摘要
建立了用顶空气相色谱–质谱联用仪测定土壤中丙烯腈的方法。优化色谱–质谱联用仪和顶空仪对温度、时间等分析条件的设置,选用HP–INNOWAX(30 m×0.32 mm,0.50μm)毛细管柱,在柱流速1.5 mL/min条件下采用电子轰击电离源,选择离子m/z 53进行外标法定量。该方法线性良好,相关系数r=0.9997。当土壤取样量为2.0 g时,方法检出限为0.22 mg/kg。在两个不同加标水平下,丙烯腈测定结果的相对标准偏差为4.1%～10.0%(n=6),土壤样品的加标回收率为87.2%～97.0%。该方法可快速、准确测定土壤样品中的丙烯腈。
A method was established to determine acrylonitrile in soils by headspace-gas chromatography-mass spectrometry.The analytical conditions such as temperature and time of headspace and chromatography-mass spectrometry were optimized.The analysis was carried out with a capillary column （HP-INNOWAX 30 m × 0.32 mm, 0.50 μm） on electron ionization conditions at a flow rate of 1.5 mL/min, and the quantitation was performed by the external standard method using selected ion of m/z 53. The calibration curve showed a good linearity for acrylonitrile （r=0.999 7）. The detection limit was 0.22 mg/kg when using 2.0 g soil samples. At two different concentration levels, the relative standard deviation of acrylonitrile determination results was 4.1% -10.0%（n=6）. The recoveries of spiked soil samples were in the range of 87.2% --97.0%. The method can determine acrylonitrile in soil samples rapidly and accurately.
出处
《化学分析计量》
CAS
2011年第6期51-53,共3页
Chemical Analysis And Meterage
基金
杭州市环境保护科研课题(2010013)
