By Ross W. Moshier
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Additional info for Analytical Chemistry of Niobium and Tantalum
Separation and recovery of niobium and tantalum. Majumdar and Mukherjeeß1'33,34> From Procedure I, the resulting ignited mixed earth acids are fused directly in the silica crucible with 10 times (not less than 2 g) their weight of potassium pyrosulfate. Extract the cooled melt with 50 ml of a 5 per cent tartaric acid solution with constant agitation and warming. 0 by the addition of ammonium acetate solution, and heat the mixture to boiling. Precipitate the niobium by the dropwise addition, while stirring, of a 10 per cent alcoholic solution of N-benzoyl-Nphenylhydroxylamine to the appearance of a white turbidity.
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.
Add 50 ml of 10 per cent calcium chloride solution to the gently boiling solution while stirring. Remove the beaker from the hot plate and continue to stir until the supernatant liquid is clear. Test for complete precipitation by the addition of a little more calcium chloride solution. Turbidity in the supernatant liquid indicates that more reagent is required to complete the precipitation. Filter the hot mixture on an 11 cm paper, and wash with hot 2 per cent sodium salicylate solution until the washings are colorless, denoting that all the titanium salicylate complex has been removed.