Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1    3
Author: Subject: The true mad science, hydrogen azide distillation
The_Davster
A pnictogen
*******




Posts: 2861
Registered: 18-11-2003
Member Is Offline

Mood: .

[*] posted on 6-12-2013 at 06:50


Quote: Originally posted by Tetrakis  
I feel that the board lacks a safety culture...


And I feel that the average chemist has his balls in OSHA's purse, and is unable to accurately gauge risk thanks to years of safety indoctrination.

It seems we are at an impasse.

You should direct your eyes to the name of the site "ScienceMADNESS" as well as "The ART and science..."

Picasso painted lots of paintings, because that's what he did, that was his method of expression, through art. Here, synthesis is our art.


Perhaps the facebook group "I fucking love science" would be more your style.
View user's profile View All Posts By User
woelen
Super Administrator
*********




Posts: 7727
Registered: 20-8-2005
Location: Netherlands
Member Is Offline

Mood: interested

[*] posted on 6-12-2013 at 07:33


Quote: Originally posted by Tetrakis  
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.

I myself would not have done this experiment (at least not in this form), but your way of expressing is simply exaggerating the situation. The single reason for me not doing this experiment myself is the risk of violent explosion. I am not afraid of a whiff of HN3. A single whiff of this will not kill you. HN3 is not a cumulative poison and has no irreversible after effects. That makes a great difference for me.

Quote:
If the distillate had detonated, you would have not only been injured but you and your surroundings sprayed with HN3 solution.

Spraying around of HN3 solution is not good at all, but it is not the end of the world. It is volatile and quickly will evaporate. Plante1999 writes he had a double coat, face protection and double gloves, one pair being big leather ones. The chance of getting his own body sprayed with HN3 is practically zero.
I agree though that detonation of the solution IS a great risk. I think that explosion of 3 ml of HN3 can have devastating effects on your hearing capabilities and if you have the bad luck to have your hand very close at the moment of explosion, I can imagine that it is irreversibly damaged, even when gloved! That is the reason for me not to do this experiment.


Quote:
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.

I have done distillation of bromine myself: http://woelen.homescience.net/science/chem/exps/raw_material...
Of course you need to be careful and you need to know what you are doing, but it definitely can be done in an amateur setting! I would also do a benzene distillation if I had the means to prepare that chemical and wanted to isolate it.

Quote:
Do you even have a serious plan for its safe disposal?

Disposal of HN3 is not a problem at all. Just dilute with a lot of water and pour in excess solution of NaNO2 (ingredient of curing salt), which converts all azide to N2 and then flush down the drain the remaining nitrite-solution. Even if you don't have NaNO2 (which to my opinion should be present in your home lab when you experiment with azides), then I think that strong dilution with a lot of water and then flushing it down the drain (remember, we are talking about 3 ml only) with a bucket more of water is OK. Half-life of HN3 in the environment is low, maybe hours, at most days.

Quote:
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...

Amateur chemistry very very seldomly leads to accidents which other people besides the experimenter himself notices. When did you hear of an accident in the lab of an amateur chemist, such that other people had to be evacuated or such that a house burned down or something like that? Sometimes you hear such things from people making fireworks or from illegal drug labs who have a solvent fire, but a general home chemist blowing up things, poisoning the area around the house or some other major incident are unknown to me. That is the best evidence for me that there hardly is any need to talk so lowly about amateur chemistry.

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.

There is no deathwish in plante1999, and I think that he has quite some respect for what you call 'my field'.

Altogether I also am inclined to say that this experiment is beyond what you should do at an amateur level, and in my previous post in this thread I have expressed my concern about plante1999's safety, but the way you respond to this is 'whoaah look at how dangerous this is, he is going to kill himself and he destroys the environment'. We have enough nannies around us already who tell us what we may do and what we may not do.

It would be more interesting to think about modifications of this experiment, such that its risk is reduced. Think of DJF90's remarks, such as assuring that the liquid remains boiling hot, such that a lot of water vapor comes with the HN3. So, not simply dismissing things, but trying to think about improvements of the process is the key to getting people with you and having people listen to you. I can imagine that one day I also try to make some HN3 at low concentration, and then I most likely will remember this thread and implement safety measures, which plante1999 did not think of, but which he now knows about and can implement in the future. We can learn from each other, but only if we provide constructive remarks and not just yell about how dangerous and irresponsible someone has been.

