气相色谱-质谱法测定含油污泥中16种多环芳烃

Determination of 16 PAHs in Oily Sludge Soil by Gas Chromatography-Mass Spectrometry

采用超声提取和固相萃取小柱净化的前处理方法,结合气相色谱-质谱法(GCMS),建立了含油污泥中16种多环芳烃的检测方法。以新疆的油田采油或钻井等过程中产生的含油污泥为样品,经超声提取,固相萃取(SPE)小柱除杂净化后,用GC-MS法进行定量分析。16种多环芳烃在0.005~0.200mg/L范围内线性关系良好,相关系数为0.998~0.999,检出限(S/N=3)在0.26~2.38μg/kg之间,以0.200、0.500和1.000mg/L添加浓度水平进行方法学验证,回收率在60.20%~149.66%范围内,相对标准偏差为3.37%~16.84%。该方法具有快速、简便、灵敏度高等特点,能满足含油污泥中16种多环芳烃的检测要求。

A rapid method for the detection of 16 PAHs in oil sludge of hazardous waste was established by using gas chromatography-mass spectrometry（GC-MS）combining with pre-treatment method of ultrasonic extraction and solid phase extraction（SPE）.Samples were collected from Xinjiang Petroleum during oil extraction or drilling process.After oil sludge were extracted with ultrasonic and cleaned up with SPE,qualitative and quantitative analysis were completed by GC-MS with external standard method.The results showed that the 16 kinds of PAHs had a good linearity over the concentration range of 0.005-0.200mg/L with correlation coefficients of 0.998-0.999.The detection limits（S/N=3）were in the range of 0.26-2.38μg/kg.The recoveries of the PAHs were in the range of 60.20%-149.66%at the standard addition levels of 0.200,0.500 and 1.000mg/L,and the relative standard deviations were in the range of 3.37%-16.84%.It would hopefully serve as an useful method for testing of PAHs in oil sludge.