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在线衍生-膜进样-VUV电离-飞行时间质谱法测定废水中酚类化合物

Online Measurement of Phenols in Wastewater by Membrane Inlet-VUV Ionization-Time of Flight Mass Spectrometry

    摘要
  • 摘要: 酚类化合物是染料、炼焦、造纸等工业废水中的主要污染物，污染范围广、危害大，因此有必要发展在线灵敏的测量方法对其进行监测和控制。我们利用自主研制的膜进样-真空紫外(VUV)电离-飞行时间质谱仪(time of flight mass spectrometer, TOFMS), 发展了一种快速测量水中苯酚、3-甲酚、2-氯酚和2，4-二氯酚的方法。实验发现：经乙酸酐衍生化反应后，酚类化合物的检测灵敏度可以大大提高；用聚二甲基硅烷（PDMS）膜直接进样可以缩短样品的分析检测时间，使单个样品的分析时间小于15 min。同时，由于单光子电离技术产生的碎片峰很少，谱图解析方便，可以不用分离直接测量混合物样品。优化实验参数（反应时间、pH值、乙酸酐加入量等）后，苯酚、3-甲酚、2-氯酚和2，4-二氯酚的检出限分别达到3、6、8、14 μg•L-1，线性范围达到2个数量级。

     

    Abstract: Developing new methods for online monitoring of phenols in wastewater is highly demanding, as phenols are common pollutes in wastewater from dying, coking and papermaking industry. In this work, a new method was introduced for online determination of phenols in wastewater by membrane inlet-vacuum ultraviolet (VUV) ionization-time of flight mass spectrometry (TOFMS). The fragment-free ionization technique (single-photon ionization, SPI) using vacuum ultraviolet (VUV) lamp was especially useful for online measurement of organic compounds without pre-separation. Phenols was introduced directly into MS through polydimethylsilane (PDMS) membrane after derivatization, the analysis time of individual sample was less than 15 min. Parameters, such as the acetylation reaction time, pH, the added amount of acetic anhydride and flow rate, etc, were optimized. At optimization condition, the limits of detection for phenol, 3-methylphenol, 2-chlorophenol, 2,4-dichlorophenol are 3，6，8，14 μg•L-1, respectively, and the linear dynamic ranges are two orders. The present online monitoring method of phenols shows great potential applications to detect phenols in wastewater.

     

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