摘要
污染场地调查土壤污染物检测是场地调查中的重点难点项目。本文建立了气相色谱质谱法测定污染场地调查土壤中邻苯二甲酸酐。样品首先进行水分测定,加压流体萃取,氮吹浓缩。浓缩液经过层析柱净化或者硅胶柱子净化后定容至1.0m L,气相色谱质谱法测定。结果表明,邻苯二甲酸酐的线性关系良好,相关系数达到0.9999,检出限为0.07 mg/kg,测定下限为0.28 mg/kg,不同浓度的加标回收率为73.3%~126.7%,符合标准方法70%~130%的要求。同时测得精密度(相对标准偏差)为4.4%~9.5%,符合标准方法中实验室内相对标准偏差≤20%的要求。该方法操作简单方便,重现性好,回收率符合要求,精密度高,能够有效检测污染场地调查土壤污染物邻苯二甲酸酐。
The detection of soil pollutants in contaminated sites is a key and difficult project in site investigation.A gas chromatography-mass spectrometry(GC-MS)method was established for the determination of Phthalic anhydride in soil of contaminated sites.The sample is first subjected to moisture determination,pressurized fluid extraction,and nitrogen blowing concentration.The concentrated solution is purified by chromatography or silica gel column,and then brought to a constant volume of 1.0 mL for determination by gas chromatography-mass spectrometry.The results showed that the linear relationship of Phthalic anhydride was good,the correlation coefficient reached 0.9999,the detection limit was 0.07 mg/kg,the lower limit of determination was 0.28 mg/kg,and the recovery rate of different concentrations of spiked phthalic anhydride was 73.3%~126.7%,meeting the requirements of the standard method of 70%~130%.The precision(relative standard deviation)measured simultaneously is 4.4%~9.5%,which meets the requirement of laboratory relative standard deviation≤20%in the standard method.This method is simple and convenient to operate,with good reproducibility,satisfactory recovery rate and high precision,and can effectively detect Phthalic anhydride,a soil pollutant in contaminated sites.
作者
陈秋雯
罗杰鸿
Chen Qiuwen;Luo Jiehong(Guangdong Anna Testing Technology Co.,Ltd.,Guangzhou 510000,China)
出处
《广东化工》
CAS
2023年第22期136-138,共3页
Guangdong Chemical Industry
关键词
污染场地调查土壤污染物
气相色谱质谱法
邻苯二甲酸酐
加压流体萃取
层析柱净化
polluted site investigation of soil pollutants
gas chromatography-mass spectrometry
phthalic anhydride
pressurized fluid extraction
chromatography column purification
