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Author: Subject: Chloroform Synthesis problems
D2DT
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[*] posted on 6-7-2016 at 00:01
Chloroform Synthesis problems


Hi,
I was synthesising some chloroform and I followed Nile red's video, but a white precipitate appeared that would only stay with the Chloroform as I can't use it for extractions because of the contamination. So is there any way to remove it or how to prevent it from occurring again. I used sodium hypochlorite bleach and acetone.
Thanks for your help. :)
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j_sum1
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[*] posted on 6-7-2016 at 01:18


Sounds like some kind of additive in your bleach. Try buying the dirt cheap stuff.



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bolbol
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[*] posted on 6-7-2016 at 12:15


I had that happen too but it was very little and it made the chloroform cloudy. Distillation should do the trick
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Texium (zts16)
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[*] posted on 6-7-2016 at 12:18


I would recommend using the pool chlorinator type of hypochlorite. It's cheaper, more concentrated (10%), and doesn't have any additives.



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Zandins
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[*] posted on 6-7-2016 at 23:58


Also, if you wish to avoid the trouble with commercial bleach, you can always make your own NaClO by unseparated electrolysis of NaCl.
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hyfalcon
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[*] posted on 7-7-2016 at 05:11


Quote: Originally posted by Zandins  
Also, if you wish to avoid the trouble with commercial bleach, you can always make your own NaClO by unseparated electrolysis of NaCl.


To to this you must keep your reaction vessel temperature cool. If you don't have cooling then you will be making chlorate.
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NEMO-Chemistry
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[*] posted on 7-7-2016 at 06:27


Do you have a pic of the chloroform you made? Sounds a bit like my last batch, i ended up washing mine with potassium carbonate solution (almost saturated) then distilled.

But i could be talking utter bollocks without a pic to see if it was like mine. I now get my bleach from a local company that sells cleaning products, i buy 5 ltr for £1.75 no frills plain bleach. Say's 12% on the container but i buy the stuff almost out of date so maybe its slightly weaker, hence the low price :D.

The place i was buying acetone from has stopped selling it in the last 2-3 weeks! now they do an alternative thats utter crap! I am trying to make chloroform via IPA i found on a thread here.

So far it seems to be working! Yield seems a bit lower but hardly ANY rise in temperature from the reaction, i will post it up once i done a second run.

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aga
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[*] posted on 7-7-2016 at 09:08


In every case of making chloroform it seems that distillation is always required to obtain a relatively pure product.



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NEMO-Chemistry
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[*] posted on 7-7-2016 at 09:17


Quote: Originally posted by aga  
In every case of making chloroform it seems that distillation is always required to obtain a relatively pure product.

I will see if i can find the vid again, the washing step seems to clear the milky colouring you sometimes get on the chloroform.

Although subjective the washed and distilled chloroform 'seems' cleaner/purer than plain distilled, but no proof of that.

I think the milky part is water? its normally in kind of patches around the outside of the blob of chloroform.

Distilled chloroform has a real sparkle to it, i noticed over time this goes a bit, if i have any around long enough to loose the sparkle i normally re-distill when i make another batch.

I am pretty sure the video will be a nurdrage/nile red or myst vid, it might be from someone else but i tend to stick to the well known ones like chemplayer and the guys from here.

Acetone is suddenly hard to get locally, no idea why that is. Everyone seems to have switched to the mickey mouse version.

Oh and evostick contact adhesive!!! Couldnt find any locally at all.

[Edited on 7-7-2016 by NEMO-Chemistry]
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D2DT
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[*] posted on 13-7-2016 at 04:37


Hi,
Thanks for all the replies. I tried using cheeper bleach which turned out great and the chloroform was clear. The problem with the other bleach I got the smell of chloroform but there was a white precipitate mixed with it below the water layer. Must of been some kind of additive, Anyway at last now the cheeper bleach works so i have some chloroform for extractions :)
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