Chemistry Experiment: Synthesis of Chloroform by Distillation

[MrPiano2525]

I like your set up. A few questions.. What height is your vigreux column? What type of condenser is that, jacketed dimroth? Curious.. is it a 19/22 setup?

[ytmachx]

@MrPiano2525 Thanks! All the joints are 24/40. The first condenser is a 600mm Allihn. The Vigreux is also 600mm. The condenser used in the distillation at 1:01 is a Friedrich.

[RealChemLabs]

Great synthesis ytmachx! For another synthesis of chloroform check out our channel, Real Chem!

[deltaxcd]

if this reaction is so slow it takes 2 days to complete why do you care about vapors and heat? At this rate it cant produce any heat.

[ytmachx]

@deltaxcd When the reactants are first combined it creates a great deal of heat, in fact, it is difficult to control and prevent a runaway. The time was given because I did not have mechanical stirring during the initial combination of reactants. I used the two days to agitate the solution from time to time to make sure the reaction was complete.

[crudeoilsystems]

thanks very much for this

[ytmachx]

@crudeoilsystems Thanks! Btw, love your centerfuge!

[tommytintran]

wow cool !!!!!!!!!!!!!!!!

[douro20]

Did you have CaCl2 in the ice bath?

[ytmachx]

@douro20 Certainly not.

[MrSmudger687]

@ytmachx - Given that acetone is highly miscible with water, couldn't you have just washed the chloroform with water several times to get rid of the acetone? Then it would just be standard procedure to dry the chloroform of any residual water.

[glorymashy]

what laborator apparatus used to hold wire gauze while heating ..except tripod???

[ytmachx]

@glorymashy ???

[98JMA]

@ytmachx

Ring stand with ring/clamp?

[aeroscope]

How much does ur kwik fit cost?

[ytmachx]

@aeroscope It really depends on the specific piece. Everything can be found on ebay.

[mikegLXIVMM]

Some uses for Chloroform:

*Glue Plexiglass, Lexan, ABS or Polystyrene plastics together.

*If you collect insects, a small amount of Chloroform on a cotton-ball in a sealed jar will knock it out for good in about five minutes.

*Extract Alkaloids from plant substances.

[mikegLXIVMM]

You say the chloroform after the last step is 97% pure.

Do you know what the impurities are?

Could they be Carbon Terachloride?

[ytmachx]

@mikegLXIVMM Water and acetone mainly and you are correct about the carbon tet.

It is interesting to note that during the first distillation from the reaction mixture, carbon tet can be seen on the bottom of the flask. It appears as a large drop (1-2 cc) of clear liquid on the bottom of the flask in the solution. This is removed in the first re distillation.

[mikegLXIVMM]

@ytmachx I read that Carbon Tet is toxic to the liver and kidneys, I will have to make sure to remove it when I make a batch of Chloroform. -Thanx

[ytmachx]

@mikegLXIVMM Yes, that's right. 

[Phil6590]

So apparently it looks much easier to just pay a chemist to synthesize the stuff needed to knock someone out

[soroka69]

My test was 7Lb of 10%NaClO (hydrochloride) (pool cleaner) and 650ml of acetone . My yield was 550ml of chloroform. The problem I could not keep temperature below 50degrees Celsius. Keep temperature down! ! ! Add acetone slower! ! ! For best result freeze acetone (hold it in the freezer for a day or so)! ! ! If you can cool the bleach to, before put it into reaction. You will experience the large loses of chloroform if you let temperature to rise over 55 degrees Celsius

[ytmachx]

That is why there is an ice bath and reflux condenser.

[soroka69]

Hello.

I use Ice and Salt mixture...

I think that I add acetone to fast...

Did this by molar weight + more for good measure

Next step is to get addition funnel so I can control amount of acetone per minute added to bleach.

Thank you.

[arkfussion]

does chloroform evaporate befor the acetone?

[ytmachx]

I don't think so. The bp of acetone is 56.5C and the bp of chloroform is 61.1C

[arkfussion]

K thanks! nice apparatus. My Ap chem teacher just gave me a whole lot of distillation equipment! so happy!

[GingyPno123]

@ytmachx Whats the reaction?

[ytmachx]

@GingyPno123 ???

[ytmachx]

@GingyPno123 It is called the Haloform reaction.

[GingyPno123]

@ytmachx I mean the chemical reaction. Example: 2K + 2H2O=2KOH +H2

[haxforcandy]

Do you dry it with Magnesium sulfate after you separate the two layers or just leave it as is?

[ytmachx]

I just left it after settling the water out. I think maybe 3a molecular sieves would be the best drying agent.

[haxforcandy]

sounds good, hey do you have any books to recommend?

[ytmachx]

I did use an excess of hypochlorite. It just didn't fully react. Why don't you post a video and show us how you do it?

[bcubed72]

Bleach+acetone in an empty gal. wine jug is how I roll. 7.25:1 NaOCl/acetone gets the job done nicely.

My fractional distillation setup is Cu, not glass, and I don't want to run anything non-potable thru it.

[ExClUr]

The distlillation requires heating up the chloroform, right? Isn't that dangerous, it could react with oxygen and form phosgen, could it not?

[ytmachx]

It could, if it got hundreds of degrees hotter. Distillation only takes 60-80 degrees

[ExClUr]

That's odd because normally chloroform reacts with oxygen into phosgen under room temperature in the presence of light. Or at least so I read. I though increasing the temperature to the boiling point which is about 60°C would speed up the reaction.

[ytmachx]

It takes a long time to decompose to phosgene and the distilling temp is not a significant enough increase in temp.

[ytmachx]

I think it was 6lbs hypochlorite and about 500/600ml of acetone. Yeild ca. 450ml

[quantumdude]

97 % CHCl3 out of how much acetone and calcium hypochlorite ? What is the quantitative yield ?

[ytmachx]

Chloroform is an excellent solvent for extraction, isolation and purification.

[megafeltch]

what is chloroform good for? in chemistry