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By W. T. Elwell

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Many colorimetric reagents are available for this 42 BERYLLIUM purposed 7 31 43 but none is specific, and a preliminary isolation of beryllium is usually necessary. -nitrobenzene-azo-orcinol in a buffered ( p H 12-7) s o l u t i o n , [ 7 4 , 7 5 ' ' ' 7 6] separation of interfering elements is made by a mercury-cathode electrolysis. The presence of up to 1-5 per cent of aluminium or 0-1 per cent of t i t a n i u m or zirconium, does not interfere. Interference from the trace of copper remaining after a mercury-cathode electrolysis is eliminated by the presence of E D T A .

M . , and the complete scheme of analysis is as follows: After the precipitation (and filtration) of arsenic, selenium and tellurium with hypophosphorous acid, antimony and bismuth remaining in solution are deposited on to copper foil (Reinsch reaction), and are afterwards recovered by solution in sodium peroxide. Copper (from the foil) and bismuth are precipitated as sulphides, and antimony is determined colorimetrically as the pyridine/iodide complex. The precipitate of elemental arsenic, selenium and tellurium is dissolved, selenium is precipitated with hydriodic acid, recovered and oxidised to selenous acid; the trace of copper invariably present in solution is removed as the cobalticyanide, and the determination of selenium is completed iodometrically.

Procedure for Aluminium Contents above 2 per cent. Transfer 0-25 g of the sample to an Erlenmeyer flask (500 ml), and add 5 ml of nitric acid ( 1 + 1 ) . Warm to assist solution of the sample and to expel oxides of nitrogen, then dilute the solution to about 25 ml. If a precipitate is present, filter it off on to a small filter pad and wash with hot nitric acid (1 + 2 0 0 ) . Dilute the solution to about 100 ml. A d d ammonia solution until a permanent precipitate is just formed, re-dissolve the precipitate with a slight excess of hydrochloric acid ( 1 + 1 ) , then add 2 drops of the acid in excess.

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