By Ross W. Moshier
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Extra resources for Analytical Chemistry of Niobium and Tantalum
Add a little filter paper pulp and allow to cool before filtering. The mixture may be allowed to stand overnight if sufficient time is not available for filtration. Filter through a 9 cm close texture filter paper and wash 8 times with a cold 4 per cent hydrochloric acid solution. Char and ash the paper and precipitate in a platinum crucible at 600° until the carbon has completely disappeared. Moisten the residue in the crucible with water, add 3 ml of 50 per cent sulfuric acid and 3 ml of concentrated hydrofluoric acid, and heat moderately until solution is complete.
The filtrate is brought to boiling and more tannin solution is added dropwise to produce an orange precipitate. The precipitate is a mixture of tantalum-niobiumtannin and becomes progressively more red as the precipitation proceeds. When the precipitate formed on further addition of tannin solution is definitely red the tannin addition is stopped, and the precipitate is filtered off and washed. The filtrate contains only pure niobium and is preserved. The precipitation process must now be repeated on the orange precipitate.
Ignite the paper and residue and then fuse and dissolve as above. Filter off any undissolved material, wash the filter with water, and discard the paper. The combined filtrates and washings should contain 3 g of tartaric acid and have a volume not greater than 85 ml. 5 ml of 10 per cent oxalic acid dihydrate solution, and immediately 25 ml of 10 per cent selenous acid solution. Dilute the mixture to 150 ml with water. Cover the beaker and digest on a steam bath for 3 hr, add filter paper pulp, and filter through a dense paper.
Analytical Chemistry of Niobium and Tantalum by Ross W. Moshier