便携式GC/MS在含硫有机恶臭气体应急监测中的应用  

Application of portable GC/MS for measuring organic malodor with sulfur in case of emergency monitoring

作　　者：周守毅[1] 

机构地区：[1]上海市环境监测中心,上海200030

出　　处：《安全与环境学报》2014年第3期321-323,共3页Journal of Safety and Environment

基　　金：上海市青年科学家环保科研项目(2012-15)

摘　　要：采用便携式GC/MS建立了含硫有机恶臭气体应急监测方法。通过稳定性试验，选用硅烷化苏玛罐作为存贮标准气体的容器。比较Tri-bed和Tenax 2种填料对含硫有机恶臭气体的吸附能力，发现采用Tri-bed填料的捕集管吸附能力好于Tenax。通过优化分析条件，使得4种含硫有机恶臭物质（二甲二硫、乙硫醚、噻吩、二硫化碳）分析时间在5 min内。使用Entech 4600动态气体稀释仪将标准气体分别稀释20倍、40倍、50倍、80倍、100倍后分析并建立标准曲线，发现标准曲线相对标准偏差均小于8.7%。采用便携式GC/MS配置的手持探头采集200 mL样品，对样品中的二甲二硫、乙硫醚、噻吩、二硫化碳进行快速定性、定量分析。结果表明，该方法具有检出限低（9-29 μg/m^3 ）、相对标准偏差小、分析时间短的优点。通过实样分析证明该方法适用于大气中含硫有机恶臭气体的应急监测。The paper intends to present the emergency method for analyzing the organic malodor with sulfuric accident. As is known, sulfur malodor is a byproduct of chemical industry, which is the main cause of many environmental emergencies in the oil refining industry. As is known, the standard gas of organic malodor with sulfur is usually stored in three containers, which can be analyzed in three days. Customarily, the standard gas is stored in a silanized canister, tedler bag or a polished canister. The test results of our research have shown that the standard gas can best be preserved in a silanized canister. A contrast experiment can be made between the Tri-bed and Tenax material. The results indicate that the Tri-bed turned to be better in absorbing the organic malodor with sulfur. After improving analytical condition, a portable GC/MS can be made more convenient to conduct the analysis, because it is possible to finish the testing analysis of the four organic malodors （dimethyl disulfide, diethyl sulfide, carbon disulfide and thiophene） in five minutes. However, it is better to prepare the standard gas of different levels with Entech 4600 dilutor, which can be diluted into 20 times, 40 times, 50 times, 80 times and 100 times, accordingly. A hand-held probe can also be attached to the portable standard GC/MS to gather the 200 mL sample. Besides, a calculation curve can be made by analyzing the standard gas of different levels. The RSD of calculation curve is less than 8.7%. According to current method, the tests of precision were made by analyzing the sample 7 times. The test of accuracy was made by analyzing spiked samples. MLD were calculated by St（n -1, 0.99）. The results prove that the analytical method for dimethyl disulfide, diethyl sulfide, carbon disulfide and thiophene enjoys the advantages in high speed, low detection limits （9-29 μg/m^3 ） and little RSD （RSD〈7.8%）. This method can thus be successfully used for in-situ determination of organic malodor with sulfur in the environmental emer

关 键 词：环境工程学 突发环境事件 应急监测 恶臭 

分 类 号：X830.7[环境科学与工程—环境工程]