静态顶空-气相色谱/质谱法同时检测环境水体中59种挥发性有机物

Simultaneous Determination of 59 Volatile Organic Compounds in Environmental Water Using Headspace Sampling Method Coupled to Gas Chromatography-Mass Spectrometry

中文关键词:  环境水体  挥发性有机物  静态顶空-气相色谱/质谱法

英文关键词:environmental water  volatile organic compounds  HS-GC/MS

中文摘要:

      静态顶空法是一种简单、环保的样品前处理方法.通过对比试验，优化了影响静态顶空进样方法灵敏度的主要因素，确定了较佳的样品盐度（40%）、平衡温度（80℃）、平衡时间（10 min）、平衡压力（0.103 4 MPa）、定量环平衡时间（20 s）、进样时间（3 min）等前处理方法参数.采用优化后水样前处理条件及1.00 kV的检测器电压，59种挥发性有机物在特定的线性范围内，标准曲线线性相关系数均大于0.998，方法检出限为丙烯腈4.4 μg/L、硝基苯7.6 μg/L，其余挥发性有机物（VOCs）介于0.06~1.4 μg/L，饮用水源水及污水处理厂进水实际样品加标回收率为60%~110%，精密度（RSD）为0.33%~22%（n=6）.建立的静态顶空-气相色谱/质谱法（HS-GC/MS）水样前处理过程自动化，可同时对水中59种挥发性有机物进行检测.

英文摘要:

      The headspace sampling (HS) method is a simple, environmentally friendly method. The measurement of 59 kinds of volatile organic compounds(VOCs) in environmental water using HS coupled gas chromatography/mass spectrometry (GC/MS) was discussed. Under the optimal headspace sampling conditions, a detector gain of 1.00 kV, a sample salinity of 40%, an equilibrium temperature of 80℃, an equilibrium time of 10 min, an equilibrium pressure of 0.103 4 MPa, a pressure equilibration time of 45 s, a loop equilibration time of 20 s, a loop inject time of 3 min were get up, and the obtained detection limits were 0.06~7.6 μg/L, with r>0.998. The obtained average recovery ratios were 60%~110% (n=6) in spiked samples from drinking source and sewage plants, with a RSD of 0.33%~22% (n=6). The HS-GC/MS method with automatic water pretreatment can be applied to the simultaneous measurement of 59 VOCs in water samples with high efficiency.