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通过优化顶空气相分析中的平衡温度、平衡时间、加盐量及固液比等实验参数,建立自动顶空—气相色谱快速测定生活饮用水中6种消毒副产物残留的方法。结果表明:在固液比为1∶1,加氯化钠量为3 g,70℃下平衡15 min后进行顶空自动进样分析,6种消毒副产物灵敏度大幅提高,该法操作简单,可节省大量时间,适用于水样批量检测。通过方法学验证的结果显示,6种目标物在相应浓度范围内的线性关系良好(R~2>0.998),检出限为0.004μg/L(四氯化碳)~0.342μg/L(二氯甲烷),定量限为0.013μg/L(二氯一溴甲烷)~1.34μg/L(二氯甲烷);不同浓度水平的加标回收率在82.9%~97.5%范围内,相对标准偏差为0.86%~3.25%(n=5)。方法适用于基层疾控中心对生活饮用水卫生监测的需要。
The method of rapid determination of six kinds of disinfection by-products in domestic drinking water by automatic headspace-gas chromatography was established by optimizing the experimental parameters such as equilibrium temperature, equilibration time, salt addition and solid-liquid ratio in headspace gas analysis. The results showed that the headspace autoinjection analysis was carried out at the solid-to-liquid ratio of 1: 1, the addition of sodium chloride at 3 g and the equilibrium at 70 ℃ for 15 min. The sensitivity of six kinds of disinfection by-products was greatly increased. Can save a lot of time, suitable for batch testing of water samples. The results of methodological validation showed that the linearity of the six target compounds was good (R ~ 2> 0.998) with the detection limits of 0.004μg / L (CCl 4) ~ 0.342μg / L The limits of quantification were 0.013μg / L (dichloromethane) to 1.34μg / L (dichloromethane). The spiked recoveries of different concentrations ranged from 82.9% to 97.5% with a relative standard deviation of 0.86 % ~ 3.25% (n = 5). The method is suitable for the needs of the grass-roots CDCs for the sanitary monitoring of drinking water.