石油炼制与化工 ›› 2012, Vol. 43 ›› Issue (5): 88-92.

• 分析与评定 • 上一篇    下一篇

废水中萃取性石油烃的测定

周艳红,李凌波   

  1. 中国石化抚顺石油化工研究院
  • 收稿日期:2011-10-14 修回日期:2011-11-03 出版日期:2012-05-12 发布日期:2012-04-28
  • 通讯作者: 周艳红 E-mail:zyh126126@126.COM

DETERMINATION OF EXTRACTABLE PETROLEUM HYDROCARBONS IN WASTEWATER

  • Received:2011-10-14 Revised:2011-11-03 Online:2012-05-12 Published:2012-04-28

摘要: 建立了废水中萃取性石油烃(EPH)的液液萃取/硅酸镁净化/气相色谱分析方法,考察了溶剂萃取、萃取物净化和浓缩、气相色谱分析等条件。结果表明:活化硅酸镁净化过程中石油烃的回收率为99.7%~100.0%,不同浓度极性非烃模拟物棕榈酸甲脂或油酸甲脂的脱除率为90.7%~100%;酸碱条件下各萃取3次EPH的回收率为90.3%~92.5%;EPH空白加标回收率为92.0%,EPH基体加标回收率为81.5%,方法检出限为15.2 μg/L,某炼油厂废水6次测定的相对标准偏差为4.1%。

关键词: 废水, 萃取性石油烃, 液-液萃取, 气相色谱法, 硅酸镁净化

Abstract: A method for the determination of extractable petroleum hydrocarbons (EPH) in wastewater, comprising liquid-liquid extraction, purification by florisil and gas chromatography determination, was developed. Sample preparation and analytical conditions were investigated and optimized, including sample extraction, purification and concentration of extracts, and operating parameters of gas chromatography. The results showed that the recovery rates of EPH reached 99.7%—100% during purification by activated florisil; the removal rates of polar non-hydrocarbon model compounds (methyl palmitate or methyl oleate) were in the range of 90.7%—100%; EPH recovery rates reached 90.3%—92.5% by 3-times acidic extraction followed by 3-time alkali extraction. The detection limit of this method was 15.2 μg/L, blank spike and matrix spike recoveries were 92.0% and 81.5%, respectively. A case study of testing a refinery effluent showed that the relative standard deviation (RSD) of determination was 4.1% (n=6).

Key words: wastewater, extractable petroleum hydrocarbons, liquid-liquid extraction, gas chromatography, purification by florisil

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