广州化工2025,Vol.53Issue(1) :102-106.DOI:10.20220/j.cnki.1001-9677.2025.01.029

磁子搅拌法提取土壤中11种半挥发性有机物的测定

Determination of 11 Semi-volatile Organic Compounds from Soil by Magnetic Netic Stirring

何国忠 王克华 李军 赵志敏 姚路鹏
广州化工2025,Vol.53Issue(1) :102-106.DOI:10.20220/j.cnki.1001-9677.2025.01.029

磁子搅拌法提取土壤中11种半挥发性有机物的测定

Determination of 11 Semi-volatile Organic Compounds from Soil by Magnetic Netic Stirring

何国忠 1王克华 1李军 2赵志敏 1姚路鹏1
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作者信息

  • 1. 新疆水清清监测技术服务有限公司,新疆 乌鲁木齐 830000
  • 2. 鉴优检测技术江苏有限公司,江苏 苏州 215000
  • 折叠

摘要

采用磁子搅拌法提取土壤中11种半挥发性有机物的测定.称取20.0 g制备好的土壤样品,以(1+1)二氯甲烷-丙酮混合液为提取剂,在保持磁子转速为高速、提取液温度45℃下提取30 min,提取液经无水硫酸钠干燥,高通量真空平行浓缩仪浓缩,弗罗里硅土固相萃取小柱净化后继续浓缩定容至1.0 mL,用气相色谱-质谱仪检测土壤中11种半挥发性有机物,内标法定量.11种半挥发性有机物在曲线浓度范围1.0~40 mg/L之间相关系数均大于等于0.994,检出限为0.05~0.1 mg/kg,测定下限为0.2~0.4 mg/kg,加标回收率为55.7%~106%,相对标准偏差为0.8%~12%,和现有标准方法的检出限0.04~0.4 mg/kg,测定下限0.16~1.6 mg/kg,加标回收率47%~119%,相对标准偏差2.9%~44%;相比检出限,测定下限,加标回收率,相对标准偏差相比较均满足要求.

Abstract

11 semi-volatile organic compounds in soil by magnetic stirring method were determined.20.0 g prepared soil samples were weaghted,with(1+1)chloride-acetone mixture as extraction agent,keeping the magnetic speed speed for high speed,extracted for 30 min in 45 ℃,drying by anhydrous sodium sulfate,concentrated,by high throughput vacuum parallel concentration instrument purified to 1.0 mL by florida silicon soil solid phase extraction column,11 kinds of semi-volatile organic compounds in soil were analyzed by gas chromatography-mass spectrometer,and determined by internal standard.The correlation coefficients between 11 semi-volatile compounds concentrations range of 1.0 to 40 mg/L were greater than or equal to 0.994,the detection limit was in the range of 0.05 to 0.1 mg/kg,The lower measurement limit was in the range of 0.2 to 0.4 mg/kg,55.7%to 106%,the relative standard deviation was in the range of 0.8%to 12%,and the detection limit was in the range of 0.04 to 0.4 mg/kg,lower measurement limit was in the range of 0.16 to 1.6 mg/kg,47%to 119%,relative standard deviation was in the range of 2.9%to 44%.Compared to the detection limit,lower measurement limit,spiking recovery rate,the relative standard deviation all meet the requirements.

关键词

磁子转速/提取剂温度/提取时间/提取效率/土壤/11种半挥发性有机物

Key words

magnetic speed speed/extraction temperature/extraction time/extraction efficiency/soil/11 kinds of semi-volatile organic compounds

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出版年

2025
广州化工
广州市化工行业协会 广州市化学化工学会 广州市化学工业研究所

广州化工

影响因子:0.358
ISSN:1001-9677
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