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By W. T. Elwell

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M . The sample is dissolved in nitric acid, and the solution is then fumed with sulphuric acid and potassium hydrogen sulphate; hydrazine sulphate is added to reduce arsenic to the trivalent state. Arsenous chloride is distilled and titrated with a standard solution of potassium bromate, using methyl-orange indicator. Provided that the distillation temperature does not exceed 105°C, antimony does not interfere. 2). 2 the sample is dissolved in a hydrochloric acid/ hydrogen peroxide mixture; pentavalent arsenic is reduced with hypophosphorous acid, and an empirical extraction of arsenous chloride into chloroform is made.

Add, separately, 0-5,1-0, 1-5, 2Ό, 3 0 and 4 0 ml of the standard aluminium solution (1 ml = 0 0 1 mg Al) to six 100-ml calibrated flasks. A d d to each (and a blank), 1-5 ml of copper sulphate solution ( l m l Ξ 1-0 mg Cu), and dilute each solution to about 25 ml. Proceed with each solution as follows : Add 2 ml of thioglycollic acid ( 1 + 2 5 ) and 15Ό ml of the aluminonbuffer composite solution, then stand the flask in boiling water for exactly 5 minutes. Remove the flask from the water-bath, cool to room tempera- 33 ALUMINIUM ture, then transfer to a cold-water bath ( 2 0 ± 2 ° C ) for 20 minutes.

Dilute the solution to 1 litre. Standardise the solution against the standard aluminium solution, as follows : Dilute a 25-ml aliquot of the standard aluminium solution (1 ml Ξ 1-2 mg Al) to about 100 ml, add about 30 ml of the EDTA solution (0-05 M), about 5 ml of the standard copper solution (0Ό5 M) and 2 to 3 drops of methyl-red solution, then continue as described in the Procedure. 2. Procedure. Transfer 0-3 g of the sample (Note 1) to a beaker (250ml), and add 10ml of sulphuric acid ( 1 + 3 ) and 2 m l of cone, nitric acid.

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