By W. T. Elwell

ISBN-10: 0080121608

ISBN-13: 9780080121604

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3. Procedure. a blank on the reagents—this should include 1 g of copper. To 1 g of the sample (Note J) add 5 ml of cone, hydrochloric acid (Note 2), and continue as described under Preparation of Calibration Graph. In the examination of samples containing above about 0-1 per cent of tellurium, proceed as indicated but, after the evaporation to dryness, dissolve the cold residue in 30 ml (in place of 50 ml) of cone, hydrochloric acid. Adjust the temperature of the solution to 20°C, add 3 O m l of hypophosphorous acid (50 per cent w/w), then allow to stand for 5 minutes.

Preparation of Calibration Graph. Transfer 0 1 g of copper to each of six beakers (50 ml) and add to each, 5 ml of cone, hydrochloric acid and 1 ml of cone, nitric acid. Warm gently to assist solution of the copper. g Sb) to five of the beakers; use the remaining solution as a blank. Proceed with each solution as follows: Evaporate on a steam-bath to about 1 ml, then cool. A d d about 5 ml of cone, hydrochloric acid, transfer the solution to a 50-ml graduated separating-funnel, then dilute to 17 ml with cone, hydrochloric acid.

Add 20 ml of cone, nitric acid and evaporate the solution to fumes of sulphuric acid—add more nitric acid to clear the solution if necessary— then cool. Dilute the solution to about 200 ml, boil until soluble salts are dissolved, add 10 ml of tartaric acid solution (50 per cent), a few drops of methyl-red ALUMINIUM 29 solution, then ammonia solution until the colour of the solution is yellow. Heat the solution to 50 to 55°C, and precipitate aluminium with 8hydroxyquinoline potassium sulphate solution (5-5 per cent); use 0-7ml per mg of aluminium present, and an excess of 5 ml over this calculated volume.

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Analysis of Copper and its Alloys by W. T. Elwell

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