Gas-chromatographic and thermogravimetric analyses of metal chelates of 2-picolylalkylketones

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Other Title
  • 金属キレートのガスクロマトグラフィー　Ｖ　　２‐ピコリルアルキルケトン金属キレートの熱重量分析およびガスクロマトグラフィー
  • 2 ピコリルアルキルケトン キンゾク キレート ノ ネツ ジュウリョウ ブンセ
  • 2-ピコリルアルキルケトン金属キレートの熱重量分析及びガスクロマトグラフィー
  • 金属キレートのガスクロマトグラフィーに関する研究(第5報)

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Abstract

Some new ligands, 2-picolylalkylketones, which can coordinate to metals through oxygen and nitrogen atoms and their metal chelates were synthesized. Thermal stabilities, volatilities, gas-chromatographic behaviors of these metal chelates and then analytical applications by gas-chromatography were investigated. 2-Picolyllithium prepared from 2-picoline and phenyllithium was acylated with ethyl esters of acetic acid, isobutyric acid, pivaric acid, and trifluoroacetic acid, and their reaction products were 2-picolylmethylketone (PMK)H, 2-picolyl-iso-propylketone (PIPK)H, 2-picolyl-t-butylketone (PTBK)H, and 2-picolyltrifluoromethylketone (PTFMK)H, respectively. Beryllium, copper, zinc, nickel and chromium chelates of (PTFMK)H and beryllium and copper chelates of (PMK)H, (PIPK)H and (PTBK)H were formed by a conventional method. The result of thermogravimetric analysis(TGA) indicated that beryllium, copper, zinc, and nickel chelates of (PTFMK)H were thermally stable enough to apply to gas-chromatography, but the chromium chelate was so unstable that it decomposed prior to vaporization. IR spectrum of the metal chelate in the vapor state was compared with that in the solid state. IR spectrum of the vaporized stable metal chelate was the same as that of the solid chelate, while IR spectrum of the vaporized unstable metal chelate was the same as that of the vaporized free ligand. Typical gas chromatograms were obtained by stable metal chelates of (PTFMK)H and a linear relationship was held between the injected amount of the chelate and the peak area over a considerable range of sample amount, and the gas-chromatographic method was applicable to the determination of these metal ions.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 26 (1), 19-24, 1977

    The Japan Society for Analytical Chemistry

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