甲醇等5种强极性有机物污染事故中的监测分析方法

Analysis Methods for Detecting Strong Polar Organics in Sudden Water Pollution Accidents such as Methonal

建立了在突发性水污染事故中定量分析水样中甲醇、丙酮、乙腈、N,N-二甲基甲酰胺和N,N-二甲基乙酰胺等5种极性有机物的实验室和现场应急监测分析方法。采用顶空-车载气相色谱质谱法用于现场快速定性定量分析;顶空-气相色谱法用于实验室准确定量分析。通过优化顶空及气相参数,在最佳实验条件下测得顶空-气相色谱质谱法中甲醇、丙酮、乙腈、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺等5种化合物的检出限分别为1.0、0.06、0.5、10.0、15.0 mg/L,平行测定7次结果的相对标准偏差分别为2.1%~3.8%,加标回收率为69.4%~104%;顶空-气相色谱法灵敏度高于气相色谱质谱法,检出限分别为0.08、0.01、0.03、1.7、1.7 mg/L,平行测定7次结果的相对标准偏差分别为2.5%~4.1%,加标回收率为78.1%~116%。

A simple method was developed to rapidly quantitative and qualitative analyse methonal,acetone,acetonitrile,N,Ndimethyl formamide and N,N-dimethyl-Acetamide in sudden water pollution accidents. A headspace-vehicular GC-MS method was adopted to rapidly detect five strong polar volatile organic compounds at water pollution accidents site; a headspace-GC-ECD method was used in laboratory analysis. Under optimum conditions,the detect limitation of GC-MSD method of methonal,acetone,acetonitrile,N,N-dimethyl formamide and N,N-dimethyl-Acetamide were 1. 0,0. 06,0. 5,10. 0 and 15. 0 mg/L respectively,and the relative standard deviation were between 2. 1%-3. 8%（ n = 7） reapectively; the spiked recovery of these five compounds were between 69. 4%-104%; the detect limitation of GC-ECD method of methonal,aceton,acetonitrile,N,Ndimethyl formamide and N,N-dimethyl-Acetamide were 0. 08,0. 01,0. 03,1. 7 and 1. 7 mg/L respectively,and the relative standard deviation were between 2. 5%-4. 1%（ n = 7） reapectively; the spiked recovery of these five compounds were between78. 1%-116%.