振荡提取-荧光分光光度法分析土壤样品中石油类物质

TL271%S151.9; 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...

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Published in岩矿测试 Vol. 42; no. 6; pp. 1240 - 1247
Main Authors 李媛, 段小燕, 施玉格, 李刚
Format Journal Article
LanguageChinese
Published 新疆生态环境监测总站,新疆乌鲁木齐 830011 01.11.2023
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ISSN0254-5357
DOI10.15898/j.ykcs.202211150218

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Abstract TL271%S151.9; 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.
AbstractList TL271%S151.9; 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_FL 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.
Author 李刚
李媛
段小燕
施玉格
AuthorAffiliation 新疆生态环境监测总站,新疆乌鲁木齐 830011
AuthorAffiliation_xml – name: 新疆生态环境监测总站,新疆乌鲁木齐 830011
Author_FL LI Yuan
DUAN Xiaoyan
LI Gang
SHI Yuge
Author_FL_xml – sequence: 1
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DocumentTitle_FL Determination of Petroleum Oil in Soil by Fluorescence Spectrophotometry with Oscillatory Extraction
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Keywords fluorescence spectrophotometry
hexane
oscillatory extraction
正己烷
petroleum oil
石油类
振荡提取法
soil
土壤
荧光分光光度法
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Title 振荡提取-荧光分光光度法分析土壤样品中石油类物质
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