顶空-GC/MS法同时测定废水中16种挥发性酮、醇、酯、腈类化合物

为了准确分析挥发性酮、醇、酯、腈类化合物在废水中的残留情况，建立了顶空-气相色谱-质谱法测定废水中16种挥发性酮、醇、酯、腈类化合物的方法，选用DB-624（30 m×0.32 mm×1.8 μm）毛细管柱，在柱流速1.5 mL/min条件下，采用电子轰击电离源，全扫描定性，选择离子进行外标法定量。结果表明16种化合物线性良好，相关系数r>0.995。当废水取样量为10.0 L时，方法检出限为0.04~0.95 mg/L，在3个不同加标水平下，实际废水样品中16种化合物的相对标准偏差为0.32%~7.61%，加标平均回收率为89.2%~118%。本方法可快速、准确测定废水样品中的16种挥发性酮、醇、酯、腈类化合物。

Simultaneous Determination of Sixteen Kinds of Volatile Ketones, Alcohols,Esters,Nitriles in Wastewater by Headspace-GC/MS

In odrer to accurately analyze the residue of volatile ketone,alcohol,esters,nitriles in wastewater,the method was established to determine 16 kinds of volatile Ketones,Alcohols,Esters,Nitriles in wastewater by headspace-gas chromatography-mass spectrometry.The analysis was carried out with a capillary column DB-624(30 m×0.32 mm×1.8 μm)under electron ionization conditions at a flow rate of 1.5 mL/min,the qualitation was performed by the mode of scanning and the quantitation was performed by the external standard method using selected ion.The results showed that all calibration curves of 16 kinds of compounds had good linearity for acrylonitrile(r>0.999 5).The detection limits were in the range of 0.04—0.95 mg/L when using 10.0 mL wastewater samples.At three different concentration levels,the average recoveries of 16 kinds of compounds in spiked practical wastewater samples were in the range of 89.2%—118% with relative standard deviation of 0.32%—7.61%.The method can rapidly and accurately monitor sixteen kinds of volatile Ketones,Alcohols,Esters,Nitriles in wastewater.