making chloroform attempt 2
This is a direct continuation on previous post which ended in a failure. I won't be repeating on the descriptions i've made about the process itself.
Reagents used:
- solution of sodium hypochlorite
- acetone
- ice
bleach
I've bought a 5L 15% sodium hypochlorite solution that together with the container weighted 5084g
To weight the empty container i've transferred the solution to a bucket, it had beautiful piss yellow color that was clearly different from bleach in previous attempt. The smell was like toned down musky chlorine and was surprisingly faint.
The empty container has weighted 186g
Part of it was saved into a 1L bottle since otherwise there wouldn't be enough space to perform the reaction
After that the vessel weighted 4187g, so there was 4187-186 = 4001g of the solution used for the reaction
which amounts to (4187-186)*0.15 = 600.15g of sodium hypochlorite ( 600.15/(23+35.45+16) = 8.06 moles )
amount of acetone
8.06*0.95/3 = 2.55 moles of acetone ( 8.06*58.08 = 148.26g)
then the theoretical amount of chloroform produced should be 2.55*(12+1+35.45*3) = 304.66g
preparations
I've wrapped the vessel in plastic wrap and put it into a couple plastic bags to avoid leakage and i've put it into a food freezer for the night (should have been chilled up to -19C).
I have to say it was quite a not ideal situation since if it was to leak i'd have a lot of food contaminated in piss like chlorine water
reaction
Acetone was measured out
and after taking the vessel from the freezer and unpacking it i've immediately started pipeting in the acetone, capping the container and mixing from time to time. After adding about half of the acetone the temperature has risen to about 20C and i've put the vessel into an ice bath
But i've found it to be more efficient to add the ice directly into the container instead of water.
The mixture has become cloudy and chloroform layer started separating on the bottom, i took a picture of it being tilted but absolutely nothing is visible on camera :/
After waiting 10 minutes for things to settle i've started decanting it, which didn't make it more visible for the camera.
I've transferred it into a water bottle (made of PET) and washed it 2 times with water
But that was stupid for 3 reasons:
- i should have added sodium chloride to the solution before decanting so that more of chloroform would settle to the bottom
- chloroform is quite soluble in water (8.6g per litre at 20C) so i've got rid of my product by washing it with too much water
- chloroform started dissolving the PET
I've washed it again with dilute sulfuric acid to get rid of sodium hydroxide that would eat the chloroform, and transferred it to a polypropylene yogurt cup decanting most of the water.
So i've 181.5-10.6 = 170.9g of dirty chloroform, which amounts to 56.09% yield. Quite bad but better than i've initially though since density of chloroform is quite high (1.489g/cm^3).
I didn't bother with distilling such a small amount though. I've just moved it into an old soy sauce bottle
conclusion
Making chloroform through sodium hypochlorite is expensive and requires handling large volumes of liquids for small amounts of product. In the future i'll attempt making chloroform though calcium hypochlorite route.
Here's some discussion about it: https://www.sciencemadness.org/whisper/viewthread.php?tid=158939#pid677069 https://www.sciencemadness.org/talk/viewthread.php?tid=65712 https://www.sciencemadness.org/whisper/viewthread.php?tid=159821#pid686900