<報文>光電分光光度計による比色法の研究(第4報) : Nitroso R Saltによる微量の鐵の定量(2)
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Critical studies were made on the determination of iron with nitroso R salt. The reagent and its complex with ferrous iron were sensitive to changes of hydrogen ion concentration. An aqueous solution of nitroso R salt is yellow having deep absorption below ca. 520 mμ. Above 540 mμ, transmittancy was almost 100%. With 2.5×10^<-4> M/L solution of the reagent, for instance, percent transmittancy at 540 mμ was about 99.6 at pH 6.53. But when pH of the solution was raised above 7.17,another absorption band appeared around 580 mμ and the solution became greenish. Therefore, when the complex was formed at pH above 6.5,attention must be paid to the absorption due to the reagent itself. On adjusting pH of the solution after the reagent had been added to ferrous iron, green color developed immediately. But intensity of the color changed markedly with lapse of time. Absorbancy increased in the wave-length range of 560-660 mμ and above 740 mμ in the period of 94 hours. Between 740 and 660 mμ, it decreased considerably. That is, spectral absorbancy curve became shallower and broader on standing. A long reaction period was necessary to reach the final stable form of the complex. When the solution was warmed for about 5〜10 min on a water bath after pH of the solution had been adjusted, definite transmittancy readings were obtained immediately. The reaction was accelerated by warming. Hydrogen ion concentration allowable for a complete color development depended upon the amount of the reagent present. When the reagent was present ten times as much as iron in molar ratio, full color developed within pH range of 5.31 to 7.24. But with the reagent four times as much as iron, color development was not complete below pH 6.0. The ferrous complex showed maximum transmittancy at 550 mμ. Absorption in the wave-length range below 550 mμ overlapped that of the reagent and was not available for estimation of iron. The absorption band above 550 mμ showed a absorption maximum at 715 mμ.
- 東北大学の論文
- 1953-09-10
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