For the determination of bromide in the presence of chloride, bromide is usually oxidized to bromate by the addition of sodium hypochlorite or calcium hypochlorite.
In this report, an electrolytic oxidation of bromide to bromate in the solution containing chloride was devised.
As the experiments, Kolthoff-Yutzy method in determination of bromide in the presence of chloride, preparations of hypochlorous acid, hypochlorite and chlorate by the direct electrolysis of sodium chloride solution and electrolytic conditions in the formation of bromate from chloride-bro-mide solution were studied.
By Kolthoff-Yutzy method using sodium hypochlorite as an oxidant, results of high degree of accuracy, repeatability and reproducibility in the determination of bromide were obtained. However, in the presence of magnesium or calcium, removal of them before determination was considered preferable.
The determination of bromide and bromate each in the mixture by this method was found to be able.
In the preparation of hypochlorous acid and hypochlorite, by the variable current densities, recognizable effect were not observed. But in the presence of the more amount of sodium chloride and the less amount of sodium hydroxide, the higher maximum value of the concentration of hypochlorous acid and hypochlorite in the solution was obtained and the larger rate of formation were observed.
And the higher amounts of sodium chloride and sodium hydroxide present, the less became the formation of chlorate.
For the quantitative electrolytic oxidation of bromide to bromate, presence of chloride was seemed indispensable. From this fact, the author considered that bromide was directly oxidized on the anode, and also it was oxidized by hypochlorous acid and hypochlorite which were produced in thesolution by the discharge of chlorine ion.
When 50 ml. of a sample solution having a concentration as much as 0.002M bromide was used, it was possible to form bromate quantitatively by passing a quantity of electric current of 0.5 ampere hour through the solution at 10°C in the presence of sodium chloride and sodium dihydrogen phosphate.
In this method, the recovery rate of bromide to bromate was very high, and the repeatability and the reproducibility of bromate-formation were good. So, it is considered that this electrolytic method is applicable to determination of bromide in the presence of chloride.
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