N-ベンゾイル-N-フェニルヒドロキシルアミンとピリジルアゾ色素の配位子交換反応を利用する環境試料中の微量バナジウム(V)の抽出 : 吸光光度定量

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タイトル別名
  • Extraction/spectrophotometric determination of trace amounts of vanadium in environmental materials by the ligand exchange reaction between N-benzoyl-N-phenylhydroxylamine and pyridylazo dye.
  • Ｎ‐ベンゾイル‐Ｎ‐フェニルヒドロキシルアミンとピリジルアゾ色素の配位子交換反応を利用する環境試料中の微量バナジウム（Ｖ）の抽出／吸光光度定量
  • N ベンゾイル N フェニルヒドロキシルアミン ト ピリジルアゾ シキソ ノ

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説明

N-benzoyl-N-phenylhydroxylamine (BPHA) react with V(V) in the range from 3 to 5 mol dm-3 hydrochloric acid to form a selectively extractable complex into chloroform. The chloroform extract of V(V) is shaken with acetic acid and N, N-dimethylformamide (DMF) mixture containing 2-(5-bromo-2-pyridylazo)-5-diethyl-aminophenol (5-Br-PADAP) and potassium periodate. Vanadium (V)-5-Br-PADAP complex formed from the ligand exchange reaction between V(V)-BPHA complex and 5-Br-PADAP has an absorption maximum at 600 nm with molar absorptivity of 5.4 × 104 dm3 mol-1 cm-1 The system obeys Beer's law up to 3.8 μg V(V) (organic phase). Considerable amount (10 mg) of several cations and anions may be tolerated. However, the tolerance limit for W(VI) is 2-folds higher by weight ratio. The presence of large amount of Fe(III) may be separated previously from 6 mol dm-3 hydrochloric acid sample solution by shaking with ether. The selectivity of 5-Br-PADAP reagent was highly improved by introducing a ligand exchange reaction as described above. The recommended procedure is as follows: taking an aliquot of sample solution containing up to 7.6 μg V(V) in a separatory funnel, add 0.3 % potassium permanganate solution dropwise until the pink color appears, 0.5 cm3 of 20% urea solution and 0.5% sodium nitrite adding dropwise until the pink color disappears. Add 2 cm3 of saturated sodium fluoride solution and hydrochloric acid to give the concentration of 4 mol dm3, then dilute to a fixed volume with water. Extract V(V) with 10 cm-3 of 0.02% BPHA in chloroform by shaking for 3 min. Transfer 5 cm3 of orgnic phase into another separatory funnel. Add 4 cm3 of 0.1 % 5-Br-PADAP in DMF solution, 1 cm-3 of 0.4% potassium periodate and 10 cm3 of 0.1 mol dm3 acetic acid solution. Shake for 30 min and allow the organic phase to separate. Measure the absorbance of the organic phase at 600 nm against a reagent blank. The method was successfully applied to the determination of trace amounts of V(V) in environmental materials (Vehicle Exhaust Particulates, Urban Particulate Matter and Sediments).

収録刊行物

  • 分析化学

    分析化学 38 (2), 76-81, 1989

    公益社団法人 日本分析化学会

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