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建立了吹扫捕集气相色谱质谱联用法测定水中吡啶、丙烯腈、四乙基铅和松节油的方法,对吹扫时间进行了优化,研究了pH值对吹扫捕集率的影响。结果表明,在pH值为6~10时,吹扫时间为11 min时吹扫捕集效率最高,用脉冲控制自动进标样的方法绘制工作曲线,曲线相关系数在0.996~0.999 9之间,方法的检出限在0.06~1.0μg/L之间,相对标准偏差在1.1%~6.2%之间,方法具有很好的线性和精密度。方法用于地表水、生活污水和化工废水中吡啶、丙烯腈、四乙基铅和松节油测定,并进行了加标回收实验,地表水回收率在86.8%~112.1%之间,生活污水回收率在91.9%~99%之间,废水回收率在82.2%～104.3%之间,表明方法具很好的准确度,可用于地表水、生活污水和化工废水中吡啶、丙烯腈、四乙基铅和松节油测定。
A method for the determination of pyridine, acrylonitrile, tetraethyl lead and turpentine in water by purge and trap gas chromatography-mass spectrometry (GC-MS / MS) was established. The purge time was optimized and the effect of pH value on purge and trap efficiency was studied. The results showed that the purge and trapping efficiency was the highest when the purge time was 11 min at the pH value of 6 ~ 10, and the working curve was plotted by pulse-controlled automatic standard injection. The correlation coefficients of the curves ranged from 0.996 to 0.999 9, The detection limits of the method ranged from 0.06 to 1.0 μg / L, with relative standard deviations between 1.1% and 6.2%. The method had good linearity and precision. The method was applied to the determination of pyridine, acrylonitrile, tetraethyl lead and turpentine in surface water, domestic sewage and chemical wastewater, and the spiked recovery experiments were carried out. The recovery rates of surface water were between 86.8% and 112.1% Between 91.9% and 99%, the recovery rate of wastewater was between 82.2% and 104.3%, indicating that the method has good accuracy and can be used for the determination of pyridine, acrylonitrile, tetraethyl lead in surface water, domestic sewage and chemical wastewater And turpentine determination.