化学発光による過酸化水素の定量

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The reaction between hydrogen peroxide and luminol (5-amino-2, 3-dihydrophthalazine-1, 4-dione) in alkaline aqueous medium was catalyzed by tetram-minediaquacobalt(III) ions {See. H. Ojima, Nippon Kagaku Zasshi, 79, 188 (1958)}. The chemiluminescence reaction in luminol-cobalt(III)-hydrogen pero-xide system was used for the determination of micro amounts of hydrogen peroxide, and the method was applied to the determination of H2O2 formed in irradiated water. This system may be used as a dosimeter in the range of 104107 roentgen with 60Co γ-rays. The reaction mixture (8.57 × 10-5M luminol, 0.57 M Na2CO3, _??_8.57 × 10-5 M H2O2, 1.71 × 10-4 M[Co-(H2O)2(NH3)4]3+) exhibits strong luminescence with an emission maximum at 430 nm. Luminescence measurements were carried out with a Hitachi spectrophotometer Model 139 equipped with a chemiluminescence compartment constructed by the authors(Fig. 1). Several conditions for the luminescence development were investigated, and the following procedure has been established. Ten milliliters of 2 M Na2CO3 solution, 3 ml of 10-3 M luminol solution(in 0.1M NaOH solution) and 16 ml of water were added to 3 ml of sample solution (containing 2.8 × 10-643.6 × 10-5 M of H2O2) with continuous stirring. The mixture was kept at 25°C. Ninety seconds after the addition of luminol, 3 ml of 2 × 10-3 M of [Co(H2O)2(NH3)4]3+ solution. was added to the solution, and the luminescence intensity was immediately recorded. The peak height registered by the recorder (Hitachi QPD recorder) gave a reproducible luminescence intensity, which was proportional to hydrogen peroxide concentration. The calibration curve was linear for 2.86 ×10-68.57 × 10-5 mol of H2O2 in the final volume of 35 ml, and in this procedure hydrogen peroxide can be determined within 10% error. The concentrations of hydrogen peroxide were measured in redistilled water and in 1 M sodium carbonate sample solution which had been irradiated with 60Co γ-radiation to a dose of 5 × 104 roentgens to 1 × 107 roentgens. A plot of luminescence intensity against the dose gave a straight line, and G(H2O2) value was determined from the slope of the line. The value of G(H2O2) was obtained as 1.2±0.1 per 100 eV for 60Coγ-radiation.
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化学発光による過酸化水素の定量

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