吹扫捕集-气相色谱-质谱联用测定水中的双环戊二烯

Determination of Dicyclopentadiene in Water by Gas Chromatography-Mass Spectrometry with Purge and Trap

建立了测定水中双环戊二烯(DCPD)的吹扫捕集-气相色谱-质谱联用方法。对吹扫捕集测定条件进行了考察和优化,确定的最佳实验条件如下,吹扫气流速为40 m L/min,吹扫时间为11 min,解吸温度为250℃,解吸时间为2. 0 min。选用选择离子模式(SIM)进行检测,在2. 0~200. 0 ng/L范围内,DCPD浓度与仪器响应值间的线性相关系数为0. 999 1,方法的测定下限为2. 0 ng/L;地下水、地表水和出厂水中三种不同浓度加标水平(2. 0、100. 0、180. 0 ng/L)的平均回收率为103. 30%~108. 77%,相对标准偏差<5%(n=6)。利用本方法测定的含有汽油味的水中的DCPD含量分别为地下水685. 921、5 380. 327 ng/L,地表水84. 589、151. 157 ng/L和饮用水12. 277、10. 924 ng/L。

The analysis method was established for the determination of dicyclopentadiene （DCPD） in water by gas chromatography-mass spectrometry with purge and trap （P ＆ T-GC-MS）. The optimum experimental conditions were as follows ： purge gas flow rate was 40 mL/min, purge time was 11 min, the desorption temperature was 250 ℃, and desorption period was 2.0 min. Under the selective ion monitoring （SIM） mode, a good linear relation was observed between the concentration of DCPD and the response of the signal within the range of 2.0 - 200.0 ng/L, the correlation coefficient was O. 999 1. The lower limit of detection was 2.0 ng/L. The relative standard deviation was less than 5% （ n = 6）. The average recovery of DCPD ranged from 103.30% - 108.77% in the spiked concentration levels of 2.0 ng/L, 100.0 ng/L and 180.0 ng/L, respectively. Finally, the method established in the present study was examined by the gasoline-flavored water samples analysis. The content of DCPD detected was 685. 921 ng/L and 5 380.327 ng/L for ground water, 84. 589 ng/L and 151. 157 ng/L for surface water, 12. 277 ng/L and 10. 924 ng/L for drinking water, respectively.