理化检验-化学分册2024,Vol.60Issue(8) :796-801.DOI:10.11973/lhjy-hx230262

超声辅助乳化萃取结合气相色谱-质谱法测定废水中8种酚类污染物的含量

Determination of 8 Phenolic Pollutants in Wastewater by Gas Chromatography-Mass Spectrometry Coupled with Ultrasound-Assisted Emulsion Extraction

柴瑞娜 陈鹏飞 成建国 马力通 段建国
理化检验-化学分册2024,Vol.60Issue(8) :796-801.DOI:10.11973/lhjy-hx230262

超声辅助乳化萃取结合气相色谱-质谱法测定废水中8种酚类污染物的含量

Determination of 8 Phenolic Pollutants in Wastewater by Gas Chromatography-Mass Spectrometry Coupled with Ultrasound-Assisted Emulsion Extraction

柴瑞娜 1陈鹏飞 1成建国 2马力通 2段建国3
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作者信息

  • 1. 内蒙古科技大学化学与化工学院,包头 014010
  • 2. 内蒙古科技大学化学与化工学院,包头 014010;生物煤化工综合利用内蒙古自治区工程研究中心,包头 014010
  • 3. 内蒙古科技大学化学与化工学院,包头 014010;化工煤炭综合利用实验室,包头 014010
  • 折叠

摘要

通过优化萃取条件和色谱条件,提出题示方法测定废水中苯酚、邻氯苯酚、邻甲酚、对甲酚、2,5-二甲基苯酚、3,5-二甲基苯酚、2,4-二甲基苯酚、喹啉等8种酚类污染物的含量.废水样品经沉淀、过滤后,分取样品20 mL,加入4.0 g氯化钠,振荡2 min.加入20 mL二氯甲烷,超声乳化萃取5 min,置于分液漏斗中静置5 min.分取有机相,于10 ℃浓缩至2~3 mL,用二氯甲烷稀释至5 mL.加入1 g无水硫酸钠,放置10 h,脱去水分,所得溶液进入气相色谱-质谱仪,在Agilent DB-VRX色谱柱(30 m×0.25 mm,1.4 μm)上程序升温分离样品溶液中8种酚类污染物,分别采用全扫描(SCAN)、选择离子监测(SIM)模式进行定性和定量分析.结果表明:8种酚类污染物的质量浓度在0.50~500.00 μg·L-1内和峰面积呈线性关系,检出限(3S/N)为0.02~0.07 μg·L-1.按照标准加入法进行回收试验,回收率为76.8%~114%,测定值的相对标准偏差(n=6)不大于10%.方法用于地表水和煤化工废水样品的分析,地表水中检出了 2.40 μg·L-1苯酚和1.3 μg·L-1对甲酚,煤化工废水中检出了 8种酚类污染物(检出量1.21~30.63 μg·L-1).

Abstract

By optimizing extraction and chromatographic conditions,the title method was proposed to determine 8 phenolic pollutants in wastewater,including phenol,o-chlorophenol,o-cresol,p-cresol,2,5-dimethylphenol,3,5-dimethylphenol,2,4-dimethylphenol,and quinoline.After settling and filtering the wastewater sample,20 mL of the sample was taken.Then 4.0 g of sodium chloride was added,and the mixture was shaken for 2 min.After 20 mL of dichloromethanen was added,ultrasonic emulsification extraction was performed for 5 min.The mixed solution was placed into a separating funnel to settle for 5 min.The organic phase was taken,and concentrated to 2-3 mL at 10 ℃.The concentrated solution was diluted to 5 mL by dichloromethane,and 1 g of anhydrous sodium sulfate was added.The mixture was settled for 10 h to remove the moisture,and the resulting solution was introduced into the gas chromatograph-mass spectrometer.Program temperature separation of 8 phenolic pollutants in the sample solution was conducted on the Agilent DB-VRX chromatographic column(30 mm×0.25 mm,1.4 μm).Qualitative and quantitative analysis was performed by full scan(SCAN)and selective ion monitoring(SIM)modes,respectively.It was shown that linear relationships between values of the mass concentration and peak area of 8 phenolic pollutants were kept in the range of 0.50-500.00 μg·L-1,with detection limits(3S/N)in the range of 0.02-0.07 μg·L-1.Test for recovery was made according to the standard addition method,giving recoveries in the range of 76.8%-114%,and RSDs(n=6)of the determined values not more than 10%.The proposed method was used for the analysis of surface water and coal chemical wastewater samples,2.40 μg·L-1 phenol and 1.3 μg·L-1 p-cresol were detected in surface water,and 8 phenolic pollutants were detected in coal chemical wastewater with detection amounts in the range of 1.21-30.63 μg·L-1.

关键词

超声辅助乳化萃取/气相色谱-质谱法/酚类污染物/废水

Key words

ultrasound-assisted emulsion extraction/gas chromatography-mass spectrometry/phenolic pollutant/wastewater

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基金项目

内蒙古自然科学基金项目(2022QN02007)

内蒙古自治区教育厅项目(NJZY21402)

2022年内蒙古自治区大学生创新训练项目()

出版年

2024
理化检验-化学分册
上海材料研究所

理化检验-化学分册

CSTPCDCSCD北大核心
影响因子:0.647
ISSN:1001-4020
参考文献量16
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