In this camp layer,
prepare isopropyl nitrate.
This is a pretty simple reaction between sodium nitrite and isopropyl alcohol in acid conditions,
but needs some caution due to toxic gases.
Start by weighing 72 grams of sodium nitrite and dissolve in 120 ml of water.
This will require stirring for a few minutes.
Next, place 90 ml of isopropyl nitrate.
Add isopropanol into a beaker.
I've put a thermometer in to show you the temperature change.
Now carefully add 135 ml of concentrated hydrochloric acid to the beaker.
Use ventilation because this fumes in air, and the mixture will also fume.
Note the increase in temperature.
Chill this mixture before the next step.
Place the sodium nitrate in the beaker.
Get solution in a 500 ml flask, and place in a nice salt bath with magnetic stirring.
Place the chilled alcohol and acid mixture into an addition funnel.
Get the temperature to below 5 degrees and then begin slow addition of the mixture.
Immediately you will see the flask filling with brown nitrogen oxides.
Be sure to use ventilation for this reaction because these are highly toxic.
And to keep the temperature low in the ice bath as the reaction is quite exothermic, especially
to begin with, add ice to top up the bath as necessary.
You'll see a blue color in the flask.
This is the unstable nitrous acid species created by the reaction of the nitrite and
the acid.
This is the reactive species in the reaction.
Note how the brown fumes seem to have disappeared.
This is the reaction.
Complete addition should take 50 minutes to an hour.
The blue color will fade and a yellow oil appears in the flask.
As we open the apparatus up to the air, the brown fumes reappear.
The colorless gas in the flask was actually nitric oxide, which now oxidizes to brown
nitrogen dioxide.
Here's the reaction flask at completion.
Note the salt at the bottom.
You can use sulfuric acid to do this reaction, but the salt buildup is much greater and can
inhibit stirring and reduce the yield.
Filter the salt and pour into a separating funnel.
Remove the bottom aqueous layer.
The important thing now is to remove all trace of acid from the product as this can make
it unstable.
This is the reaction.
First we wash with 40 mils of sodium bicarbonate solution.
Keep the flask cool and take extra care when venting, as pressure will build up.
Drain off the bottom layer and repeat the bicarbonate wash.
The washed product will look like this.
Pour the product into a flask and to dry it, add anhydrous magnesium sulfate.
Remember to keep the flask cool.
Allow the product to cool throughout the process as isopropyl nitrite boils at around 40 degrees
and it's possible to lose product to evaporation.
The fumes are also toxic and will make you feel quite dizzy and potentially give you
a bad headache.
And here's our finished product, 65 grams of isopropyl nitrate corresponding to a 70%
yield from sodium nitrite.
And it's ready!
not shelf-stable long-term and you will notice a pressure buildup in the bottle
over time due to nitrogen oxide generation be sure to relieve the
pressure in the bottle every few weeks in store in a cool and dark place