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采用超临界流体(SFE)萃取和固相萃取柱(SPE)净化的前处理方法结合气相色谱-质谱法(GC-MS)建立了危险废物含油污泥中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原料,经超临界流体萃取,SPE固相萃取小柱除杂净化后,用GC-MS进行定量分析。16种多环芳烃在0.005~0.200 mg/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1.000 mg/L添加量水平进行方法学验证,回收率在48.2%~113.3%范围内,相对标准偏差为3.5%~14%。
A method for determination of 16 polycyclic aromatic hydrocarbons (PAHs) in oily sludge of hazardous wastes was established by gas chromatography-mass spectrometry (GC-MS) with SFE and SPE pretreatment methods. Taking oily sludge produced in the process of oil recovery or drilling in Xinjiang oilfield as raw material, the sample was purified by supercritical fluid extraction (SPE) and SPE solid phase extraction (SPE) cartridge, and then quantified by GC-MS. The correlation coefficients of the 16 PAHs in the range of 0.005 ~ 0.200 mg / L were 0.998 ~ 0.999. The detection limits (S / N = 3) ranged from 0.26 to 2.38 μg / kg and the correlation coefficients were 0.200, 0.500 and The method was validated by the level of 1.000 mg / L, the recoveries ranged from 48.2% to 113.3%, and the relative standard deviations were 3.5% ~ 14%.