発光分光型検出器を用いる極微量ベリリウムのガスクロマトグラフィー

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タイトル別名
  • Gas chromatography of traces of beryllium using the microwave plasma detector
  • ハッコウ ブンコウガタ ケンシュツキ オ モチイル キョク ビリョウ ベリリウ

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A sensitive and rapid method has been developed for the determination of picogram quantities of beryllium. Beryllium was converted to its trifluoroacetylacetone (TFA) chelate and separated on a glass column (90cm×3mm i.d.) packed with 0.5% SE-30 on glass beads {(6080) mesh} at 130°C, with argon containing 0.05% TFA vapor as carrier gas. Spectra were excited in the plasma of a low-wattage 2450 MHz electrodeless discharge at atmospheric pressure, and the Be I 234.9 nm line was monitored. To eliminate the high background emission due to argon and chloroform used as solvent, a quartz plate vibrating at 108.8 Hz was mounted behind the entrance slit of a monochromator, and a lock-in amplifier was tuned to twice the frequency of the vibration. The chromatographic peak height was proportional to the beryllium quantity over the range (0.0021) ng, with an error of 5% at 0.1 ng. The lower limit of detection was 0.001 ng of beryllium (0.03 ng with a mechanical disk chopper and a lock-in amplifier, and 0.1 ng with a DC amplifier). The proposed method was applied to the determination of beryllium at the low ppm level in samples of aluminum metal and aluminum-magnesium alloy. A sample {(2040) mg} was dissolved in hydrochloric acid and beryllium was extracted with 2 ml of 0.1 M TFA in chloroform at pH 6.5 in the presence of EDTA to mask aluminum. A 1 μl aliquot of the organic phase was then injected into the gas chromatograph. A determination required (11.5) hrs.

収録刊行物

  • 分析化学

    分析化学 25 (2), 85-89, 1976

    公益社団法人 日本分析化学会

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