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Oscillographic polarography in quantitative analysis. XVI. The determination of ruthenium and osmium

P. Beran, M. Burian, and J. Doležal

Karlova University, Prague.

 

Abstract: cf. CA 55, 15182f; 60, 7447h. In a.-c. oscillographic polarography, an anodic peak at -1.2 v. is formed on the curve dE/dt = f(E) in the presence of Ru in 0.6M HCl + 0.1M NaCl. Thus, it is possible to det. (2-40) × 10-6 g. of Ru in 5 ml. of soln., the peak height being directly proportional to Ru concn. To det. Ru in fission products of nuclear reactors, dissolve the sample contg. (5-80) × 10-6 g. of Ru in HNO3, ext. with Bu3PO4, evap. with addn. of 4 ml. of 2M H2SO4 + 0.1-0.2 g. of NH2OH.HCl to formation of white fumes, dil. with H2O, add 8 ml. of M BaCl2 and 2.5 ml. of M NaCl, make up to 25 ml. with H2O, allow the ppt. to settle 30 min., and measure the anodic peak on the curve dE/dt = f(E). The Ru detn. is possible in the presence of Nb, Zr, U, Pd, and Os. In the presence of Os(IV) in 0.6M HCl + 0.1M NaCl, break occurs on the cathodic branch of the oscillographic curve. Thus, (10-125) × 10-6 g. of Os in 5 ml. of soln. can be detd. in the presence of Ru.

Full paper in Portable Document Format: 177a517.pdf (in Czech)

 

Chemical Papers 17 (7) 517–523 (1963)

Tuesday, June 18, 2024

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