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本文采用顶空气相色谱法测定大气中微量甲硫醇.标准甲硫醇气体由本实验室合成的甲硫醇铅配制而成.配气时,在密闭的容器中需充N_2,避光,加抗氧化剂可较好地解决甲硫醇不稳定性问题.测定时采用顶空气相色谱法,选用5%OV-101涂在ch-romosorb W AW DMCS 80～100目作为固定相填充在1.2m×4mm i.d.的玻璃柱内;用NaOH为吸收剂.冷阱采样.用磷酸释放甲硫醇.进1ml顶空气体,制作标准曲线.此法相对标准偏差为8%,检测限<1ppb,测大气中微量甲硫醇可得到满意结果.
In this paper, the determination of trace amount of methanethiol in the atmosphere by headspace gas chromatography.The standard methanethiol gas is prepared by the synthesis of methylmercaptide in this laboratory.With the gas, in a closed container to be filled N_2, dark, plus Antioxidants can solve the problem of methylmercaptan instability.Using headspace gas chromatography, 5% OV-101 was applied to ch-romosorb W AW DMC 80 ~ 100 mesh as the stationary phase to fill in 1.2m × 4mm id glass column; NaOH as absorbent cold trap sampling release of methyl mercaptan with phosphoric acid into 1ml headspace gas, making a standard curve. The relative standard deviation of this method is 8%, detection limit <1ppb, measuring the atmosphere Medium trace methanethiol gives satisfactory results.