Transfer by pipette into the dry flask of the apparatus (5.2) a portion of filtrate (7.1) containing a maximum of 20 mg ammoniacal nitrogen. Connect up the apparatus. Place in the 300 ml Erlenmeyer flask 50.0 ml standard 0.1 N sulphuric acid solution (4.14) and an amount of distilled water such that the level of the liquid is about 5 cm above the opening of the intake tube. Introduce through the side neck of the reaction flask distilled water so as to bring the volume to about 50 ml. Shake. To avoid foaming during aeration add several drops of octan-l-o 1 (4.15). Add 50 ml saturated potassium carbonate solution (4.16), and immediately begin to expel the ammonia thus released from the cold suspension. A strong current of air is necessary (flow rate of about 3 litres per minute) and should be purified by passing it through washing flasks containing dilute sulphuric acid and dilute sodium hydroxide. Instead of using air under pressure, a vacuum may be used (water pump) provided that the connections between the apparatus are air tight. The liberation of ammonia is generally complete after three hours. However, it is desirable to make certain of this by changing the Erlenmeyer flask. When the process is finished, disconnect the Erlenmeyer flask from the apparatus, rinse the end of the intake tube and the walls of the Erlenmeyer flask with a little distilled water, and titrate the excess acid against standard 0.1 N sodium hydroxide solution (4.17).

See 7.2.3.