Warning: Diethyl ether is highly flammable, fire safety protocols must be in place.
Greetings fellow nerds.
Diethyl ether is a very famous and commonly used solvent in chemistry labs.
It's non-polar and has a very low boiling point of just 34.6 degrees celsius.
Lower than human body temperature.
So that makes it easy to remove from chemical reactions by boiling it off.
This is tremendously useful for solvent extractions.
Additionally it's not very reactive, but polar enough that it can support grignard reactions.
I want diethyl ether for both purposes.
Now diethyl ether can be made from sulfuric acid and ethanol but a much more accessible source is car starter fluid.
This is a usually a mixture of diethyl ether and n-heptane.
Other sources may have other components but almost all of them have diethyl ether.
If you buy these cans in bulk, this can be a far cheaper source of diethyl ether than making it yourself.
Now to separate out the ether we're going to distill it.
First spray the contents into a flask.
Mine didn't come with a spray straw so i'm using this distillation adapter to direct the spray into the flask.
This is completely optional though.
I'm just doing it because it lets me hold the can upright.
I'm wearing a glove because the can was previously cooled in a freezer overnight to lower the temperature.
This is to help reduce evaporative losses.
Nonetheless some will escape so do this outside or in a fume hood.
Anyway, here is our flask of car starter fluid.
Now to separate out the ether by distillation.
Set up a fractional distillation apparatus around the flask.
Now the cooling water you use should be ice cold so i recommend using an ice water reservoir.
Diethyl ether has a low boiling point of 34.6 degrees celsius so room temperature cooling water will have diminished effectiveness condensing it.
Now turn on the heating and start distilling.
Start off at a very low temperature and very slowly ramp up.
Diethyl ether is very volatile and it doesn't take much heat to start it boiling.
If you prefer, you can use a warm water bath instead of direct heating on the hotplate.
Now you don't need a fractional distillation setup and simple distillation will work.
But i prefer fractional distillation as heptane is still quite volatile in of itself and a small length of fractional distillation column greatly improves purity.
As you distill the flow will drop and you'll need to raise the temperature as you progress.
Try to keep a constant flow.
Go in small increments and wait for the temperature to stabilize before going further.
Diethyl ether can boil so fast that it blows apart the distillation apparatus.
Considering it has very low autoignition temperature, it can easily catch fire if the vapors find their way to the hotplate.
So go slowly.
It's for this reason that many chemists prefer to boil ether with hot water as hot water is below the autoignition temperature of diethyl ether.
Eventually as you continue to increase the heating in small amounts,
When the temperature shoots up past 70 celsius even though the flow rate is very low you're done distilling diethyl ether and are now starting to distill heptane.
Stop heating and let everything cool.
And here it is, diethyl ether distilled from car starter fluid.
Now a special note about long term storage.
Diethyl ether like most ethers is notorious for reacting with air and light to generate highly explosive organic peroxides as it sits in storage.
This is relatively safe in small concentrations but if you evaporate the ether or distill it off as you would for solvent extractions
then the peroxides would concentrate in the residue and explode.
So don't keep diethyl ether for extended lengths of time.
Use it within several months.
Alternatively, you can store diethyl ether over sodium hydroxide or sodium metal.
You can even use the sodium magnesium oxide aggregate i showed how to make in a previous video.
To be honest though, don't even bother storing your ether separately.
Instead, keep the original can and only distill it out when you want to use it.
Distilling it out and not using it is kinda unnecessary.
In here it's protected from light and more importantly, there is no air, only carbon dioxide propellant.
So it can last for many years without peroxide formation.
Anyway, let's say you have distilled it out and have used it, you might be wondering what to do with the heptane residue.
It's actually a nice clean aliphatic solvent and wonderful for cleaning oily residues and contaminants.
It's very inert and you can even store sodium metal in it.
In fact it's great for washing off the mineral oil from sodium if you want relatively clean sodium for your reactions.
The heptane itself evaporates quickly and can also be distilled out if you prefer.
Being clean and nonpolar it's also an excellent solvent for solvent extractions.
So you can get two very useful chemicals from starter fluid.
I'll be using my diethyl ether for solvent extractions and grignard reactions in upcoming videos.
Thanks for watching.
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