 at 08:08


An interesting experiment with your HN3 would be to make some ClN3 from it. This is a colorless gas, but it is yellow in solution. It only dissolves a little bit in water, but dissolves better in organic solvents, such as CCl4 and CHCl3. Such solutions can be used for substituting azide groups for hydroxyl groups in organic compounds.

If you have HN3, dissolved in water, then add some of the solution (10%, not more concentrated!) to a solution of NaClO (5% active chlorine is OK). You get a yellow solution and production of a colorless gas. The simplest experiment you can do is bubble this colorless under water with dish washing soap and ignite the bubbles, sticking at the surface of the water. You will be really amazed by the incredible powerful BANGs from even small bubbles, especially if you keep in mind that the gas explodes unconfined!

Do this experiment on a very small scale, use face protection and hand protection. The gas may explode without apparent reason! I have done this experiment once myself, IIRC the description lingers around on sciencemadness somewhere in an old thread. I used an aqueous solution of NaN3 which I added to slightly acidified bleach. With your HN3 the experiment should run much smoother.

-------------------------------

I do agree with vulture, but I really hope, however, that you will remain safe and healthy. Doing potentially dangerous chemistry is not a no go in my opinion (I also sometimes do, as the above experiment shows), but be VERY careful and always think about what can go wrong and if things go wrong what can be done to alleviate the consequences of this. For me the line is where experiments can go wrong in such a way that they permanently damage my body, such that I get handicapped for the future. It is not worth such an offer. But DJF90 also had a very good remark: there is only one plante1999. It would be a really sad thing if this person would be severely damaged or even die.




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Want to wonder? Look at https://woelen.homescience.net
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Random
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[*] posted on 4-12-2013 at 13:22


Before attempting ClN3 synthesis read this:

http://www.lateralscience.co.uk/oil/


Then decide for yourself. Woelen seems quite experienced dealing with extremly dangerous stuff such as handling smaller quantities of this or HCN easily but he is woelen after all. I mean just check his experiments on the site.

I wouldn't be surprised with him playing with phosgene or something even worse than that but I can't say that is for everyone. He has a lot of experience and caution, something a younger chemist might lack.




Story with Klute and H2S is also something I'm not gonna forget so easily. He would have died if he didn't inject himself with LAB GRADE nitrite iirc.

[Edited on 4-12-2013 by Random]
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plante1999
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[*] posted on 4-12-2013 at 13:44


Nitrogen trichloride and chlorine are not the same thing, funnily, I had already did experiments with chlorine azide before Woelen mentionned it.



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woelen
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[*] posted on 5-12-2013 at 01:12


@Random: You are referring to the compound NCl3, I am talking about ClN3. Both are dangerous compounds, but I think NCl3 is somewhat more dangerous, because it is a liquid and hence inherently much more concentrated. I never made NCl3 in more than microquantities (and with micro I mean really micro, droplets of at most 0.5 mm diameter). I would feel really uncomfortable if I had a ml of NCl3.

ClN3 also is very dangerous, like NCl3 it can explode apparently without reason. Don't look at it too angrily, it may hit back at you by exploding! In my experiments with ClN3 I was really amazed by the power of its explosions. A bubble of only 1 ml of gas, when ignited, gives an impressively loud BANG!




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Random
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[*] posted on 5-12-2013 at 08:16


I know it's not the same compound woelen but seems similar. It should be an example of what explosives are able to cause. Care should be taken with both of these compounds.
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plante1999
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[*] posted on 5-12-2013 at 18:16


Yes of course, but it is not like if they seamed really stable...

I won't be able to titrate this week, but still take suggestions.




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[*] posted on 5-12-2013 at 18:30
Lateral Science is (Mostly) Fiction!!!


Quote: Originally posted by Random  
Before attempting ClN3 synthesis read this: http://www.lateralscience.co.uk/oil/ Then decide for yourself.
Quote: Originally posted by bfesser  
Please, not that <em>Lateral Science</em> site again! Just so you're aware, that site is heavily <em>fictional</em>. The proprietor came around here a few <del>weeks</del> [months] ago advertising for his new novel (you may find the post in <strong>Detritus</strong>;). I caution you to be skeptical of anything you read on that website! It can be tricky to sort out the factual information from the rest of it.




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watson.fawkes
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[*] posted on 5-12-2013 at 18:49


bfesser, did you even bother read the page in question before your own internal fulminating humors detonated and splattered all over the board? There's nothing on that page that's more recent than a century and a half except a quotation from a 1929 Encyclopedia Brittanica article. There's absolutely nothing remotely controversial about it.

Yeah, we get it. You don't like the site. But all you're proving is that your personal opinion is nothing but prejudice in this case.

Quoting the entirety of the above post for the record.
Title: Lateral Science is (Mostly) Fiction!!!
Quote: Originally posted by bfesser  
Quote: Originally posted by Random  
Before attempting ClN3 synthesis read this: http://www.lateralscience.co.uk/oil/ Then decide for yourself.
Quote: Originally posted by bfesser  
Please, not that <em>Lateral Science</em> site again! Just so you're aware, that site is heavily <em>fictional</em>. The proprietor came around here a few <del>weeks</del> [months] ago advertising for his new novel (you may find the post in <strong>Detritus</strong>;). I caution you to be skeptical of anything you read on that website! It can be tricky to sort out the factual information from the rest of it.

