メチルイソブチルケトンを用いる溶媒抽出ポーラログラフィー

概要

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Only few examples of direct polarographic determination of extracted materials in organic solvents are known as yet, because of the difficulty to find a soluble supporting electrolyte in such a solution. Methylisobutylketone (MIBK) containing small amounts of tetraethylammonium hydroxide was distilled using a column packed with helipack and then the distillate at 116°C was further purified by redistillation. The accessible potential range of this distillate in the presence of 0.1 M tetrabutylammonium perchlorate (TBAP) was about +0.7-2.6 volt (vs. SCE). To determine Cu(II), add 5 ml of 30% ammonium citrate, 5 ml of 10% triethanolamine, 15 g of ammonium sulfate and 50 mg of tetraethylammoniumpyrrolidinedithiocarbamate. Adjust the pH to 9.5 with concentrated ammonium hydroxide and dilute to 50 ml with distilled water. Extract the solution with 25 ml of MIBK. Stay for 5 minutes and then add TBAP as the supporting electrolyte. Purge oxygen from the solution with highly purified nitrogen. From the first reduction wave height of Cu(II)pyrrolidinedithiocarbamate, Cu(II) in the range of 5 × 10-58× 10-4 M can be determined successfully. This method can be applied to the determination in ion pair complex system.
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