ク形波ポーラログラフによる微量ヒ素の定量

概要

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Several acids as supporting electrolyte have been tested for square-wave polarographic determination of trace amounts of arsenic in highly pure substances. In sulfuric, phosphoric, perchloric and nitric acid solutions, the separation of the first and the second wave of arsenic was incomplete. But in hydrochloric acid solution, two waves have been separated clearly. The shape of the second wave is better than the first, and was scarcely affected by a number of diverse metallic ions. The peak of the first wave appeared at -0.42 V (vs. S. C. E.) in 2M hydrochloric acid solution, and that of the second wave at -0.63 V (vs. S. C. E.). Calibration lines were linear in the range of 2×10-61.6×10-5M of arsenic. The proposed method was applied for the determination of arsenic in white phosphorous as follows: phosphorous was dissolved with nitric acid by warming on a water bath, and heating was continued to expel the excess nitric acid. Two ml of 4M sulfuric acid and 0.2g of hydrazine sulfate was added to it, and was heated to fume. After the cooling, hydrochloric acid was added and polarogram was recorded. Good results were obtained.
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