Introduction
You can find two synthesis method of Nitric acid in this topic. The first one have more common reagents such as sodium nitrate and sodium bisulfate monohydrate, which are very spread, this path gives good yield 95%! Second method from conc. sulfuric acid (96%) and ammonium nitrate has the same easy level, but need hard to obtain sulfuric acid. Nevertheless, second way give ~90% (fuming nitric acid) with great yield.
Safety note: You must have proper PPE including a face shield, chemical resistant apron, and chemical gloves. This again should be done in a fume hood. NO2 Vapors can cause cancer, nitric acid may cause chemical burns on skin and mucous membranes. Can call fire and explosion under high pressure and temperature. Pay a lot of attention to safety notes!
Safety note: You must have proper PPE including a face shield, chemical resistant apron, and chemical gloves. This again should be done in a fume hood. NO2 Vapors can cause cancer, nitric acid may cause chemical burns on skin and mucous membranes. Can call fire and explosion under high pressure and temperature. Pay a lot of attention to safety notes!
Boiling Point: 68% solution boils at 121 °C/760 mm Hg;
Melting Point: -42 °C;
Molecular Weight: 63.012 g/mole;
Density: 1.51 g/cm3, 1.41 g/cm3 [68% w/w];
Index of Refraction: 1.397 (16.5 °C);
CAS Number: 7697-37-2.
From sodium nitrate and sodium bisulfate monohydrate
Equipment and glassware:
- 0.5 L flat-bottomed distillation flask;
- Distillation apparatus;
- Retort stand and clamp for securing apparatus;
- Glass rod;
- Magnetic stirrer with heater;
- Laboratory scale (1 - 100 g is suitable);
- 500 ml x2; 100 ml x2 Beakers;
- 250 ml Erlenmeyer flask;
- Glass bottle (dark glass).
Reagents:
- 43 g, 0.53 mole sodium nitrate (NaNO3);
- 150 g, 1.09 mole sodium bisulfate monohydrate (NaHSO4*H2O).
Procedure
1. Place 43 g (0.53 mole) sodium nitrate (NaNO3) and 150 g (1.09 mole) sodium bisulfate monohydrate (NaHSO4*H2O)(excess) in a 0.5 L flat-bottomed distillation flask, mix thoroughly with a glass rod;
2. Place the anchor from the magnetic stirrer into the flask;
3. Assemble the distillation apparatus: install the Liebig straight condenser through the Würz nozzle, flask connector and 250 ml receiving flask (Erlenmeyer flask fits);
4. Turn on Liebig condenser chilling and start stirring;
5. Start heating (about 120 °C), after the start of the reaction, brown gas starts to form and distillation begins;
6. Stop heating as soon as nitric acid stops dripping into the receiving flask;
As a result of the experiment, nitric acid with a concentration of about 75% will be obtained, the yield is 95%. Calcium nitrate can be used instead of sodium nitrate, it is not recommended to use ammonium nitrate due to its explosiveness.
2. Place the anchor from the magnetic stirrer into the flask;
3. Assemble the distillation apparatus: install the Liebig straight condenser through the Würz nozzle, flask connector and 250 ml receiving flask (Erlenmeyer flask fits);
4. Turn on Liebig condenser chilling and start stirring;
5. Start heating (about 120 °C), after the start of the reaction, brown gas starts to form and distillation begins;
6. Stop heating as soon as nitric acid stops dripping into the receiving flask;
As a result of the experiment, nitric acid with a concentration of about 75% will be obtained, the yield is 95%. Calcium nitrate can be used instead of sodium nitrate, it is not recommended to use ammonium nitrate due to its explosiveness.
From sulfuric acid and ammonium nitrate
Equipment and glassware:
- 500 ml x2; 100 ml x2 Beakers;
- 500 ml Boiling round bottom flask;
- Distillation apparatus;
- Retort stand and clamp for securing apparatus;
- Glass rod;
- Oil bath;
- Laboratory grade thermometer (50-250 °C);
- 250 ml Erlenmeyer flask;
- Glass bottle (dark glass);
- Laboratory scale (1 - 100 g is suitable).
Reagents:
- Concentrated (96%) sulfuric acid (H2SO4);
- Dry ammonium nitrate (NH4NO3).
Procedure
1. Roughly 5 g of concentrated (96%) sulfuric acid (H2SO4) are added to every 4 g of dry ammonium nitrate (NH4NO3) prills used. The mixture is stirred until no solid remains. Ensure that the prills are fully dissolved before attempting to distill them. This action is very fumy and requires reliable ventilation.
2. The slurry is poured into the boiling round bottom flask (500 ml) while a hot oil bath (175-190 °C) waits below.
3. The apparatus is capped and lowered into the hot oil. install the Liebig straight condenser through the Würz nozzle, flask connector and 250 ml receiving flask (Erlenmeyer flask fits). Be sure to grease the glass joints of your apparatus with silicone grease. Temperature control is the key to not burning your laboratory down.
4. After several minutes, a condensation front appears and is driven upwards by heat. The acid is seen refluxing as it condenses on the arm of the distillation flask. Fumes are displacing air and nitrogen dioxide, caused by oxygen reaction with nitric oxide being produced by thermal decomposition.
5. After a few minutes, you will notice that the drip rate of acid out of the condenser has become slow and irregular. At about this point, turn off the hot plate and let your apparatus sit for a few minutes to finish up.
6. Transfer acid to a bottle (plastic is not appropriate). Your nitric acid has turned yellowish from exposure to atmospheric oxygen. It is still very pure, ~90% (fuming nitric acid) as determined by a density table.
2. The slurry is poured into the boiling round bottom flask (500 ml) while a hot oil bath (175-190 °C) waits below.
3. The apparatus is capped and lowered into the hot oil. install the Liebig straight condenser through the Würz nozzle, flask connector and 250 ml receiving flask (Erlenmeyer flask fits). Be sure to grease the glass joints of your apparatus with silicone grease. Temperature control is the key to not burning your laboratory down.
4. After several minutes, a condensation front appears and is driven upwards by heat. The acid is seen refluxing as it condenses on the arm of the distillation flask. Fumes are displacing air and nitrogen dioxide, caused by oxygen reaction with nitric oxide being produced by thermal decomposition.
5. After a few minutes, you will notice that the drip rate of acid out of the condenser has become slow and irregular. At about this point, turn off the hot plate and let your apparatus sit for a few minutes to finish up.
6. Transfer acid to a bottle (plastic is not appropriate). Your nitric acid has turned yellowish from exposure to atmospheric oxygen. It is still very pure, ~90% (fuming nitric acid) as determined by a density table.
The Complete Aqueous Nitric Acid Solutions Density-Concentration Calculator: https://www.handymath.com/cgi-bin/nitrictble2.cgi?submit=Entry
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