Spectrophotometric Determination of Phosphorus in Iron and Steel by Extaction of Phosphovanadomolybdate with Methyl-iso-buthyl Ketone

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  • リンバナドモリブデン酸-メチルイソブチルケトン抽出による鉄鋼中リンの吸光光度定量
  • リンバナド モリブデンサン-メチルイソブチルケトン チュウシュツ ニ ヨル テッコウ チュウ リン ノ キュウコウ コウド テイリョウ

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The elimination of factors affecting the phosphovanadomolybdate method for photometric determination of phosphorus in iron and steels were studied, and the optimum conditions for them were determined. The following new analytical procedure is proposed. Dissolve 0.2∼0.5 g of sample with 7 mL of HNO3 (1:1) and 16 mL of HClO4 (70%) and evaporate HClO4 in fume for 5 min. Add 40 mL of distilled water and KMnO4 solution (1%) dropwise, if it necessary, then and NaNO2 solution (5%) dropwise and boil until precipitate is dissolved and Cr (VI) is reduced if it present. After the solution is cooled until room temperature, add 10 mL of ammonium vanadate solution (0.24%) and 15 mL of ammonium molybdate solution (15%), and allow to stand for 7 minutes. Then add 10 mL of citric acid (500 g/L) and extract the complex with 10 mL of it methyl-iso-buthyl Ketone twice immediately. Dry the extract with Na2SO4 anhydrous and make up to 25 mL, and measure its absorbance at 400 mμ or 490 mμ.

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