引用本文:李媛,王荟,胡冠九,李晨.大体积直接进样气相色谱法测定环境空气与无组织排放中硫化氢等16种含硫化合物[J].环境监控与预警,2023,15(1):44-51
LI Yuan, WANG Hui, HU Guan-jiu, LI Chen.Determination of 16 Sulfur Compounds in Ambient Air and Fugitive Emission Samples by Gas Chromatography through Large Volume Direct Injection[J].Environmental Monitoring and Forewarning,2023,15(1):44-51
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大体积直接进样气相色谱法测定环境空气与无组织排放中硫化氢等16种含硫化合物
李媛,王荟,胡冠九,李晨1,2,3
1.国家环境保护地表水环境有机污染物监测分析重点实验室,江苏 南京 210019;2.江苏省环境监测中心,江苏 南京 210019;3.江苏省苏力环境科技有限责任公司,江苏 南京 210019
摘要:
采用冷冻聚焦-硫发光检测器气相色谱仪测定环境空气与无组织排放中硫化氢等16种含硫化合物。结合大体积(5 mL)进样,对最优仪器条件进行研究。结果表明:在最佳条件下,16种含硫化合物的相关系数均>0.997,方法检出限为0.14~0.59 μg/m3 ,相对标准偏差为0.7%~4.6%。且硫化氢、羰基硫、甲硫醇、甲硫醚、二甲基二硫醚、二硫化碳、噻吩、四氢噻吩这8种化合物的检出限均小于嗅阈值,解决了能够闻到含硫化合物的臭味,却检测不出的难题。该方法极大地提高了检测精度,适用于环境空气与无组织排放中痕量含硫化合物的测定。
关键词:  含硫化合物  冷冻聚焦  直接进样  硫化学发光检测器  嗅阈值
DOI:
分类号:X831
基金项目:江苏省环境监测科研基金项目(1911,2222)
Determination of 16 Sulfur Compounds in Ambient Air and Fugitive Emission Samples by Gas Chromatography through Large Volume Direct Injection
LI Yuan, WANG Hui, HU Guan-jiu, LI Chen1,2,3
1.State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface Water, Nanjing, Jiangsu 210019, China;2.Jiangsu Provincial Environmental Monitoring Center, Nanjing, Jiangsu 210019, China;3.Jiangsu Suli Environmental Technology Co., Ltd., Nanjing, Jiangsu 210019, China
Abstract:
16 sulfur compounds in ambient air and fugitive emission samples were determined by cryo focusing gas chromatography with sulfur chemiluminescence detector (SCD) through direct injection in this study. By the optimization of instrument conditions coupled with large volume injection of 5 mL, the detection accuracy was greatly improved. Results showed that under the optimal conditions, the correlation coefficients of the linear regression equations of the 16 organic sulfides were all above 0.997, the method detection limits (MDL) were 0.14~0.59 μg/m3, and the relative standard deviations were 0.7%~4.6%. The MDL of hydrogen sulfide, carbonyl sulfur, methanethiol, methyl sulfide, dimethyl disulfide, carbon disulfide, thiophene, and tetrahydrothiophene were all lower than the olfactory thresholds. Our finding solves the technical issue that these sulfur compounds can be smelled but could not be detected, which is suitable for the determination of trace sulfur compounds in ambient air and fugitive emission samples.
Key words:  Sulfur compounds  Cryo focusing  Direct injection  Sulfur chemiluminescence detector  Olfactory threshold