By Ross W. Moshier
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Extra info for Analytical Chemistry of Niobium and Tantalum
Dissolve the melt with about 100 ml of water in a conical flask. 5 g of anhydrous sodium carbonate in the same platinum dish, dissolve it in the minimum volume of water, and add this solution to the sample solution. Boil the solution, allow it to cool, and add 5 g of solid ammonium chloride and 1 g of tannic acid slowly while stirring. Make the solution acid to litmus, and finally add 5 ml of 6N hydrochloric acid in excess. Add 5 ml of cinchonine solution (5 g in 100 ml of 6N hydrochloric acid) and 2 squares of Whatman disintegrated filter pulp.
Filter the mixture on a Whatman No. 40 paper and wash with a cold 1 per cent ammonium hydroxide solution. Ignite the precipitate and filter in the original platinum crucible at 700°. Fuse the residue in the covered crucible with 2 g of anhydrous sodium carbonate at red heat for a period of 15 min. Dissolve the melt in a minimum of water, not more than 100 ml, and transfer the solution to a 250 ml conical flask. 1 g of silica (fused with sodium carbonate). Boil and cool the mixture, add 5 g of ammonium chloride, and add 1 g of tannin while stirring.
1 g of ascorbic acid and dilute the mixture to 85 ml with water. Heat to boiling and reprecipitate the niobium with tannin as described above. Ignite the paper and precipitate in a platinum dish, cool, and fuse the ash with 2 g of potassium pyrosulfate. Dissolve the cooled melt by digesting with 20 ml of 4 per cent oxalic acid solution. Determine the niobium by the double cupferron precipitation as described above in the procedure for the determination of niobium in tungsten-silicon-niobium alloys.