Division 1.1.2 Determination of BaO
United Kingdom
Weigh, to within 0·0001 grammes, about 0·5 grammes of powdered glass and place in a platinum dish. Moisten with water and add 10 millilitres of hydrofluoric acid and 5 millilitres perchloric acid. Heat in sand bath until white fumes are given off.
Allow to cool and add a further 10 millilitres hydrofluoric acid. Heat until reappearance of white fumes. Allow to cool and rinse the sides of the dish with distilled water. Heat again and evaporate until almost dry. Start again with 50 millilitres of a 10% solution of hydrochloric acid and heat gently to aid dissolution. Transfer to a 400 millilitres beaker and dilute to 200 millilitres with water. Bring to boil and pass a current of hydrogen sulphide through the hot solution. When the precipitate of lead sulphide drops to the bottom of the beaker, turn off the hydrogen sulphide. Pass through a fine filter paper and wash with cold water saturated with hydrogen sulphide.
Boil the filtrates and then, if necessary, reduce them by evaporation to 300 millilitres. Add to boiling mixture 10 millilitres of a 10% solution of sulphuric acid. Remove from heat and leave to stand for at least four hours.
Pass through a fine filter paper, wash with cold water. Calcine the precipitate to 1050 °C, and weigh the BaSO4.