吹扫捕集-气相色谱-质谱法同时测定水中11种醚类化合物

Simultaneous Determination of 11 Ether Compounds in Water by GC-MS with Purge and Trap

采用已加入4g质量比为3∶1的碳酸钠和氯化钠的混合物(盐析剂)的40mL棕色硼硅玻璃瓶采集水样,使水样充满样品瓶。采用吹扫捕集-气相色谱-质谱法同时测定水样中11种醚类化合物的含量。在气相色谱分离中采用HP-VOC色谱柱(90m×0.32mm,1.8μm),在质谱分析中采用选择离子监测模式。以氟苯为内标,环氧乙烷、环氧丙烷、四氢呋喃的线性范围均为5.0~100μg·L-1,其他8种醚类化合物的线性范围均为0.50~50μg·L-1,检出限为0.113~2.62μg·L-1。以空白管网末梢水样品为基体进行加标回收试验,所得回收率为85.3%~115%,测定值的相对标准偏差(n=6)为3.0%~9.4%。

Brown borosilicate glass bottle of 40 mL was used to collect water sample with 4 g of mixture of sodium carbonate and sodium chloride(mass ratio of 3∶1)as salting out agent.The bottle was filled with the water sample.GC-MS was applied to the simultaneous determination of 11 ether compounds in the water sample with purge and trap.The HP-VOC chromatographic column(90 m×0.32 mm,1.8μm)was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Fluorobenzene was used as internal standard.Linearity ranges of ethylene oxide,propylene oxide and tetrahydrofuran were found in the same range of 5.0-100μg·L-1 and linearity ranges of other 8 ether compounds were found in the same range of 0.50-50μg·L-1,with detection limits in the range of 0.113-2.62μg·L-1.On the base of blank sample of terminal tap water,test for recovery was made by standard addition method;values of recovery found were in the range of 85.3%-115%,with RSDs(n=6)of determined values in the range of 3.0%-9.4%.