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›› 2020, Vol. 42 ›› Issue (2): 138-145.

• 论文与报告 • 上一篇    下一篇

海洋污染事故中裂解碳九主要成分的监测分析方法

肖洁1,张珰妮2,张天闻2   

  1. 1. 福建省海洋环境与渔业资源监测中心
    2. 福建省渔业资源监测中心
  • 收稿日期:2019-08-22 修回日期:2019-11-13 出版日期:2020-04-24 发布日期:2020-04-28
  • 通讯作者: 张天闻
  • 基金资助:
    2016年省海洋与渔业结构调整专项资金

Analysis methods for detecting cracking C9 in sudden marine pollution accidents

  • Received:2019-08-22 Revised:2019-11-13 Online:2020-04-24 Published:2020-04-28

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、双环戌二烯、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×0.2 5 mm×0. 25 m ) 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。

关键词: 顶空气相色谱-质谱法, 裂解碳九主要成分, 海水, HS-GC/MS, cracking C9, seawater

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 0.5 μg?L-1~10.0 μg?L-1, with a correlation coefficient greater than 0.998. The detection limit of the compounds in seawater is 0.50~1.00 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 provides a reference for the determination of cracking C9 in the emergency monitoring of marine pollution accidents.

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