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Author: Subject: What was your most dangerous/risky experiment
100PercentChemistry
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[*] posted on 11-5-2016 at 16:44
What was your most dangerous/risky experiment


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Loptr
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[*] posted on 11-5-2016 at 17:54


Mine is still on-going, it's called life.

But in all seriousness it would have to be distilling HCN.
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DraconicAcid
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[*] posted on 11-5-2016 at 17:57


Trying to extract Mn2O7.



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ChemTchr
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[*] posted on 11-5-2016 at 18:02


This probably isn't nearly as risky as most, but every year I make a large batch of nitrocellulose and have to use a mixture of azeotropic sulfuric and nitric acids, which get pretty hot when mixed. So far, haven't gotten a burn.
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[*] posted on 11-5-2016 at 21:26


I was attempting to make potassium formate, but accidentally made iodoform instead. It freaked me out a bit because I know iodoform is a fair amount more toxic than chloroform, which I hadn't planned on.



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[*] posted on 11-5-2016 at 22:36


I'm going to start distilling HClO4 soon... Cl2O7 is not fun.
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Metacelsus
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[*] posted on 12-5-2016 at 06:34


I've done a perchloric acid distillation, although I carefully planned it so that the concentration wouldn't go above azeotropic. Unless you are prepared to handle anhydrous perchloric acid, you should also do this. With proper planning, you will not form any dichlorine heptoxide.



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skip
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[*] posted on 12-5-2016 at 16:56


I have distilled at least a gallon of HCN, thats a cake walk. Sodium in ethanol really had me nervous , I thought with all the hissing and boiling that it was gonna catch fire. I was going slow too with addition of sodium. Had a fire extingusher in my hand almost the whole time. To hell with that !
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Loptr
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[*] posted on 12-5-2016 at 17:20


Quote: Originally posted by skip  
I have distilled at least a gallon of HCN, thats a cake walk. Sodium in ethanol really had me nervous , I thought with all the hissing and boiling that it was gonna catch fire. I was going slow too with addition of sodium. Had a fire extingusher in my hand almost the whole time. To hell with that !


Well, we all have our own perspective on such matters, and here is a case example.

[Edited on 13-5-2016 by Loptr]
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[*] posted on 12-5-2016 at 17:26


I think I would be a lot more nervous about distilling HCN than ethanol/sodium.
With the latter, if it starts looking crazy, you simply cover the vessel with something to exclude oxygen and back out of the room.
If you catch a lungful of HCN you have other problems. And not trivial ones.




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JJay
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[*] posted on 12-5-2016 at 21:50


I'm not sure... probably lighting acetylene on fire....



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Scalebar
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[*] posted on 13-5-2016 at 02:28


Purifying the infectious agent of CJD in bulk - but that was for work so I'm not sure it counts...
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[*] posted on 13-5-2016 at 16:25


Scalebar is declared the winner. I've done a lot of dangerous things, but that is a project I simply would have refused to perform.

No fix for that kinda poisoning. AND, me being a paranoid sort, the passage of time wouldn't put it behind me. With cyanide, you either die or you don't. With Prions, doubt stalks you.

Am I gonna be OK? Or, are there hidden changes taking place in my brain?

The idea gives me the Heebie Jeebies.
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[*] posted on 13-5-2016 at 22:19


Agreed. Scalebar, you win the thread.

My most dangerous moments have always been when something unexpected happened because I was pushing the edges of my knowledge. Notable among these was the accidental production of trichloramine. I was following a suggestion by deltaH (of "dangerous source of unreferenced speculation" fame). The target was an alternative means for producing NO2 gas. Procedure was to react urea with calcium hypochlorite. I got some lovely sharp bangs as the chloramine was produced. The saving grace was that I was somewhat forewarned and that I was working on sub-gram scale. Still, it seemed like it was nearly enough to shatter a test tube.

Other experiments that had a higher than normal risk factor: Reacting sodium with chlorine. My experiment setup was not what I would have liked and so it was not amazingly satisfying. I will try again. (Following NileRed's procedure for those who want to look it up. He got a glowing flask for a full 60 seconds.) My error was in being casual with cleaning up. there was some unreacted sodium that came in contact with water with both some glass and my hand in close proximity. It could have been messy.
Another notable one was the reaction between acetylene and chlorine. Exciting. I followed the procedure in experiment 101 of this source. It worked like a charm.




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[*] posted on 14-5-2016 at 03:07


Made a few hundred milligrams of chromyl chloride CrO2Cl2. It's very volatile and carcinogenic.

It does form a nice complex with slightly acidified H2O2 solution, though.
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[*] posted on 14-5-2016 at 16:43


Forming NCl3 unintentionally is always a surprise. Luckily it was a test tube scale (small) experiment and no real harm came from it other than aerosol in my face. Not my finest hour. It was an impulsive experiment to say the least and related to aga's nitric acid competition.

[Edited on 15-5-2016 by Loptr]
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