RI 5242 Spectrophotometric determination of tantalum with gallic acid

"Gallic acid is a sensitive, stable, colorimetric reagent for the determination of tantalum in the range of 2 to 40 µ g.Ta/ml. The method consists of the fusion of tantalum oxide with potassium pyrosulfate and solution of the cooled melt in saturated ammonium oxalate, followed by development of a yellow complex with an ethanolic solution of gallic acid. The tantalum-gallic acid complex absorbs over a broad region in the blue and near ultraviolet. Adverse effects due to interfering ions and solution conditions, such as oxalate concentration and pH, can be minimized by a suitable choice of wave length.by a suitable choice of wave length.A new and sensitive colorimetric method is provided that has been used successfully at the Northwest Electrodevelopment Laboratory of the Federal Bureau of Mines for determining minor amounts of tantalum.INTRODUCTIONThe development of corrosion-resistant alloys at the Northwest Electrodevelopment Laboratory prompted a review of the analytical chemistry of columbium (niobium) and tantahnn. Not only are these elements difficult to determine in small amounts, but tantalum especially lacks both sensitive and characteristic color reactions. Various phenolic compounds have been suggested as colorimetric reagents for tantalum, Quentin and Wagner (10, p. 24B) 1/ recommend the use of tannin. The use of pyrogallol was suggested originally by Krivoshlykov (6, pp. 59-60), whose method recently has been subject to a number of modifications (3, pp. 249-254; 5, pp. 1340-1344; 1, pp. 1803-18oi; 4, pp. 345-350). The yellow coloration produced by pyrocatechol in an oxalate solution containing tantalum may also be used to estimate tantalum ( 11, pp, ll-1-4-148) . The use of hydrogen peroxide has been recommended also (7, pp. 164-165; 9, pp. 926-931).Aside from a lack of specificity and sensitivity, the major failing of phenolic reagents is their susceptibility to air oxidation. The oxidation products are highly colored and absorb in the same spectral region as the tantalum complex. Holding reductants are not completely satisfactory in minimizing this effect. Increasing the acidity, while retarding the oxidation, has an adverse effect on the tantalum sensitivity."