New PDF release: Analytical Chemistry of Niobium and Tantalum
By Ross W. Moshier
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Additional info for Analytical Chemistry of Niobium and Tantalum
If the precipitate is dirty grey it is zirconium, beryllium or aluminum; if brown it is uranium. When the presence of titanium and niobium is indicated a further precipitation with a little tannin and ammonium hydroxide is required. A reprecipitation purification is necessary by repeating the complete process, starting with the fusion of the ignited and weighed precipitate from above. After the second ignition in a porcelain crucible, wash the precipitate into a 50 ml beaker, add 1 ml of I N hydrochloric acid, digest on the water bath for 30 min to dissolve soluble alkali salts, and then make the solution ammoniacal.
Add 3 ml of perchloric acid and continue heating until dense white fumes are evolved. When cool, dilute with 100 ml of water containing 1 g of EDTA, add 3 drops of methyl orange solution, and adjust the acidity with ammonium acetate until the indicator is just yellow. Dilute to about 300 ml with cold water, and cool the beaker and contents to 10° in an ice bath. Precipitate the titanium by the slow addition of a 5 per cent aqueous cupferron solution with vigorous stirring. Excess cupferron is present when the crystals of cupferron formed at the point of addition redissolve and leave no turbidity.
Weigh accurately a 50-60 mg sample of tantalite ore; a semimicrobalance should be used. 5 g of potassium pyrosulfate in a silica crucible of capacity 50 ml. 5 g tartaric acid. Uninterrupted stirring is necessary in the dissolution process to prevent the local hydrolysis of tantalum at the surface of the pieces of the melt. Any material which resists dissolution consists principally of stannic oxide and silica but may retain some tantala. Filter on a small paper and wash twice with water. Ignite the paper and residue and then fuse and dissolve as above.
Analytical Chemistry of Niobium and Tantalum by Ross W. Moshier