By Ross W. Moshier
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Additional info for Analytical Chemistry of Niobium and Tantalum
Digest the cooled fusion product with 10 ml of halfsaturated sodium chloride solution on a hot plate for 5 min. Allow to stand for 2 hr at room temperature. Stir in a small quantity of filter pulp, and filter on a bare funnel containing a tightly packed pad of filter pulp in its apex. Wash the filter with 2 ml portions of half-saturated sodium chloride solution until the washings show little trace of alkalinity. Rinse the pulp into a 50 ml beaker, acidify with hydrochloric acid, and digest for 30 min to remove the sodium from the precipitate and paper.
Precipitate the zirconium by the addition of excess of a 1 per cent solution of salicylhydroxamic acid in hot water. 5 using 4N ammonium hydroxide and a pH meter or suitable indicator. 1 per cent salicylhydroxamic acid and 1 per cent ammonium nitrate. Ignite the paper and precipitate. It is advisable to dissolve the precipitate and reprecipitate the zirconium to remove traces of coprecipitated niobium. The final precipitate is ignited to constant weight and weighed as zirconium oxide. For recovery of the niobium the filtrate and washings are combined, evaporated to a volume of 200 ml, and boiled until all of the hydrogen peroxide has been decomposed.
Dilute the residue to 180 ml with water, and disregard any light-to-black precipitate. 2 g of ascorbic acid, and heat the mixture to boiling. Add 10 ml of a freshly prepared 1 per cent aqueous tannin solution dropwise with continuous stirring. Tungsten coprecipitates at this point; however, niobium is freed from the large quantity of other metals present in the steel. Maintain the solution at the boiling point for 3 hr to permit complete coagulation of the precipitate. Add a little filter paper pulp and allow to cool before filtering.
Analytical Chemistry of Niobium and Tantalum by Ross W. Moshier