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Preparation of liquid nitrogen dioxide - Video Tutorial

Preparation of liquid nitrogen dioxide

Today we're celebrating our 1000th Kimplaheer channel subscriber, and as a reward this video

here we've got some old foreign currency left over from an exotic vacation

sadly we will be unlikely to return to the beautiful country for a while

but the coins are made of cut pro nickel

which is seventy percent copper so we'll have to put them to a chemical use

let's first do a quick test

this is 68 percent concentrated nitric acid

and a coin

and a coin

yeah this works

the brown fumes are nitrogen dioxide with a boiling point of around 20

degrees

see it should be possible to prepare liquid nitrogen dioxide so we rigged up

a special apparatus we've got the 500 mil to neck flask and we've got the

large neck stopper and the small neck leading to an adapter the large neck

will fit our coins

the adapter then leads to a tube and condenser

and then we've got the receiving adapter and a small flask sitting in a bowl

we've also got a takeoff using an old nasty bit of plastic tubing and this

leads up to our extractor and means we hopefully won't die of nitrogen dioxide

poisoning use ventilation this stuff is very toxic and unpleasant we've got some

loose cotton and a coin inside the bottle this process is extremely difficult to achieve a

We'll open the adapter, and we've covered this with a few centimeters deep of anhydrous calcium chloride.

This will hopefully absorb moisture and stop any acid aerosol from getting into our product.

We've got the condenser hooked up to ice water for cooling.

And we've got the receiving flask in a bath of ice and water.

Okay, so that's our setup. Not too complex.

Here's our large-scale acid. 100 mils of 68% concentrated nitric acid.

Let's get this into the flask.

And now we're just waiting for the temperature to drop.

Okay, so, here we are in our ice bath to drop nicely and level out.

The reaction is exothermic, so we've got the reaction flask sitting in a bowl of water to moderate the temperature a bit.

Okay, let's get on with the show.

The reaction kicks off fast with lots of brown nitrogen dioxide gas coming off.

At the other br…

we've initially got a lot of brown gas escaping and being drawn away by the

extractor and we then start to see the gas escape die down and a dark colored

liquid is condensing into our receiving flask

the reaction in the flask is vigorous and produces quite a lot of heat the

liquid collection starts to slow down after a few minutes

it looks like our drying setup is working as well

and our ice baths are still nice and cold

distillation has stopped so we're going to add a couple more coins to the flask

again

as before we've initially got some brown gas

emitted and then we're going to add a couple more coins to the flask again

but then soon after we start receiving the liquid again this is rather

interesting and we'll come back to this later on nitrogen dioxide actually

exists in an equilibrium between the single nitrogen dioxide species and the

timer species which is known as di nitrogen tetroxide at lower temperatures

and the timer species which is colorless his favorite and you can see hearing our

apparatus as the gas passes through our image we can see that our brown gas is

into the chilled condenser it changes to a paler color.

We've also got a little of the liquid condensing at the top here.

You can see it's actually got a blue color to it.

The reaction with nitric acid also produces some nitrogen monoxide, or nitric oxide.

Although it's not supposed to happen except for at low temperatures, we seem to have some

of the nitric oxide reacting with the brown nitrogen dioxide to form dinitrogen trioxide,

which is then obviously soluble in the liquid nitrogen dioxide.

Although liquid nitrogen dioxide contains a lot of colorless dinitrogen tetroxide, when

pure it's still a dark brown color.

Dinitrogen trioxide however is blue.

You can see the blue color quite clearly in the receiving adapter.

We added two more coins, making six in total, and continued to collect the blue colored

distillate.

The temperature of the reaction has raised our water bath temperature a bit, but it's

under control.

No more distillate coming off now, so it looks like we're done.

We quenched the reaction by adding 100 mils of cold water.

This reduced the gas evolution down to virtually nothing.

We then prepared a solution of sodium carbonate in water, on adding some of this a little at

a time, and restoppering the flask.

We then added a little bit of sodium carbonate in water.

We were able to purge most of the browned gas out of the apparatus.

This is a little safer and easier to dismantle now!

Here's our product.

About six or seven mils of a dark blue liquid which we think is mostly nitrogen dioxide,

but with some dioxide present.

nitrogen trioxide dissolved in it it seems to be fairly stable when cold

and we didn't notice any pressure buildup in the flask with the white

background you can see the blue color a bit more clearly okay now let's do some

experiments first dripping some onto a glass dish at room temperature it

creates producing heavy brown nitrogen dioxide fumes

and soon disappears without a trace

here's some cool water

it doesn't stick around for long as it reacts with the water it heats up

causing it to boil off

as brown fumes again.

The resulting solution containing nitric and nitrous acids is strongly acidic as you can

see here.

If this forms inside your lungs, you are in whole worlds of trouble.

Now for something more exotic.

Here's some solid hypoxylamine hydrochloride.

It's a very vigorous reaction.

We decided not to add the solid to the liquid as it could well be explosive on a larger

scale.

Now some ethanol.

Very pretty miniature explosions.

The liquid remaining has a very strong aldehyde aroma.

That was pretty so let's do it again.

Next, here's some benzyl alcohol.

Not as vigorous as ethanol, but the liquid heats up and there's a very strong almond

aroma of benzaldehyde produced.

Not a very practical synthetic method though.

Finally, ice cold potassium hydroxide solution.

Very vigorous and it looks like most of the product escaped as gas.

Well that's all our experiments done and our product used up.

But it was a very interesting experiment.

We're intrigued by the way that the brown nitrogen.

Too much nitrogen.

Nitrogen dioxide gas comes off the reaction at first but doesn't condense.

Even when the condenser is already ice cold it takes about 10 to 15 seconds and then the

blue liquid is seen.

Maybe somehow it takes the generation of nitric oxide to get the product to actually condense.

Although nitric oxide has a much lower boiling point, perhaps it forms some sort of a seatrope

or abduct with nitrogen dioxide and dinitrogen dioxide which is what we end up with here.

We're interested to hear your ideas and theories.

Thanks for watching.