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Author: Subject: Safe practices when synthesizing nitrobenzene
thors.lab
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[*] posted on 11-8-2019 at 18:09
Safe practices when synthesizing nitrobenzene


Hi,

In my next video, I will be synthesizing nitrobenzene by nitration of benzene.

I understand that this nitration is highly exothermic and prone to thermal runaway. I also understand that di- and trinitrobenzenes are highly explosive, and that all nitrobenzenes are extraordinarily toxic.

I plan to run this reaction at a 0.33 molar scale based on benzene (30mL benzene, slight excess of nitric acid and sulfuric acid).

At this small scale, it should be possible to regulate temperature using an ice water bath, no? Nitrile gloves, long-sleeved jacket, and safety goggles will be worn. A large fan will be set up in a well ventilated room (2 windows and one door to outside in a roughly 10x4 foot area). During distillation, a hose will be connected to the vacuum adapter and lead outside.

The flask will be evenly heated with an oil bath during reflux, and the temperature carefully monitored. Hot plate will be made easily removable by raising it with wooden blocks that can be easily removed to lower the hotplate. A pot of ice water will be readily available for cooling.

Are there any other safety precautions I should take?

Thanks,

Thor




Please check out my latest video: Synthesizing Nitrobenzene, and the last one:
Making Nitric Acid.
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BromicAcid
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[*] posted on 11-8-2019 at 18:30


What procedure are you following? Follow a set procedure, don't wing it.

PS: It is one of the best smelling compounds I ever synthesized but it will give you a nitro headache in a heartbeat.

[Edited on 8/12/2019 by BromicAcid]




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thors.lab
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[*] posted on 11-8-2019 at 20:03


Quote: Originally posted by BromicAcid
||
|| What procedure are you following? Follow a set procedure, don't wing it.
||
|| PS: It is one of the best smelling compounds I ever synthesized but it will give you a nitro headache in a heartbeat.
||
|| [Edited on 8/12/2019 by BromicAcid]

I'm following NileRed's procedure, which in turn was a procedure from Rhodium. I can't link it here because the spam filter has a tendency to ban me.




Please check out my latest video: Synthesizing Nitrobenzene, and the last one:
Making Nitric Acid.
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Felis Corax
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[*] posted on 11-8-2019 at 20:24


Depending on the concentration of your nitric acid using nitrile gloves may provide only a brief window of protection. Fuming nitric acid will even cause then to ignite, making the gloves more dangerous than handling the acid with bare hands.

I look forward to your next video.




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thors.lab
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[*] posted on 12-8-2019 at 01:48


Quote: Originally posted by Felis Corax
||
|| Depending on the concentration of your nitric acid using nitrile gloves may provide only a brief window of protection. Fuming nitric acid will even cause then to ignite, making the gloves more dangerous than handling the acid with bare hands.
||
|| I look forward to your next video.

Thank you!

Yes, I was actually thinking about this but wasn't sure if it was a myth or not. I heard that gloves may make it harder to feel when acid touches your skin, so you may be less inclined to wash them.

Still, I don't want to encourage unsafe practices on my channel. Since I only have the option for latex, nitrile, or no gloves, which would you recommend?




Please check out my latest video: Synthesizing Nitrobenzene, and the last one:
Making Nitric Acid.
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Ubya
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[*] posted on 12-8-2019 at 04:00


which gloves to use depends on the acis concentration, nile red made a video about nitric acid igniting gloves. nile red made also a video of the reaction of various acids on your hands, and guess what? nitric acid was the worst, you can feel the burning sensation after just a few seconds. the correct use of gloves is to remove them as soon as theh get contaminated, they are just a buffer, not a barrier.

one tip i have is first try at least once the reaction, many rhings can go wrong, or you could have unsuspected results, if everything goes well, or you have resolved the various issues, then make the video with a new batch and with new knowledge.
i see many times people filming a reaction they have never done if not in front of the camera, and things can go wrong, and then it's not an educational video anymore, it's just a video version of lab notes





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[*] posted on 12-8-2019 at 04:14


Do a test. Put some of your acid on a nitrile glove. If it ignites you're better off gloveless. If it doesn't, wear gloves but know to remove them if they get contaminated.



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thors.lab
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[*] posted on 12-8-2019 at 12:39


Quote: Originally posted by Ubya
||
|| which gloves to use depends on the acis concentration, nile red made a video about nitric acid igniting gloves. nile red made also a video of the reaction of various acids on your hands, and guess what? nitric acid was the worst, you can feel the burning sensation after just a few seconds. the correct use of gloves is to remove them as soon as theh get contaminated, they are just a buffer, not a barrier.
||
|| one tip i have is first try at least once the reaction, many rhings can go wrong, or you could have unsuspected results, if everything goes well, or you have resolved the various issues, then make the video with a new batch and with new knowledge.
|| i see many times people filming a reaction they have never done if not in front of the camera, and things can go wrong, and then it's not an educational video anymore, it's just a video version of lab notes
||

That's a good tip. However, sometimes I wish NileRed and the others did show their failures because it would be helpful to learn how to deal with setbacks in the lab.

Perhaps I will make more benzene so that I can try this reaction twice.

Thanks,

Thor




Please check out my latest video: Synthesizing Nitrobenzene, and the last one:
Making Nitric Acid.
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