顶空-气相色谱质谱法检测污泥中挥发性有机硫化物方法探讨

Study on the Detection of Volatile Organic Sulfides in Sludge by Headspace-Gas Chromatography Mass Spectrometry

建立了顶空-气相色谱质谱联用法分析污泥中挥发性有机硫化物的方法。针对污泥中四种挥发性有机硫化物(甲硫醇、乙硫醇、二甲基硫、二硫化碳),研究了顶空平衡时间,加热温度,色谱柱对分析结果的影响。载气为高纯氦气,流速为1.0 mL/min,色谱柱为DB-5MS色谱柱(30 m×0.32 mm×0.25 um),柱温:40℃(5 min)→5℃/min→90℃(2 min)→8℃/min→200℃(5 min);在实验条件下,本方法测定甲硫醇、乙硫醇、二甲基硫、二硫化碳的线性范围为10~5000 ng/Kg;回收率分别为91.6%~101.3%,91.8%~98.4%,83.2%~97.5%,90.6%~103.4%,相对标准偏差均小于10%,满足实际分析需求。

A method was developed for the analysis of volatile organic sulfides in sludge by headspace-gas chromatography-mass spectrometry.Aiming at the four volatile organic sulfides(methyl mercaptan,ethyl mercaptan,dimethyl sulfur,and carbon disulfide)in the sludge,the effects of headspace equilibrium time,heating temperature,and column on the analysis results were studied.The carrier gas is high-purity helium,the flow rate is 1.0 mL/min,and the column is a DB-5MS column(30 m×0.32 mm×0.25 um).2 min)→8℃/min→200℃(5 min);Under the experimental conditions,the linear range of this method for the determination of methyl mercaptan,ethyl mercaptan,dimethylsulfide,and carbon disulfide is 10~5000 ng/Kg;the recovery rates are respectively It is 91.6%~101.3%,91.8%~98.4%,83.2%~97.5%,90.6%~103.4%,and the relative standard deviations are all less than 10%,which meets the actual analysis needs.