石油炼制与化工 ›› 2018, Vol. 49 ›› Issue (9): 96-100.

• 分析与评定 • 上一篇    下一篇

固相萃取-气相色谱法测定催化裂化柴油中的酚类化合物

史得军,陈菲,王春燕,王飞   

  1. 中国石油石油化工研究院

  • 收稿日期:2018-04-17 修回日期:2018-05-24 出版日期:2018-09-12 发布日期:2018-09-28
  • 通讯作者: 史得军 E-mail:shidejun163@163.com
  • 基金资助:
     

DETERMINATION OF PHENOLIC COMPOUNDS IN FCC DIESEL OIL BY SOLID PHASE EXTRACTION-GAS CHROMATOGRAPHY

  1.  
  • Received:2018-04-17 Revised:2018-05-24 Online:2018-09-12 Published:2018-09-28
  • Supported by:
     

摘要: 采用固相萃取法将催化裂化柴油中的酚类化合物与烃类化合物进行分离。优化了固相萃取的洗脱条件,考察了方法的回收率与重复性。采用气相色谱-质谱、气相色谱-氢火焰离子化检测器对分离富集的酚类化合物进行定性与定量分析。结果表明:在最优洗脱条件下,酚类化合物的回收率在93%~108%之间;同一样品重复分离5次后测定目标化合物的含量,结果的相对标准偏差小于5%,方法重复性较好;酚类化合物含量在2~300 μg/g内与峰面积具有良好的线性响应,不同类型酚类化合物的相对响应因子较为接近;催化裂化柴油酚类化合物主要是苯酚、萘酚、菲酚类化合物,其中以苯酚类化合物为主,其含量占酚类化合物总量的69.4%。固相萃取方法可以有效分离催化裂化柴油中的酚类化合物,可用于酚类化合物的定性定量分析过程。

关键词: 固相萃取, 催化裂化, 柴油, 酚类化合物

Abstract: Solid phase extraction (SPE) was used for sample pretreatment to enrich phenolic compounds from FCC diesel oil. The sample was separated into two classes: phenolic compounds and hydrocarbons. The elution conditions of the SPE column were optimized with the standard sample. The recovery and repeatability were tested under the optimized conditions. The qualified and quantified analysis of the compositions of phenolic compounds in fraction rich in phenolic compounds by gas chromatography-mass spectrometry, gas chromatography-flame ionization was conducted. It was shown that the recoveries of the standard compounds are 93%~108% and the relative standard deviation is less than 5% after repeated separation of the same sample for 5 times, indicating a good repeatability of the method. It was revealed that the flame ionization detection has a good linear response in the range of 2~300 μg/g of phenolic compounds; the difference among the relative response factor of phenolic compounds is not significant. It was found that phenols, naphthols and phenanthrols are the main components, of which the phenols account for 69.4%. It is concluded that the phenolic compounds in FCC diesel could be effectively enriched by the SPE method, which could be used for the qualified and quantified analysis of phenolic compounds.

Key words: solid phase extraction, catalytic cracking, diesel oil, phenolic compounds

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