涡旋辅助分散液液微萃取-气相色谱法测定饮用水中11种氯苯类化合物

移取饮用水样品10.0mL,加入0.5g氯化钠和100μL二硫化碳,以2 500r·min^-1转速离心5min,静置5min后,移取离心管底部的沉积相(约65μL),采用气相色谱法测定其中11种氯苯类化合物的含量。11种氯苯类化合物用Agilent J&W DB-WAX毛细管色谱柱分离,电子俘获检测器检测。11种氯苯类化合物的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.032～0.97μg·L^-1。以空白样品为基体进行加标回收试验,所得回收率为86.7%～101%,测定值的相对标准偏差(n=6)为1.2%～3.3%。

GC Determination of 11 Chlorobenzenes in Drinking Water with Dispersive Liquid-Liquid Microextraction Assisted by Vortex

The drinking water sample(10.0 mL) was taken,and then sodium chloride(0.5 g) and carbon disulfide(100μL) were added.The above mixture was centrifugated for 5 min at the speed of 2 500 r·min-1.After standing for 5 min,the sedimentation at the bottom of centrifugal tube(about 65μL) was taken.GC was applied to the determination of 11 chlorobenzenes in the sedimentation.11 chlorobenzenes were separated on Agilent J&W DBWAX capillary chromatographic column and detected by ECD.Linear relationships between values of peak area and mass concentration of the 11 chlorobenzenes were kept in definite ranges.Detection limits(3S/N)of the method ranged from 0.032 to 0.97μg·L-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 86.7%-101%,with RSDs(n=6) of determined values in the range of 1.2%-3.3%.