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赵江华, 王鹏, 黎卫亮, 李忠煜. 复垦土地样品中石油类物质加速溶剂萃取-荧光分光光度法分析方法研究[J]. 岩矿测试, 2021, 40(3): 375-383. DOI: 10.15898/j.cnki.11-2131/td.202011200150
引用本文: 赵江华, 王鹏, 黎卫亮, 李忠煜. 复垦土地样品中石油类物质加速溶剂萃取-荧光分光光度法分析方法研究[J]. 岩矿测试, 2021, 40(3): 375-383. DOI: 10.15898/j.cnki.11-2131/td.202011200150
ZHAO Jiang-hua, WANG Peng, LI Wei-liang, LI Zhong-yu. Determination of the Petroleum Substances in Samples of Reclaimed Land by Fluorescence Spectrophotometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis, 2021, 40(3): 375-383. DOI: 10.15898/j.cnki.11-2131/td.202011200150
Citation: ZHAO Jiang-hua, WANG Peng, LI Wei-liang, LI Zhong-yu. Determination of the Petroleum Substances in Samples of Reclaimed Land by Fluorescence Spectrophotometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis, 2021, 40(3): 375-383. DOI: 10.15898/j.cnki.11-2131/td.202011200150

复垦土地样品中石油类物质加速溶剂萃取-荧光分光光度法分析方法研究

Determination of the Petroleum Substances in Samples of Reclaimed Land by Fluorescence Spectrophotometry with Accelerated Solvent Extraction

  • 摘要: 作为土地环境质量的一项重要指标,石油类物质含量决定了土地的用途。对于复垦土地样品,在一定程度上反映了污染土地的复垦、治理效果。土壤样中的石油类物质测定方法主要有气相色谱法、红外分光光度法、紫外光谱法等。气相色谱法主要应用于测定样品中的饱和烷烃;红外分光光度法通过测定不同波数下的特征吸收值来表征样品中石油类物质,但采用四氯乙烯为溶剂,试剂环境危害大,前处理效率低,检出限高。本文针对复垦土地样品中石油类物质含量不高,组分多为难挥发且结构复杂、基质干扰大的特点,采用正己烷为溶剂、加速溶剂萃取(ASE)前处理,荧光分光光度计测定样品中的石油类物质。以海洋环境监测石油标准物质为标准样品配制工作曲线,线性相关系数r2=0.9997;方法检出限为0.40mg/kg,检测下限为1.60mg/kg;实际样品方法精密度为1.10%~8.76%;基质加标回收率为89.0%~95.7%;检测实际样品的结果与现行有效的HJ 1051—2019红外分光光度法基本一致,高含量样品的测定结果高于红外法。本方法所用溶剂正己烷的毒性小于四氯乙烯,前处理方法ASE的自动化程度高,萃取效率高,精密度提高11.5%~67.3%。对于石油类组分结构相对复杂、难提取的样品,本方法检出限低于红外法(4mg/kg)。

     

    Abstract:
    BACKGROUNDAs an important index of land environmental quality, the content of petroleum substances determines the use of the land. It also reflects the effect of reclamation and treatment of polluted land to a large extent. The determination methods of petroleum substances in soil samples include gas chromatography, infrared spectrometry, and ultraviolet method. The gas chromatography mainly analyzes saturated alkanes in the samples. The infrared spectrometry identifies the petroleum substances in the samples by measuring the characteristic absorption values under different wave numbers. However, tetrachloroethene used as the solvent is harmful to the environment. Moreover, the pretreatment efficiency is low and the detection limit is high.
    OBJECTIVESTo develop a method with high pre-treatment efficiency, low detection limit and good reproducibility.
    METHODSPetroleum substances in the reclaimed land samples have low content, most of the components are difficult to volatilize, the structure is complex, and the matrix interference is large. Using n-hexane as the solvent and accelerated solvent extraction (ASE) as the pretreatment method, the petroleum substances in the samples were determined by fluorescence photometer.
    RESULTSUsing the petroleum standard material for marine environmental monitoring as the calibration material to prepare a working curve, the linear correlation coefficient was 0.9997, the detection limit was 0.40mg/kg, precision was 1.10% to 8.76% and the recovery was 89.0% to 95.7%. The results of actual samples were consistent with those of the currently valid infrared spectrophotometry method HJ 1051-2019, and the measurement results of high-content samples were higher than those of the infrared method.
    CONCLUSIONSThe pretreatment method ASE has high automation and high extraction efficiency. It can be used to increase the precision by 11.5%-67.3%. For samples with a relatively complex structure of petroleum components and that are difficult to extract, the detection limit of this method is lower than that of the infrared method (4mg/kg).

     

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