摘要
本研究优化建立了硫化物浓缩仪-气相色谱联用法测定环境空气中硫化氢、甲硫醇、甲硫醚及二甲基二硫醚的分析方法。采用Rtx-1色谱柱(30 m×0.32 mm×1μm)配合火焰光度检测器(FPD),通过系统优化硫化物浓缩仪参数:设置前/后烘烤时间8 min,冷阱吸附温度^(-2)5℃(解析温度180℃),控制气体进样流量60 mL/min,进样体积100 mL。实验表明,在硫化氢(1.28×10^(-3)~1.28×10^(-2)mg/m^(3))、甲硫醇(1.72×10^(-3)~1.72×10^(-2)mg/m^(3))、甲硫醚(2.20×10^(-3)~2.20×10^(-2)mg/m^(3))和二甲基二硫醚(1.68×10^(-3)~1.68×10^(-2)mg/m^(3))的线性范围内,各组分标准曲线相关系数均>0.995,方法检出限为1.7×10^(-4)~8.8×10^(-4)mg/m^(3),定量下限为6.8×10^(-4)~3.52×10^(-3)mg/m^(3)。通过对环境空气样品低、中和高加标精密度在2.4%~10.8%,加标回收率在92.1%~114%。该方法灵敏度高、重现性好,可满足环境空气中痕量硫化物监测的技术要求。
Hydrogen sulfide,methyl sulfide and dimethyl disulfide in ambient air.were analyzed by Rtx-1 column(30 m×0.32 mm×1μm)with flame photometric detector(FPD)to optimize the parameters of the sulfide concentrator:setting before/post baking time for 8 min,the cold trap adsorption temperature was-25℃(desorption temperature was 180℃),controlling the gas injection flow of 60 mL/min and the injection volume of 100 mL.experimental result demonstrates,In the linear range of hydrogen sulfide(1.28×10^(-3)~1.28×10^(-2)mg/m^(3)),methyl thiol(1.72×10^(-3)~1.72×10^(-2)mg/m^(3)),methyl sulfide(2.20×10^(-3)~2.20×10^(-2)mg/m^(3))and dimethyl disulfide(1.68×10^(-3)~1.68×10^(-2)mg/m^(3)),the correlation coefficient of the standard curves of all components was>0.995,The method limit of detection was 1.7×10^(-4)~8.8×10^(-4)mg/m^(3),lower limit of quantification was(6.8×10^(-4)~3.52×10^(-3)mg/m^(3)).With the precision of low,medium and high calibration of ambient air samples was between 2.4%and 10.8%,the spike recovery was between 92.1%and 114%.The method with high sensitivity and good reproducibility can meet the technical requirements of trace sulfide monitoring in ambient air.
作者
何国忠
王克华
李军
秦海军
HE Guozhong;WANG Kehua;LI Jun;QIN Haijun(Xinjiang Water Qingqing Monitoring Technology Service Co.,Ltd.Xinjiang Urumqi 830000;Jiangsu Kangda Testing Technology Co.,Ltd.,Jiangsu Suzhou 215000;Gansu Intelligent Pharmaceutical Co.,Ltd.,Gansu Lanzhou 730314,China)
出处
《广州化工》
2026年第2期94-97,共4页
GuangZhou Chemical Industry
关键词
烘烤时间
吸附温度
进样流量
解析温度
硫化氢、甲硫醇、甲硫醚和二甲基二硫醚
baking time
adsorption temperature
injection flow
desorption temperature
hydrogen sulfide,methylthiol,methyl sulfide and dimethyl disulfide
