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7.—7.1 Weigh to the nearest 0.001 g, 1 g of the prepared sample and place it in the Kjeldahl flask. Add 50 ml 50% sulphuric acid (4.1), 10-15 g potassium sulphate (4.2) and one of the prescribed catalysts (4.3). Heat slowly to drive off the water, boil gently for two hours, allow to cool, and dilute with 100-150 ml water. Cool again, transfer quantitatively the suspension to a 250 ml graduated flask, make up to volume with water, shake and filter through a dry filter into a dry flask.
7.2 According to the variant chosen (see Method 2) transfer with a pipette 50, 100 or 200 ml of the solution to the distillation apparatus and add sufficient sodium hydroxide solution (4.4) to ensure a considerable excess. Distil the ammonia and titrate the excess acid as described in Method 2.
7.3 Make a blank test (omitting only the sample ) under the same conditions and allow for this in the calculation of the final result.
7.4 Before carrying out the analysis, check that the apparatus is working properly and that the correct application of the method is used, using an aliquot part of a standard solution of potassium thiocyanate (4.13), approximating to the concentration of nitrogen in the sample.
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