Determination of Semi-Volatile Organic Compounds in Petroleum Hydrocarbon Contaminated Soil by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry
摘 要
取被石油烃污染的土壤样品经快速萃取仪萃取后,用经活化的Silica硅胶小柱进行净化,用正己烷淋洗,弃去前1.0 mL正己烷淋洗液,再用体积比为1∶19的丙酮-正己烷混合溶剂洗脱。洗脱液氮吹浓缩至小于1.0 mL,加内标物并用正己烷定容至1.0 mL,过滤。滤液中半挥发性有机物(SVOC)经气相色谱分离后采用电子轰击离子源、全扫描和选择离子监测模式进行质谱分析,采用内标法定量。方法比较了不同固相萃取小柱、正己烷的用量、洗脱剂的种类等条件对样品净化效果的影响,在优化的试验条件下,SVOC的线性范围均为1~20 mg·L-1,检出限为0.06~0.30 mg·kg-1。按标准加入法在3个浓度水平进行回收试验,在低加标水平下,测得回收率较高,为35.8%~145%,测定值的相对标准偏差(n=6)为0.60%~15%。
Abstract
The sample of petroleum hydrocarbon contaminated soil was extracted by rapid extractor, and purified with activated Silica gel solid-phase extraction column. n-Hexane was used as rinse solvent, and the initial 1.0 mL of rinse solution was discarded, then the analytes were eluted from the column with acetone-n-hexane mixed solvent (the vlume ratio of 1:19). The eluate was concentrated and dried to less than 1.0 mL by nitrogen blowing, and the residue was added with internal standard and made up its volume to 1.0 mL, and the solution was filtered. Semi-volatile organic compounds (SVOC) in filtrate were separated by GC and determined by MS with EI, full scan mode and selective ion monitoring mode. The effect of the different solid phase extraction columns, the amount of n-hexane, and the type of eluent on purification of sample were compared. Under the optimized test conditions, linearity ranges of SVOC were found in the same range of 1-20 mg·L-1, with detection limits in the range of 0.06-0.30 mg·kg-1. Tests for recovery were made by standard addition method at the three concentration levels, higer values of recovery were found at the low standard addition level in the range of 35.8%-145%. RSDs (n=6) of measured values were ranged from 0.60% to 15%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202104008
所属栏目 工作简报
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收稿日期 2020/1/16
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备注黄国程,本科,研究方向为有机仪器分析
引用该论文: HUANG Guocheng,ZHENG Yaoli. Determination of Semi-Volatile Organic Compounds in Petroleum Hydrocarbon Contaminated Soil by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(4): 327~338
黄国程,郑瑶丽. 固相萃取-气相色谱-质谱法测定石油烃污染土壤中半挥发性有机物[J]. 理化检验-化学分册, 2021, 57(4): 327~338
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参考文献
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