Flameless atomic absorption spectrometry with glassy carbon strip atomizer

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  • YANAGISAWA Masaaki
    Department of Synthetic Chemistry, Faculty of Engineering, Nagoya University
  • TAKEUCHI Tsugio
    Department of Synthetic Chemistry, Faculty of Engineering, Nagoya University

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  • フレームを用いない原子吸光分析
  • フレーム オ モチイナイ ゲンシキュウコウブンセキ

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The usefulness of glassy carbon as a refractory material for atomization device in flameless atomic absorption spectrometry was described.<BR>The glassy carbon strip(0.7 mm in thickness, 45 mm in length and 2.5 mm in width) clamped to the upper ends of the two stainless-steel electrodes was electrically heated by connecting to the leads from a step-down transformer (Fig. 1). It was covered with a demountable Pyrex glass chamber (inner volume, ca. 350 ml). The chamber was purged by a stream of argon or argon-hydrogen gas before atomization.<BR>In order to get high sensitivity and the information about the atom population in narrow space above the glassy carbon strip, the incident light beam from the radiation source was narrowed by passing through a stainless-steel slit(1.0 mm × 1.0 mm). The effects of the chemical composition of samples and additives were studied.<BR>The observed atomic absorption of lead(nitrate) and copper(chloride, nitrate and sulfate) between 5.0 and 6.5 mm above the strip was only about 30% of that observed just above the strip.<BR>The effect of anions on the atomic absorption of copper was investigated at various temperatures using copper chloride, nitrate and sulfate. Copper chloride showed a lower copper absorption when compared with the nitrate and sulfate. This fact, which was not observed in atomic absorption with flame, suggests that the volatility of the compounds might be associated with the efficiency of atomization by the glassy carbon atomizer.<BR>The effect of coexisting salts on the copper absorption was studied using aluminum chloride and sodium chloride. The depression effect on the copper absorption was observed at low temperatures for sodium chloride, but no noticeable effect was observed at higher temperatures. Aluminum chloride had little effect on copper absorption of the chloride, nitrate and sulfate.The difference between sodium chloride and aluminum chloride might result from the different thermal stability of these two salts. As for aluminum chloride, the copper salts could be converted to chloride easily before vaporization by reacting with aluminum chloride.<BR>Strontium was also tested to obtain further information on glassy carbon strip. The absorption became less and lasted for a longer time, and the recorded curve became broader, the fact suggesting that glassy carbon had very little reducing power against strontium. In fact, the addition of hydrogen sharpened the curve. The use of hydrogen would be promising for flameless atomic absorption with glassy carbon mainly because of its reducing ability.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 23 (4), 364-368, 1974

    The Japan Society for Analytical Chemistry

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