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This is normal.
I kept heating this for half an hour to destroy all the impurities and make it
clear for the video,
but you dont have to go that far.
As long as its refluxing or 200 degrees Celsius you can inject the catalyst.
The catalyst I'm using is tertiary amyl alcohol.
Lifting the aluminum foil we inject 0.4 mL of it into the top of the condenser
and replace the foil.
Now every ten minutes,
add in an additional 0.1 mL of alcohol for a total of 0.6 mL,
or six times over an hour.
Combined with the initial injection thats a total of 1 mL.
After all the alcohol is injected, let the mixture reflux on its own.
Now in addition to tertiary amyl alcohol, tertiary butanol can be used aswell.
Primary alcohols like methanol and ethanol do not work for this reaction
and neither does secondary alcohols like isopropanol.
Only tertiary alcohols seem to work.
Now as we wait youll noticed these tiny little spheres
that at first look like entrapped bubbles but never seem to pop.
As they get larger and more numerous itll become obvious they are spheres
of potassium.
Youll have to be patient as it can take a couple of hours before these start to
appear.
Whats happening is the magnesium reacts with the potassium hydroxide
to produce potassium metal, hydrogen gas and magnesium oxide.
The alcohol catalyzes this reaction so it can proceed in a solution like this.
As the reaction progresses the alcohol may get consumed in side-reactions.
When this happens the potassium spheres will start to darken in color.
If you wait too long theyll even go black and stop coalescing, forming a sand.
To reverse this, simply inject another 0.1mL of alcohol.
Monitor the reaction and inject alcohol in additional 0.1mL increments if you
see the spheres going dark.
There we go,
I just added the alcohol and you can see the color change as operating
conditions are restored.
The exact interval between alcohol injections is variable
depending on impurities and reaction conditions
and some experimenters find they dont need additional injections at all.
You may ask why dont I add all the alcohol at once at the beginning.
I did experimented a lot with that approach
but after getting rather poor reproducibility I determined,
after several months of research,
that sometimes the alcohol would get consumed in side reactions
at the beginning before any potassium was made.
Occasionally the potassium metal was made but would go dark as the alcohol
ran out
and then would be completely destroyed again, resulting in no yield of
potassium.
This problem does not occur for everyone,
likely because different reagent and solvent grades have different impurities.
So you can try and add all the alcohol at the beginning,
and if it works then go for it,
but if youre having reproducibility issues
then it might be side reactions destroying your alcohol.
Thus I recommend going with the staggered addition as I've demonstrated in
this video.
Okay.
Now as we watch the reaction we see the spheres coalesce into a larger
sphere.
This is a benefit of using a high density solvent like tetrahydronapthelene.
The alcohol helps the coalescence and if you see lots of spheres collecting
but not coalescing
you might be able to help it along by injecting another 0.1 mL shot of alcohol.
But if youre using a lower density mineral oil
then the spheres will just rest on top of the potassium hydroxide and only
rarely come together.
Dont worry I'll show you how to coalesce smaller spheres of potassium later.
Now the reaction is done when there is no more magnesium.
At this point turn off the heating and let it cool.
Here is the reaction mixture after everything has solidified.
You can see many small spheres of potassium resting on the byproducts
and over here is our very large sphere of potassium.
Just scope them out with a spatula or pair of tweezers.
Although if the narrow neck is giving you trouble you can dump out the
mixture into some toluene.
The toluene also helps to wash the potassium
so I recommend dropping into toluene even if you can get the potassium
separately.
If it's really dirty I recommend washing again with fresh toluene.
After washing with toluene,
place the potassium into a clean vial with mineral oil for short term storage.
Now before we test it,
we need to render the rest of our apparatus safe by destroying any potassium
residues.
Place the flask in another beaker to contain any bubbling overflow.
And now add isopropanol to all containers that previously handled potassium.
Please do this slowly.
The isopropanol reacts with any potassium residues and forms potassium
isopropoxide,
which wont catch fire when you dispose of the wastes later and clean your
glassware with water.
Be sure to wait for all bubbling to cease before cleaning up your workspace.
Now I know some of you more foolish experimenters might think it would be
cool
just to quench the leftovers with water directly and watch the resulting
potassium fire.
But please remember we have extremely flammable solvents present,
an uncontrolled potassium fire will end very badly for you.
Okay, Ive cleaned away all the apparatus and solvents so no flammable
vapors are present.
Finally, now we can test our potassium.
With these smaller spheres we can just toss one into water.
Potassium is highly reactive and will spontaneously catch fire.
As for the larger sphere.
Muahahaha....!
So thats how you make potassium.
Now for some additional experimenter notes.
A special note about long term safety.
Do not leave potassium in storage for too long.
The potassium on the left was made today and is shiny and pure
but after storage for a month sometimes potassium will react with air and
moisture
to form a coating of potassium oxides and hydroxides as seen on the right.
The color can range from dark purple to yellow.