水銀陰極電解分離法を用いる金属シルコニウムおよび金属チタン中の極微量コバルトの比色定量

概要

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An electrolytic separation has been applied to the photometric determination of microgram quantities of cobalt in zirconium and titanium metal. A sulfuric acid solution containing 1g of the metals is electrolyzed with 2 ml of mercury as the cathode and a platinum spiral as the anode. The conditions of electrolysis are as follows: current strength, 2.0 amp; current density, 0.5 amp/cm2; electrolyte volume, 100 ml; acidity, 1.0 N; time of electrolysis 3hr. After electrolysis the mercury is drained out, distilled in a stream of nitrogen at 350°C, and the cobalt in the residue is determined by the photometric nitroso-R salt method. Tracer experiments using cobalt-60 indicate an exponential decrease in cobalt concentration of the electrolyte during the electrolysis, and an almost perfect recovery of cobalt under the prescribed conditions. One tenth to 5 ppm of cobalt can be determined with an accuracy of 0.1 ppm.