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Author: Subject: chloroform is not forming
vmelkon
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[*] posted on 17-7-2012 at 15:53
chloroform is not forming


Hello,
I had made some chloroform with commercial bleach + acetone and this worked well.

I wanted to produce some bleach myself and to try to make chloroform. After doing electrolysis of a conc solution of NaCl for 2 weeks and non-stop, I tried it. When I added the acetone, an initial whiteness was visible but it was weird. It looked like white solid particles.

I repeated the experiment. This time I took the bleach, added a few granules of NaOH and then a few drops of acetone. The same thing happened.

What could the white solid be?

Do I have too much NaCl in the solution? Is it NaCl particles?
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mnick12
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[*] posted on 17-7-2012 at 16:09


Did you confirm the presence of hypochlorite? Without doing some sort of conclusive testing it is hard to say how much hypochlorite is actually present in your solution. Titration is necessary in a situation like this, odor alone is insufficient to conclude the presence of a practical amount of hypochlorite as the odor threshold is somewhere around 0.5ppm depending where you look.

Other than that its hard to say what happened, if you are doing this for practical purposes I would suggest you stick with bleach since it gives consistent results and is very cheap.
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cyanureeves
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[*] posted on 17-7-2012 at 16:20


hey i have have made chloroform a couple of times before with cheap bleach even but i got the same results as you using the 10% green bleach from kmart.the stuff smelled like chloroform but it just never separated.as a matter of fact i used the same bleach and did not succeed at making hydrazine sulfate and i had the right strength ammonia too. i tried two times and nothing!
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Poppy
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[*] posted on 17-7-2012 at 17:23


Maybe all the chloric acid decomposed in contact with your reaction vessel, also its pretty evident you are useing the wrong cataliser for this reaction to proceed.



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Endimion17
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[*] posted on 17-7-2012 at 17:38


Why is it so hard to use the search function? There are tons of threads on chloroform synthesis. Also, wrong part of the forum.
All it takes is clicking the search link, typing c-h-l-o-r-o-f-o-r-m and clicking the search button.




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vmelkon
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[*] posted on 18-7-2012 at 05:27


Quote: Originally posted by mnick12  
Did you confirm the presence of hypochlorite? Without doing some sort of conclusive testing it is hard to say how much hypochlorite is actually present in your solution. Titration is necessary in a situation like this, odor alone is insufficient to conclude the presence of a practical amount of hypochlorite as the odor threshold is somewhere around 0.5ppm depending where you look.

Other than that its hard to say what happened, if you are doing this for practical purposes I would suggest you stick with bleach since it gives consistent results and is very cheap.


I didn't do titration.
Since I did the electrolysis for a long time, I assumed a lot of chlorine had to be generated and thus, a reasonable amount of NaClO. It is in a hoffman type apparatus that I built. The chlorine side must have a leak since the level doesn't go up. The leak must be a very tiny hole.

The only thread that I found about white precipitate is this
https://www.sciencemadness.org/whisper/viewthread.php?tid=13...
garage chemist says "I only got some white precipitate and no liquid chloroform"
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vmelkon
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[*] posted on 18-7-2012 at 05:31


Quote: Originally posted by Endimion17  
Why is it so hard to use the search function? There are tons of threads on chloroform synthesis. Also, wrong part of the forum.
All it takes is clicking the search link, typing c-h-l-o-r-o-f-o-r-m and clicking the search button.


The only thread I found was this
https://www.sciencemadness.org/whisper/viewthread.php?tid=13...
garage chemist says "I only got some white precipitate and no liquid chloroform"

but no one tries to explain what the white precipitate might be.

I was wondering if anyone else is trying the electrolysis route and what their experience is.
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Nicodem
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18-7-2012 at 09:40
vmelkon
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[*] posted on 20-7-2012 at 03:58


The white stuff has dissolved away so I think it was probably some salt.
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