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作 者:李辰[1] 王国俊[1] 李瑞玉[1] 李菊白[1] 梁冰[1]
机构地区:[1]中国科学院兰州化学物理研究所,甘肃兰州730000
出 处:《色谱》2003年第5期472-475,共4页Chinese Journal of Chromatography
基 金:中国科学院仪器研制项目.
摘 要:介绍了一种含氧有机化合物选择性检测器的原理、装置及其应用。裂解反应器温度在等于或高于1150℃时,可使有机化合物完全裂解,裂解率约为99 5%。其中含氧化合物裂解产生的一氧化碳在甲烷化微型反应器中转化为甲烷后,在气相色谱 火焰离子化检测器(GC FID)上有所响应,其响应值与化合物中的氧含量成正比,而不含氧的碳氢化合物则没有响应,从而使含氧化合物得到选择性检测。甲烷化微型反应器转化率达到95%以上,并可再生使用。在完全裂解状态下,正丁醇的线性范围为0 440~243 000g/L,最小检测量为440ng。对含醇酮混合物的正己烷和无铅汽油混合样进行了FID和含氧化合物选择性检测器(O FID)对比分析。结果表明,在色谱分离不理想的情况下,选择性检测不仅可以给出各含氧化合物的含氧量,同时也可以准确测定混合物中总氧含量。The principle, development and applications of an oxygenatedselective response flame ionization detector (OFID) are described. The organic compounds can be cracked completely at temperatures higher than 1?150 ℃.The oxygenatedcompounds were cracked into carbon monoxide and then converted into methane by the methanizer and detected by a flame ionization detector (FID). The signal produced by this detector was proportional to the oxygen contents of the cracked compounds. The hydrocarbons without oxygen did not have the signal on it, so oxygenatedcompounds were selectively detected. The sample of hexane and unleaded gasoline spiked with a mixture of alcohols and ketones were analysed comparatively by FID and OFID systems. The conversion of the methanizer was higher than 95%. The linear range for nbutyl alcohol was 0440-243000 g/L in the state of complete cracking. The minimum amount of detection for nbutyl alcohol was 440 ng. The analytical results indicated that the OFID system could detect the oxygenatedcompounds selectively among a mixture of different compounds. The method proved to be convenient to determine the oxygenatedcompounds qualitatively and quantitatively. The rule of the value of the relative O response was good, and the total contents of oxygen in the sample can be obtained without complete separation of the compounds.
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