Safety? Yes!
Listening to nannies? No!



[Edited on 6-12-13 by woelen]




The art of wondering makes life worth living...
Want to wonder? Look at https://woelen.homescience.net
View user's profile Visit user's homepage View All Posts By User
phlogiston
International Hazard
*****




Posts: 1350
Registered: 26-4-2008
Location: Neon Thorium Erbium Lanthanum Neodymium Sulphur
Member Is Offline

Mood: pyrophoric

[*] posted on 6-12-2013 at 13:58


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?



I am sorry if I sounded arrogant at all. Just trying to say it would be such a loss of a young and already very excellent scientist and experimenter (as well as a great human being). Perhaps I misinterpreted it (English is not my native language) but it seemed to me in his first posts that he doesn't place very much value on his life or limbs.
With his talents certainly he should be able to contribute to advancing the real frontiers of science soon (or whatever else he chooses to do). While, indeed, this was a fascinating and brave experiment, it is not worth losing body parts over (but, indeed, everyone should be free to decide otherwise for themselves)




-----
"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer
View user's profile View All Posts By User
ScienceSquirrel
International Hazard
*****




Posts: 1863
Registered: 18-6-2008
Location: Brittany
Member Is Offline

Mood: Dogs are pets but cats are little furry humans with four feet and self determination! :(

[*] posted on 6-12-2013 at 15:03


The Victorian period was a great time for amateur science.
Great discoveries were made by amateurs who worked in home labs.
There were disputes but many of them treated their fellow experimenters as gentle men and women.
So when you write; put on your smoking jacket, relax in your arm chair in front of cherry logs burning in the grate, puff your pipe filled with plum tobacco.
There are great discussions on here, this must be the best site for amateur science in the world.
I am off to the mountains of Brittany avec ma meuf et notre chatte, mais I hope I willl be online.
Maybe we could have a thread on Christmas Day?
Happy Christmas on Science Madness from across the world!
View user's profile View All Posts By User
bfesser
Resident Wikipedian
*****




Posts: 2114
Registered: 29-1-2008
Member Is Offline

Mood: No Mood

[*] posted on 6-12-2013 at 15:25


Quote: Originally posted by Tetrakis  
First post. What you have done was extremely stupid. … This isn't science. It sounds like science, but...
Hell of a first post! It got the attention of no less than two administrators and three moderators. Welcome to Science Madness!


<img src="http://s3.amazonaws.com/quotefully_production/photos/character/bac870c49a2511e0910f12313b10052d_small" width="100" align="middle" /> <em>"Back off, man. I'm a scientist."</em> &mdash; Dr. Peter Venkman</a>

[Edited on 6.12.13 by bfesser]




View user's profile View All Posts By User
subsecret
National Hazard
****




Posts: 426
Registered: 8-6-2013
Location: NW SC, USA
Member Is Offline

Mood: Human Sadness - Julian Casablancas & the Voidz

[*] posted on 6-12-2013 at 19:02


Tetrakis, I understand your concern for Plante, and if he were to severely injure himself, well, I would feel bad. You are free to discourage such experiments, though I do support them (as long as it's for science, and to pursue real, non-kewlish home chemistry). Even such a dangerous experiment involved lots of science, and I know that Plante took precautions to protect himself, and was aware of the dangers, thereby making himself fully aware of the risks. He proceeded to conduct the experiment without any bodily injury.

If you had asked me a year ago, I would've censured such an experiment, but I later learned that science is...science. For other references, I am a Darwinist. As for the public outlook on amateur chemistry, we must communicate that, though some of our experiments are dangerous, we take safety precautions. Chemistry can be safe or dangerous, but in the latter case, we "sure as hell" take precautions. Usually.




Fear is what you get when caution wasn't enough.
View user's profile View All Posts By User
Tetrakis
Harmless
*




Posts: 4
Registered: 5-12-2013
Member Is Offline

Mood: No Mood

[*] posted on 6-12-2013 at 21:44


I apologize for having posted in anger. Let me just say that I have respect for, and support, amateur chemistry. I am not as seasoned a chemist as many who post on this board, and have admiration for their achievements. If one needs hydrogen azide, by all means they should make it. Good chemistry, however, means achieving your synthetic goals while avoiding unnecessary risks. If the goal was to make pure HN3, there were better ways to do it... if I were to make this myself, I would have done it at 1/30th the scale in a short path distillation apparatus with flame-polished glass, and distilled it directly into a thick-walled vessel that I could seal from a distance. I would never put any part of my body near liquid HN3 unless I was sure it was in some sort of reinforced vessel. If you just wanted to obtain some pure HN3, why did you do this reaction on such a large scale? Perhaps you should read about the Texas Tech lab explosion in 2010, where students in an academic lab were maimed while inappropriately handling a large quantity of explosive material.

