By Ross W. Moshier
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Extra info for Analytical Chemistry of Niobium and Tantalum
As the melt cools rotate the crucible to make it solidify as a thin layer on the sides of the crucible. Dissolve the melt in 50 ml of 6 per cent ammonium oxalate solution by boiling gently. Transfer the solution to a 400 ml beaker. Cautiously DISSOLUTION OF THE SAMPLE 31 neutralize the solution by the dropwise addition of I N ammonium hydroxide until the first turbidity appears. Immediately add two drops of 6N hydrochloric acid so that the solution is red to litmus. Dilute with an equal volume of saturated ammonium chloride solution.
Fuse the sample of the mixed oxides with 15 times its weight of potassium pyrosulfate; but not less than 3 g should be used. Cool and extract the melt with 200 ml of 5 per cent pyrogallol solution. Bring the solution to pH 8 with dilute ammonium hydroxide, heat to boiling, add 15 ml of concentrated hydrochloric acid, and digest on a water bath for 15 min. Allow to stand overnight before filtering. Filter off the flaky precipitate of niobium-tantalum pyrogallate on paper, and wash with 1 per cent pyrogallol solution slightly acidified with hydrochloric acid.
34 ANALYTICAL CHEMISTRY OF NIOBIUM AND TANTALUM TANNIN GRAVIMETRIC METHOD FOR THE DETERMINATION OF TANTALUM AND NIOBIUM IN THEIR MIXTURES—MODIFICATION BY BHATTACHARYA^ A critical examination of the tannin precipitation-separation modificat i o n s ^ ' 16* 1 7 ) of the Schoeller method/ 1 0 , 12 · 1 8 ) has led Bhattacharya to examine the conditions controlling the precipitation of each metal. 0 before the addition of ammonium chloride and tannic acid and heating gave quantitative results for tantalum.
Analytical Chemistry of Niobium and Tantalum by Ross W. Moshier