毛细管气相色谱法测定含硫恶臭气体混合物  

Analysis of sulfur-containing odorous gas mixture by capillary gas chromatography

作　　者：赵栩澜 杜晓松[1] 高超[1] 龙吟[1] 崔进[1] 吴朋林 

机构地区：[1]电子科技大学光电信息学院,电子薄膜与集成器件国家重点实验室,成都610054

出　　处：《分析试验室》2015年第11期1263-1267,共5页Chinese Journal of Analysis Laboratory

基　　金：国家高新科技研究发展计划(2014AA063010);国家自然科学基金(61235006,61421002)项目资助

摘　　要：采用Rt-silica Bond Plot毛细管色谱柱(硅胶键合极性基团固定相)的GC-FPD色谱系统,检测了环境中的含硫恶臭气体甲硫醇、甲硫醚、乙硫醇、二硫化碳和二甲二硫的混合气体。实验研究了气相色谱柱进样口压力和升温方式对分离效果的影响,在最佳分离条件下对5种气体的混合样进行了重复性测试,并利用自制的Tenax管式富集器分析5种气体的检出限。方法的最佳进样口压力为48.26 k Pa和最佳升温方式为初始温度160℃,以30℃/min升至220℃,可以实现混合气体的完全分离,分离时间3.850 min,组分间最小分离度2.525,最佳条件下具有很好的重复性,保留时间和组分分离度的相对标准偏差均小于1%,峰面积相对标准偏差最大为5.0%,5种气体的检出限依次为45,37,21,30和22μg/m3。In this paper,a mixture sample of sulfur- containing odorous gas components like methyl mercaptan（ MM）,dimethylsulfide（ DMS）,ethanethiol,carbon disulfide（ CS2） and dimethyldisulfide（ DMDS） were analyzed and detected by an Rt-silica Bond Plot capillary column（ silica gel bonded polar group stationary phase） gas chromatography- flame photometric detector（ GC- FPD） system. The effects of GC parameters（ column injecting pressure and temperature ascending modes） on separating effects were studied. The repeatability for the five components under optimized conditions was tested. The limits of detection（ LODs） of these five gases using self- made Tenax tubular concentrator were obtained. The results indicated that the optimum injection column pressure was 48. 26 k Pa and optimum temperature ascending mode was setting from160 ℃ to 220 ℃ increasing by 30 ℃ per minute,which could realize the separation of these five gases completely. The separation time is 3. 850 min and value of the minimum resolution is up to 2. 525. It has good repeatability under optimized conditions with the relative standard deviation（ RSD） of retention times and component resolutions less than 1%,and the max RSD of the peak area is 5. 007%. LODs for MM,DMS,ethanethiol,CS2 and DMDS under optimized conditions were 4. 5 × 10^- 2mg/m^3,3. 7 × 10^- 2mg/m^3,2. 1 ×10^- 2mg/m3,5. 7 × 10^- 2mg/m^3 and 2. 2 × 10^- 2mg/m^3 respectively. This method has advantages of rapidness,sensitivity and good repeatability.

关 键 词：恶臭气体 气相色谱 分离度 Tenax管式富集器 最低检测量 

分 类 号：X131.1[环境科学与工程—环境科学]