ガスクロマトグラフ法を用いる有機ハロゲンの自動分析計の開発

概要

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The determination of organic halogens is mostly carried out by the oxygen-flask method, while very few attempts have been reported for automatic instrumentation of the halogen analyzer. A rapid and simple microanalyzer is therefore proposed using the gas-chromatographic technique by which chlorine, bromine and iodine are qualified and quantified, respectively. A sample of 1〜1.5 mg is weighed and ignited instantaneously in a quartz combustion tube at 900℃ with a carrier gas comprizing helium and oxygen (1:1) at a flow rate of 20 ml/min. The combustion gas passes through a Teflon column at 60℃ packed with methylsilicone oil as a stationary phase. Halogens coming out of the column are then chemically converted to equimolar iodine by contact with silver iodide at 200℃. The iodine vapor is spectrophotometrically detected in a small gas cell incorporated with a light source of 525 nm and a phototransistor. The retention times of the halogen peaks are 4 min for chlorine, 8 min for bromine and 35 min for iodine, respectively. By raising the column temperature to 80℃, however, iodine comes out at 15 min. Since the detector output is proportional to the light transmittance, a computer program was made to transform the signal every one second to the absorbance scale. The integrator prints out the peak data to 5 figures.
社団法人日本分析化学会の論文
1998-11-05