By Ross W. Moshier
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Extra resources for Analytical Chemistry of Niobium and Tantalum
Filter off the ferrous sulfide and wash with a solution of ammonium sulfide and ammonium chloride. Acidify the filtrate with acetic acid and boil to remove the hydrogen sulfide. To precipitate the earth acids with tannin, heat the solution to boiling, make it slightly ammoniacal, then just acidic with acetic acid, add 5 g of ammonium acetate and a fresh solution of 1 g of tannin, and boil for 5 min. Allow to stand for two hours on the water bath and then filter on a Whatman No. 41 filter to which has been added a pad of filter pulp.
The precipitate contains the titania and possibly a few milligrams of earth acids. Fuse this residue with 3 g of potassium bisulfate and recover the earth acids with tannin as described above in the pyrosulfate-tannin method. The small earth acid-tannin precipitate obtained is then added to the major precipitate preserved in the silica crucible. Ignite the precipitate at 800° and weigh as pure (Nb,Ta)2C>5. A weighed portion of this precipitate should be assayed for titanium. 01 g of titanium dioxide the entire purification should be repeated, provided that a separation of tantalum DISSOLUTION OF THE SAMPLE 33 and niobium is to be made by the tannin method.
Precipitate the niobium, tantalum and titanium from the solution by the dropwise addition of 5 per cent tannin solution (12 times the amount of tannin as the weight of the sample is required). Stir continually as the tannin solution is added. Digest the mixture on the hot plate so that flocculation occurs. Complete precipitation is indicated when the orange tint of the clear liquid has disappeared. Add more tannin solution in this case. 5 cm Whatman No. 40 filter paper containing a little filter pulp, using gentle suction and a protective filter cone.