Distilling Nitric Acid from Household Supplies

Read the following warning:

Nitric acid (\(\ce{HNO3}\)) is

  • Toxic and corrosive if ingested or contacted
  • Releases toxic \(\ce{NO2}\) gas which can cause injury
  • Handled in cool, ventilated areas

Everything done in this post it outside with proper ventilation and proper safety equipment and shouldn’t be replicated.


Preparation

I have been wanting to perform distillation for a while now, but never had the supplies or experience needed. Distillation was only something of theory in my chemistry class. But recently, I got my hands on a distillation kit along with accompanying glassware.

In fact, here is an image of my whole setup:

home lab supplies

Ingredients + Supplies:

  • 500 mL distillation flask
  • Graham condensor
  • Various size beakers
  • 10 mL gradulated cylinder
  • Respirator, blast shield, goggles, etc.
  • Hot plate and broken unglazed pottery
  • Thermometer
  • Calcium-Ammonium Nitrate (fertilizer)
  • 32 fl. oz. sulfuric acid (drain cleaner)

Reaction and Collection

To produce nitric acid, the following reaction is performed:

\[\ce{H2SO4 (aq) + Ca(NO3)2 (aq) -> 2HNO3 (aq) + CaSO4 (s)}\]

from the sulfuric acid in the drain cleaner and calcium nitrate in the fertilizer to produce mostly solid \(\ce{CaSO4}\) as a byproduct. Where calcuim nitrate is found in the form of calcium-ammonium nitrate with the formula \(\ce{5 Ca(NO3)2 . NH4NO3 . 10 H2O}\).

To react about half a bottle of drainer cleaner into nitric acid with a source of about 93% sulfuric acid (10 fl. oz. is about 296 mL) with a density of about \(\ce{1.82 \pu{g/mL}}\), a total of

\[296 \pu{mL} \textnormal{ cleaner} \times \frac{0.93 \ce{\pu{mL} H2SO4}}{1 \pu{mL} \textnormal{ cleaner}} \times \frac{1.82 \ce{\pu{g} H2SO4}}{1 \ce{\pu{mL} H2SO4}} \times \frac{1 \ce{\pu{mol} H2SO4}}{98.08 \ce{\pu{g} H2SO4}} \times \frac{2 \ce{\pu{mol} HNO3}}{1 \ce{\pu{mol} H2SO4}} \times \frac{63.01 \ce{\pu{g} HNO3}}{1 \ce{\pu{mol} HNO3}} = 643 \ce{\pu{g} HNO3}\]

is made, but requires the addition of

\[10.2 \ce{\pu{mol} HNO3} \times \frac{1 \ce{\pu{mol} NO3-}}{1 \ce{\pu{mol} HNO3}} \times \frac{1 \ce{\pu{mol} CAN}}{10 \ce{\pu{mol} NO3-}} \times \frac{1080.62 \ce{\pu{g} CAN}}{1 \ce{\pu{mol} CAN}} = 1102 \ce{\pu{g} CAN}\]

That means, I need 355mL of drain cleaner and 1102g of fertilizer (~1280g can used since ammonium nitrate is present) to get ~670mL of azeotropic nitric acid (68% concentration at \(\ce{1.42 \pu{g/mL}}\)). The percent yield will obviously be lower due to decomposition, reaction kineitcs, and improper distillation.

But to the distillation, we need to set up a safe environment, proper heating, and proper collection.