<hr/>bfesser moderator expellendus est
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[*] posted on 5-12-2013 at 19:13


Yes, I've read it. Stop quoting me.



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[*] posted on 5-12-2013 at 23:06


First post.

What you have done was extremely stupid. No fume hood, improvised distillation equipment, insufficient shielding, and you allowed yourself to breathe HN3 gas? That smell that took your breath away could have seriously injured or killed you had the vapor been more concentrated or were you less lucky. If the distillate had detonated, you would have not only been injured but you and your surroundings sprayed with HN3 solution. What shocks me even more is that you have been encouraged by well wishers on this board. I feel that the board lacks a safety culture... open benzene and bromine distillations came to mind while reading this thread. Do you even have a serious plan for its safe disposal? This kind of behavior is exactly why the general public fears amatuer chemistry. Frankly I do not understand why someone would celebrate risking their lives to make a useless, dangerous chemical that has already been thoroughly studied and reported...

You seem proud of what you did, and as a chemist I feel that you have no respect for my field. If you must pursue your death wish, I ask that you stop calling it science.
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[*] posted on 5-12-2013 at 23:11


Quote: Originally posted by quantumchromodynamics  
I realize that I am a nobody with no posts; however, I congratulate the experimental science and sheer balls it took to attempt this reaction, let alone submit it for review! New experience has created new shared knowledge. Certainly there are more standard and less suicidal ways this particular reaction could have been done, but that was not the point. To me, the point was to push a boundary and learn from experience. Bravo! Real scientists are voraciously curious. Curiosity drives us. Sometimes curiosity makes us do stupid things. Ask any cat. It takes balls to be truly and experimentally curious. Imagine the first Vikings striking out on shitty rafts just to see what the hell was in the West. The list of stupid things people have done just out of curiosity is endless. Frankly, I would rather blow myself up in some chemistry experiment, or get sucked into an electromagnetic space/time vortex, or mind wiped by a rail gun capacitor EMP, than die old and bored, whining about my fair share of government cheese.


This isn't science. It sounds like science, but there was no hypothesis being tested or question being answered; hydrogen azide has been thoroughly studied and there will be no new answers from this work. It was just a dangerous stunt.
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plante1999
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[*] posted on 6-12-2013 at 04:14


I really like these last two posts, you know, if you are scared about people distilling bromine this board is not for you really.

As a chemist, you probably know no everything is obtainable, and some chemicals must be synthesized in house to test some reactions. Having no respect for your field, well that is the best, I believe mostly everyone on this board could say I'm one of the few here that is doing study to become a chemist, and don't be too tempted to think I won't succeed.

I hope you already read older reference work of the 18th century, as that hypotesis thing for every work started at school there is about 60 years now. If you where needing iodine in an experiment and you described its synthesis, would you think an "hypothesis" would be needed? Certainly no, because you know that it will the reported procedure work.

Put your 21th century chem book aside, and read older references.

Have a good day.

[Edited on 6-12-2013 by plante1999]




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blogfast25
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[*] posted on 6-12-2013 at 06:16


Quote: Originally posted by Tetrakis  
I feel that the board lacks a safety culture... open benzene and bromine distillations came to mind while reading this thread.

[snip]

You seem proud of what you did, and as a chemist I feel that you have no respect for my field. If you must pursue your death wish, I ask that you stop calling it science.


You hardly know this board and are already judging it very superficially, not to mention use an extremely reductionist definition of science.

'No respect for your field'? You pompous git. I'm a qualified chemist and I feel he's MORE than respecting 'my field'.

Quote: Originally posted by Tetrakis  
This kind of behavior is exactly why the general public fears amatuer chemistry.


Wrong again. The public fears what they don't understand. Accidents in home labs hardly EVER affect them.

Now please bugger off or present something interesting you did yourself. And don't forget to make it jam packed with hypotheses or else it doesn't count! :P

[Edited on 6-12-2013 by blogfast25]




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[*] posted on 6-12-2013 at 06:36


<strong>blogfast25</strong>, take it easy. There's nothing wrong with a newcomer posting here. Would you rather he junk post in beginnings? [/rhetorical] <em>Down, boy! Down! Sit! Stay!</em>

<strong>Tetrakis</strong>, while I agree with many of your points, I must assert that you're wrong about this board lacking a safety culture.




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[*] posted on 6-12-2013 at 06:49


Quote:

You seem proud of what you did, and as a chemist I feel that you have no respect for my field. If you must pursue your death wish, I ask that you stop calling it science.


As a chemist I'd strongly wish you'd drop your elitist attitude. Read about Tesla, Nobel and Moore and then quietly reconsider.

There are millions of taxpayer dollars devoted to science without immediate benefit or use.

I would rather call plante's experiment science than the crap which is coming out of the publication mill nowadays.




One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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