静态顶空-气相色谱质谱法测定地表水中硝基苯、硝基甲苯和硝基氯苯的研究

Determination of nitrobenzene,nitrotoluene and nitrochlorobenzene in surface water by static headspace GC-MS

建立静态顶空-气相色谱质谱法测定地表水中硝基苯、硝基甲苯和硝基氯苯化合物的方法。采用正交试验讨论了平衡温度、平衡时间和加盐量等因素对测定结果的影响,结果表明,最优的实验条件为平衡温度85℃、平衡时间20min、加盐量3.0g。在此条件下,硝基苯、硝基甲苯和硝基氯苯能够有效分离,在2.0~100μg·L^(-1)范围内线性良好,相关系数r>0.999,检出限为0.19~0.40μg·L^(-1),加标回收率为88.8%~108.9%,相对标准偏差(n=8)为2.2%~8.9%。以地表水为基体做加标回收试验,加标回收率达到93.5%~113.1%,相对标准偏差在3.3%~5.1%。

A method for the determination of nitrobenzene,nitrotoluene and nitrochlorobenzene in surface water by static headspace gas chromatography-mass spectrometry was established.The effects of equilibrium temperature,equilibrium time and salt dosage on the determination results were discussed by orthogonal test,the results showed that the optimal experimental conditions were equilibrium temperature of 85℃,equilibrium time of 20min and salt addition of 3.0g.Under these conditions,nitrobenzene,nitrotoluene and nitrochlorobenzene can be effectively separated and the linearity was good in the range of 2.0~100μg·L^(-1)with the correlation coefficient over 0.999,the detection limit was 0.19~0.40μg·L^(-1),the recovery was 88.8%~108.9%,and the relative standard deviation(n=8)was2.2%~8.9%.Taking surface water as the matrix,the recovery rate of standard addition was 93.5%~113.1%,and the relative standard deviation was 3.3%~5.1%.