摘要
建立超声提取气相色谱质谱法测定土壤中苯胺和硝基苯的方法。土壤经40 mL二氯甲烷在超声功率60 Hz下提取30 min,经30℃水浴和7~10 psi氮吹压力浓缩至1 mL后上机测定。在优化的气相色谱条件下,苯胺和硝基苯在质量浓度50~1000μg/L范围内线性关系良好,检出限分别为1.61μg/kg和0.17μg/kg。对实际土壤样品添加10~100μg/kg进行加标回收试验,苯胺和硝基苯的回收率分别在67.7%~96.9%和83.5%~93.7%,相对标准偏差(n=6)在3.24%~10.2%和2.51%~7.26%,而且有证标准物质测定结果满意。其方法简单、快速、准确,能够满足实际大批量土壤样品快速检测的需求。
The determination of aniline and nitrobenzene in soil by gas chromatography/mass spectrometry assisted with ultrasonic extraction was proposed.Soil sample was extracted with 40 mL dichloromethane under an ultrasonic power of 60 Hz for 30 min,and then concentrated to 1 mL by a 30℃water bath and 7~10 psi nitrogen blowing pressure.Under optimized gas chromatography conditions,the linear relationship between the peak area and the mass concentration of aniline and nitrobenzene was in the range of 50.0~1000μg/L,with the detection limits of 1.61μg/kg and 0.17μg/kg,respectively.The recovery rates measured by adding standard samples to soil sample were in the range of 67.7%~96.9%for aniline and 83.5%~93.7%for nitrobenzene,with the relative standard deviations in the range of 3.24%~10.2%(n=6)and 2.51%~7.26%(n=6),respectively.Besides,the test results of certified reference materials are satisfactory.This method is simple,fast and accurate.It was suitable for the rapid determination of aniline and nitrobenzene in soil samples.
作者
刘田
陈加伟
宋洲
周宇齐
罗火焰
方绍敏
Liu Tian;Chen Jiawei;Song Zhou;Zhou Yuqi;Luo Huoyan;Fang Shaomin(Hubei Province Geological Experimental Testing Center,Wuhan,Hubei 430034)
出处
《资源环境与工程》
2020年第4期627-631,共5页
Resources Environment & Engineering
基金
湖北省地质局科研项目——水溶剂绿色提取超高效液相色谱串联质谱法测定土壤中典型极性有机污染物研究(项目编号:KJ2020-30)
湖北省地质实验测试中心科研项目——超声辅助提取气相色谱—质谱法测定土壤中苯胺类化合物。
关键词
苯胺
硝基苯
土壤
气相色谱质谱法
超声提取
aniline
nitrobenzene
soil
gas chromatography-mass spectrometry
ultrasonic extraction