My mentioning benzene and bromine distillation was unnecessarily vague; I had earlier found an example of a teenager talking about how he had enjoyed walking around with an open container of bromine, and elsewhere on the board I saw an example apparatus (impressive, but still) for high temperature benzoic acid decarboxylation without active ventilation. Benzene isn't acutely toxic, but does have a cumulative carcinogenic effect... I don't think that its unreasonable to expect volatile, toxic liquids to be handled in a more controlled manner. I use or make CO, HCN, HN3, benzene, thallium chloride, etc. all the time, but I spend just as much time planning disposal and workup as I do planning the reactions, constructing apparati, etc.

That being said, I still don't understand why anyone would prepare undiluted HN3. Its a completely impractical form of HN3, which shouldn't be stored for extended periods of time and presents unpredictable dangers. When I work with HN3, I go to great lengths to isolate such reactions from normal waste and digest it appropriately when I'm done. If you need it to make something, why not just generate it in situ? I work with plenty of dangerous materials, but always minimize my risk by avoiding them as much as possible and isolating myself from them when I do need to use or make them.
View user's profile View All Posts By User
vulture
Forum Gatekeeper
*****




Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline

Mood: No Mood

[*] posted on 7-12-2013 at 05:59


Quote:

if I were to make this myself, I would have done it at 1/30th the scale in a short path distillation apparatus with flame-polished glass, and distilled it directly into a thick-walled vessel that I could seal from a distance. I would never put any part of my body near liquid HN3 unless I was sure it was in some sort of reinforced vessel.


And you'd be exposing yourself to more risk than plante did. Why? A thick-walled vessel would only cause greater damage if HN3 exploded. Thinking that a thick-walled vessel can contain a HN3 explosion, now that is bad risk assessment.






One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
View user's profile View All Posts By User
The_Davster
A pnictogen
*******




Posts: 2861
Registered: 18-11-2003
Member Is Offline

Mood: .

[*] posted on 7-12-2013 at 11:03


I have distilled anhydrous HN3. However on 1/10th gram scale.

It detonated a few times before I was able to collect the pure material. However thanks to the protective gear I had on, only my ego was damaged each time.

Assuming adequate windflow to keep Plante upwind was present, the only potential safety issue here in my eyes is scale and handling. I am convinced his crude armour/face shield would protect from everything(shrapnel) except the pure HN3 going off in his hand. 3g is more than any anti-explosion glove can take, so the way to mitigate this is either to scale down a bit, or to have standoff from handling. This can be achieved simply by handling the collection flask with a clamp around the neck. As explosive energy scales with (cubic or square, I forget), a little standoff is hugely effective. Even a 6" clamp, keeping his hands away from the flask would leave this experiment totally fine in my books. (of course, if collecting this in a testtube, you would not want the clamp around the liquid-containing part, lest the tines turn into shrapnel itself, shrapnel that would be harder to block than glass shrapnel)

Vulture already covered the folly of thick glass.
View user's profile View All Posts By User
plante1999
International Hazard
*****




Posts: 1937
Registered: 27-12-2010
Member Is Offline

Mood: Mad as a hatter

[*] posted on 7-12-2013 at 11:27


Next time I will probably make trimethylsilyl azide to try the propreties of anh. Hydrogen azide safely with that substitute. Although It would require a good 60$ to buy some trimethylsilyl chloride...



I never asked for this.
View user's profile View All Posts By User
ScienceSquirrel
International Hazard
Thread Split
8-12-2013 at 15:46
plante1999
International Hazard
*****




Posts: 1937
Registered: 27-12-2010
Member Is Offline

Mood: Mad as a hatter

[*] posted on 15-12-2013 at 15:25


I just destroyed the azide in dilute sodium nitrite/ sulphuric acid solution because my scale completely stopped working. I may work back on that project later this year.



I never asked for this.
View user's profile View All Posts By User
 Pages:  1    3

  Go To Top