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李媛,段小燕,施玉格,等. 振荡提取-荧光分光光度法分析土壤样品中石油类物质[J]. 岩矿测试,2023,42(6):1240−1247. DOI: 10.15898/j.ykcs.202211150218
引用本文: 李媛,段小燕,施玉格,等. 振荡提取-荧光分光光度法分析土壤样品中石油类物质[J]. 岩矿测试,2023,42(6):1240−1247. DOI: 10.15898/j.ykcs.202211150218
LI Yuan,DUAN Xiaoyan,SHI Yuge,et al. Determination of Petroleum Oil in Soil by Fluorescence Spectrophotometry with Oscillatory Extraction[J]. Rock and Mineral Analysis,2023,42(6):1240−1247. DOI: 10.15898/j.ykcs.202211150218
Citation: LI Yuan,DUAN Xiaoyan,SHI Yuge,et al. Determination of Petroleum Oil in Soil by Fluorescence Spectrophotometry with Oscillatory Extraction[J]. Rock and Mineral Analysis,2023,42(6):1240−1247. DOI: 10.15898/j.ykcs.202211150218

振荡提取-荧光分光光度法分析土壤样品中石油类物质

Determination of Petroleum Oil in Soil by Fluorescence Spectrophotometry with Oscillatory Extraction

  • 摘要: 石油类物质是中国建设用地土壤污染风险管控的污染物之一,开展土壤中石油类物质的检测对土壤污染防治工作具有重要意义。本文采用正己烷为萃取溶剂,土壤经振荡提取后,以荧光光度法为检测手段,建立了一种绿色环保、灵敏高效的土壤石油类物质检测方法。通过对实验过程进行优化,该方法的线性相关系数r≥0.999,检出限为3mg/kg。使用10种不同类型土壤进行方法精密度和准确度验证,精密度为2.5%~9.2%,基体加标回收率为80.0%~110%。为验证方法可比性,分别使用本方法和《土壤 石油类的测定 红外分光光度法》(HJ 1051—2019)对5种不同类型土壤进行检测比对,测定结果相对偏差在5.0%~15%之间,具有较好的一致性。

     

    Abstract:
    BACKGROUND As an important index of soil environmental quality, the determination of petroleum oil has become one of the must-test items in environmental monitoring. The gravimetric method is not suitable for the purpose of environmental monitoring because it can only be used for the determination of non-volatile substances and has low sensitivity. Gas chromatography is mainly used for the determination of C10-C40 saturated alkanes in samples. The infrared spectrometry used characteristic absorption at different wavenumber to characterize the content of petroleum substances in the samples, but the response of infrared spectrometry to aromatic hydrocarbons is not sensitive.
    OBJECTIVES To establish a simple pre-treatment efficiency, low detection limit and good reproducible method for determination of petroleum oil in soil.
    METHODS Using n-hexane as the solvent, adsorption column as the extraction method and oscillatory as the pretreatment method, petroleum oil was extracted from soil and determined by fluorescence spectrophotometry.
    RESULTS Under the optimal conditions that with 275nm as the excitation wavelength and 315nm as the emission wavelength, the extraction solvent was n-hexane and the extraction method was adsorption column, the calibration curves of petroleum oil were linear with correlation coefficients 0.999, and the detection limit was 3mg/kg. The relative standard derivations (RSDs) were from 2.5% to 9.2% and the average spiked recoveries were between 80.0% and 110%. Compared with the currently valid infrared spectrometry method (HJ 1051—2019), the results of the two methods were consistent.
    CONCLUSIONS The solvent of n-hexane has higher toxicity and stability than tetrachloroethene, and better environmental friendliness. The oscillatory extraction method is simple and easy to operate. The detection limit of this method is lower than that of infrared spectrometry (4mg/kg), and the precision and accuracy of the method is good. This method can be used as a supplement to the existing methods for the detection of petroleum in soil.

     

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