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Reagents and equipment.

Cerium (IV) sulphate solution, 0.1 N . A stock solution of cerium (IV) sulphate was prepared by slurring 438.6 g of primary standard grade ammonium hexanitratocerate (IV) in 450 ml of concentrated sulphuric (VI) acid and slowly diluting with water to 8:1 while stirring vigorously. After standing for 2 days a significant amount of precipitate formed, and the solution therefore was decanted. It was standardized against arsenious oxide using osmium tetroxide (osmium (IV) oxide) as a catalyst, and against electrolytic iron, and found to be 0.1000 N. This value was confirmed by subsequent restandardization at intervals throughout the work.

Oxidations were carried out in 300 ml conical flasks equipped with special condenser heads to prevent loss of material by spattering and reduce the escape of perchloric acid into the atmosphere by condensing the vapours in the neck of the flask.

Samples containing 4-5meq of cerium were taken for each oxidation so that subsequent titrations could be carried out using an ordinary 50-ml Normax burette. The same burette was used for both titrations and measuring sample solutions to eliminate errors in glassware calibration.

Lesson 8

Part 1

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