石油炼制与化工 ›› 2021, Vol. 52 ›› Issue (12): 102-108.

• 分析与评定 • 上一篇    下一篇

深度加氢柴油中咔唑类化合物的测定

周婧1,2,史得军1,霍明辰1,陈菲1,李荣观1,黄星亮2   

  1. 1.  中国石油石油化工研究院
    2. 中国石油大学(北京)
  • 收稿日期:2021-03-11 修回日期:2021-06-07 出版日期:2021-12-12 发布日期:2021-12-01
  • 通讯作者: 史得军 E-mail:shidejun163@163.com
  • 基金资助:
    中石油公司发展战略与科技基础工作决策支持研究

DETERMINATION OF CARBAZOLE COMPOUNDS IN DEEP HYDROGENATED DIESEL

  • Received:2021-03-11 Revised:2021-06-07 Online:2021-12-12 Published:2021-12-01

摘要: 建立了采用气相色谱-四极杆-飞行时间质谱仪定性、定量分析深度加氢柴油中咔唑类化合物的方法。该方法可对质量分数为ng/g级的5类咔唑类化合物进行分析,定量标准曲线的线性相关系数R2大于0.9980,回收率范围为81.86%~89.27%,相对标准偏差范围为2.36%~4.14%,重复性较好,最低检出限为0.000 4~0.001 6mg/L,定量限为0.001 2~0.005 4 mg/L,灵敏度较高。利用该方法对不同加氢深度的加氢柴油中咔唑类化合物进行分析检测,结果表明:咔唑、甲基咔唑易于在加氢精制过程中脱除;1位、8位甲基取代的二甲基咔唑类、三甲基咔唑类化合物空间位阻较大,在加氢条件下较难脱除。

关键词: 气相色谱-四极杆-飞行时间质谱, 咔唑类化合物, 柴油, 加氢

Abstract: A gas chromatography quadrupole time-of-flight mass spectrometry method was developed for the qualitative and quantitative measurement of carbazole compounds in deeply hydrogenated diesel. This method could be used for qualitative analysis of five carbazole compounds with mass fraction in ng/g level,the linear correlation coefficient of the quantitative standard curve was above 0.998 0, and the recovery range was 81.86%-89.27%. The relative standard deviation range was 2.36%-4.14%,showing that the quantitative accuracy of the method was good. The minimum detection limits were 0.000 4-0.001 6 mg/L and the quantitation limits were 0.001 2-0.005 4 mg/L,illustrating that the sensitivity of the method was high. The carbazole compounds in hydrogenated diesel with different hydrofining depths were analyzed by this method. The results showed that carbazole and methyl carbazole was easily removed in the hydrofining process, and the 1- or 8-methyl-substituted dimethylcarbazole and trimethylcarbazole compounds had large steric hindrance and were difficult to be removed by hydrogenation.

Key words: gas chromatography quadrupole time-of-flight mass spectrometry, carbazole compounds, diesel, hydrogenation