顶空固相微萃取-气相色谱法测定水中四乙基铅

GC Determination of Tetraethyl Lead in Water with HS-SPME

提出了顶空固相微萃取-气相色谱法测定水中四乙基铅含量的方法。为使固相微萃取达到更高的效率,选用聚二甲基硅氧烷填料(PDMS)作为微萃取的涂层,萃取温度及时间为60℃和30min。用DB-5色谱柱分离,用电子捕获检测器检测。四乙基铅的质量浓度在0.05～20.0μg·L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)为0.02μg·L-1。以水样为基体,在3种浓度水平下进行加标回收试验,回收率在87.0%～90.1%之间,测定值的相对标准偏差(n=7)在3.7%～4.2%之间。

GC with headspace-solid phase micro-extraction（HS-SPME） was applied to the determination of tetraethyl lead in water.To attain a higher efficiency in SPME,the PDMS fiber was selected as coating for the micro-extraction,and the extraction was carried out at 60 ℃ for 30 min.The analyte were separated on DB-5 chromatography column and detected by ECD.Linear relationship between values of peak area and mass concentration of tetraethyl lead was kept in the range of 0.05-20.0 μg·L-1,with detection limit（3S/N） of 0.02 μg·L-1.Using water sample as matrix,test for recovery was made by addition of standard solution at 3 concentration levels,values of recovery found were in the range of 87.0%-90.1% with RSD′s（n=7） in the range of 3.7%-4.2%.