Division 5.3.1 Oxidation
United Kingdom
Weigh to the nearest 0,2 mg from 0,1 to 1 g of the prepared sample (5.1) into:
a 100 ml round-bottomed flask (4.1) for open hydrolysis (5.3.2.3) or,
a 250 ml round-bottomed flask (4.1) if a low sodium concentration is required (5.3.3.1) or,
a 100 ml bottle fitted with a screw cap (4.2), for closed hydrolysis (5.3.2.4).
The weighed sample portion must have a nitrogen content of about 10 mg and a moisture content not exceeding 100 mg.
Place the flask/bottle in an ice-water bath and cool to 0 oC, add 5 ml of oxidation mixture (3.23) and mix using a glass spatula with a bent tip. Seal the flask/bottle containing the spatula with an air-tight film, place the ice-water bath containing the sealed container in a refrigerator at 0 oC and leave for 16 hours. After 16 hours remove from the refrigerator and decompose the excess oxidation reagent by the addition of 0,84 g of sodium disulphite (3.4).
Proceed to 5.3.2.1.