交流ポーラログラフによる鋼および特殊鋼中の銅，スズ同時定量法

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  • Simultaneous Determination of Copper and Tin in Carbon and Alloy Steels by means of A.C. Polarography. (Studies on the Rapid Analysis of Iron and Steel by means of A.C. Polarography (1))
  • コウリュウ ポーラログラフ ニ ヨル コウ オヨビ トクシュコウ チュウ ノ ドウ , スズ ドウジ テイリョウホウ

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The routine method for the rapid A.C. polarographic determination of Cu and Sn in carbon and alloy steels was studied and the following procedure was established: A 0.5 g sample was dissolved in 10 mL of 6 N-HCl by gentle heating, and cooled and washed with 4.5 N-HCl into a 50 mL volumetric flask, which was then filled up to the mark with 4.5 N-HCl. Transfer 5 mL of the solution into a polarographic cell, add 2 drops of 1% gelatine solution and expel the dissolved oxygen by passing hydrogen through the solution for 2∼3 minutes. Record the polarogram (a Yanagimoto pen-recording polarograph was used) between −0.1 and −0.7 V, measure the wavesheight of Cu (−0.25 V vs.S.C.E.)and Sn (−0.48 V vs.S.C.E.) and determine the contents by the calibration curves. Bi, Sb, Pb, and Cd also give their waves in 4.5 N-HCl at −0.10, −0.19, −0.44 and −0.66 V. vs. S.C.E., respectively. Of these four elements, Pb over about 0.02% interferes, but the others are usually contained in carbon and alloy steels so small in quantity that they do not interfere. When chromium is contained in the alloy steels over about 5%, it is necessary to add 5 mL, of pure pyridin to the volumetric flask, and fill it with 4.5 N-HCl up to the mark. For example, Cu and Sn in carbon steel, high speed steel and stainless steel were determined with absolute error of ±0.005% against the values obtained by the iodometric method and the time required for the determination of the two elements was only 14 to 18 minutes. The influence of temperatures of the electrolytic solution upon wave-height was not appreciable in the region from 5 to 35°.

収録刊行物

  • 日本金属学会誌

    日本金属学会誌 23 (2), 100-104, 1959

    公益社団法人 日本金属学会

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