4,4'-ビス(ジメチルアミノ)チオベンゾフェノンを用いる銀及び銅地金,粗銅,及びアノードスライム中の微量パラジウムの抽出-吸光光度定量

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タイトル別名
  • ４，４′‐ビス（ジメチルアミノ）チオベンゾフェノンを用いる銀及び銅地金，粗銅，及びアノードスライム中の微量パラジウムの抽出‐吸光光度定量
  • Extraction-spectrophotometric determination of traces of palladium in silver and copper metals, crude copper and anode slime with 4, 4'-bis (dirnethylamino) thiobenzophenone
  • 4 4 ビス ジメチルアミノ チオベンゾフェノン オ モチイル ギン オヨビ

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抄録

A highly sensitive spectrophotometric method for the determination of traces of palladium in silver and copper metals, crude copper and anode slime has been developed. Palladium is extracted as its bromo complex with tri-n-octylamine (TOA) and determined photometrically with 4, 4'-bis (dimethylamino) thiobenzophenone (Thio-Michler's ketone, TMK). Conditions for the extraction and determination of palladium are investigated, and the following procedure has been established. Transfer a solution containing up to 3μg palladium to a separatory funnel. Add 5 ml of 0.5 N hydrobromic acid and 5 ml of 10 N sulfuric acid, and make up to 50 ml with water. Shake for 5 min with 5 ml of 15% (v/v) TOA solution in toluene. Wash the organic phase for 2 min with 20 ml of a wash solution (0.1 N HBr-0.5 N HClO4). Discard the aqueous phase. To the organic phase, add 3.0 ml of 0.01% (w/v) TMK solution in 1-butanol, and shake for 2 min with 50 ml of a buffer solution (1 N sodium acetate solution, pH 2.8). Measure the absorbance of the organic phase at 520 nm against the TOA solution. The absorption maximum was at 520 nm and the apparent molar absorptivity was 1.3 × 105 l mol -1 cm-1. Beer's law was obeyed over the range 03μg of palladium. The color was stable for 30 min. Copper (II) up to 0.1 g, Bi3+ up to 1 mg and Ag+ up to 0.1 mg did not interfere ; larger amounts than stated caused either positive or negative error. 0.1 mg each of Rh3+ and Ru3+ caused a negative error. Ten micrograms of Au3+, 50μg of Pt4+, 1 mg of Hg2+, and 10 mg of Tl3+ gave absorbances equivalent to 3.6, 2.2, 0.9 and 1.5 μg of palladium, respectively. The effect of Au3+ could be eliminated by the extraction of gold with ethyl acetate from 1.2 N hydrochloric acid solution. Silver could be separated as silver chloride precipitate. Preliminary extraction of palladium as dimethylglyoxime complex with chloroform from (0.11.5)N hydrochloric or (0.11)N nitric acid solution served to get rid of interferences other than gold and silver. Other 28 elements investigated at (110) mg levels did not interfere. On the basis of these observation, the method for the determination of palladium in the above materials has been established. According to the proposed method, palladium was recovered quantitatively and as little as 0.1μg of palladium in a sample or in an aliquot of the sample solution could be determined.

収録刊行物

  • 分析化学

    分析化学 28 (4), 253-258, 1979

    公益社団法人 日本分析化学会

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