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超临界二氧化碳萃取含油污泥中16种多环芳烃 被引量:11

Study of approaches about determination of 16 PAHs in oily sludge soil by gas chromatograph-mass spectrometry
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摘要 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 rapid detection method on 16 PAHs in oil sludge of hazardous waste was established by using gas chromatography-mass spectrometry (GC-MS) combined with pre-treatment method of supereritieal fluid extraction (SFE) and cleaned up with solid phase extraction (SPE). Samples are from Xinjiang Petroleum that were oil sludge created by oil extraction or drilling process. After oil sludge was extracted with SFE and cleaned up with SPE. Qualitative and quantitative analysis were completed by GC/MS with external standard method. The results showed that the 16 PAHs had a good linear relationship over concentration range of 0. 005 -0. 200 mg/L with correlation coefficients of 0. 998 - 0. 999. The limits of detection ( LODs, S/N = 3 ) were in the range of 0. 26 - 2. 38 μg/kg. The recoveries of the PAHs were in the range of 48.2% - 113.3% at the standard addition levels of 0. 200, 0. 500, and 1. 000 mg/L, and the relative standard deviations (RSDs) were in the range of 3.5% - 14%.
出处 《分析试验室》 CAS CSCD 北大核心 2017年第1期12-15,共4页 Chinese Journal of Analysis Laboratory
基金 国家自然科学基金项目(21262036)资助
关键词 含油污泥 超临界二氧化碳 固相萃取柱 气相色谱-质谱法 危险废物 Oil sludge Supercritieal fluid extraction SPE GC-MS PAHS Hazardous waste
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