海洋污染事故中裂解碳九主要成分的监测分析方法

    Analysis methods for detecting cracking C9 in sudden marine pollution accidents

    • 摘要: 研究建立了基于顶空气相色谱-质谱联用(HS-GC/MS)的裂解碳九主要成分分析方法,该方法可同时测定水体中α-甲基苯乙烯、间-甲基苯乙烯、对-甲基苯乙烯、邻-甲基苯乙烯、β-甲基苯乙烯、双环戊二烯、茚、1-甲基萘和2-甲基萘等9种裂解碳九主要成分的残留量。取10.0 mL海水样品在密封的顶空瓶中,在振荡器中于90℃下振荡10 min,使气-液两相达到动态平衡。采用DB-5MS毛细管色谱柱(30 m×0.25 mm×0.25 μm)对9种目标化合物进行分离,内标法定量。本方法在0.50~10 μg·L-1范围内线性关系良好,相关系数均大于0.998;在海水中9种化合物的检出限为0.500~1.00 μg·L-1,添加浓度为1.00~10.0 μg·L-1时,各目标化合物的平均加标回收率在82.4%~106.6%之间,相对标准偏差(n=6)在3.73%~9.41%之间。本方法操作简单、快速,灵敏度和准确度高,适用于海水中裂解碳九主要成分残留量的同时检测,为海洋污染事故应急处置分析中裂解碳九主要组成的测定提供参考依据。

       

      Abstract: In this study,a headspace gas chromatography-mass spectrometry(HS-GC /MS)method for simultaneous determination of cracking C9(including α-methylstyrene,o-methylstyrene,m-methylstyrene,p-methylstyrene,β-methylstyrene,dicyclopentadiene,ninhydrin,α-methylnaphthalene and β-methylnaphthalene)in water sample was established.Briefly,10 mL seawater was sealed in the headspace bottle and vibrated under 90 ℃ for 10 min to obtain gas-liquid dynamic equilibrium.Nine target compounds were separated by DB-5MS capillary column(30 m×0.25 mm×0.25 m),and quantified by internal standard method.The method had good linear relation in the range of 0.50~10 μg·L-1,with a correlation coefficient greater than 0.998.The detection limit of the compounds in seawater was 0.500~1.00 μg·L-1.When the concentration was 1.00~10.0 μg·L-1,the average standard recovery of each compound was 82.4%~106.6% and the relative standard deviation was 3.73%~9.41%.This simple,rapid,sensitive and accurate method was suitable for the simultaneous detection of various kinds of cracking C9 in seawater,which provided a reference for the determination of cracking C9 in the emergency monitoring of marine pollution accidents.

       

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