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    超声-微波协同萃取分离、气相色谱-质谱联用测定土壤中多环芳烃

    GC-MS Determination of Polycyclic Aromatic Hydrocarbons in Soil After Solvent Extraction Separation with co-assisted Ultrasonic and Microwave Techniques

    • 摘要: 建立了常温常压条件下超声-微波协同萃取分离、气相色谱-质谱法(GC-MS)测定土壤样品中微量多环芳烃的方法,结果表明:在土壤含水量和无机盐质量分数分别为10%和6%时,以正已烷-二氯甲烷(1+1)混合溶液40 mL作萃取溶剂,采用100 W微波辐射功率(超声振动功率固定为50 W)萃取9 min,模拟土壤样品中多环芳烃平均回收率可达86.9%,其相对标准偏差为3.6%;通过与索氏抽提、高压密闭微波和开放式微波、直接超声波和间接超声波等萃取方法相比,证明此方法具有样品容量大、萃取时间短、萃取效率高、重现性好等优点.

       

      Abstract: Ultrasonic and microwave techniques were applied in combination to the extraction of traces of polycyclic aromatic hydrocarbons (PAHs) from soil sample using mixture of n-hexane and dichloromethane (1+1) as solvent.The extract,after dehydration and concentration,was used for GC-MS determination of the PAHs.When the moisture content and inorganic salt content of the soil sample were 10% and 6% respectively,and under working conditions of ① using 40 mL of the mixed solvent,② power of microwave radiation 100 W,③ power of ultrasonic vibration 50 W and ④ time of extraction 9 min,the recovery obtained in the analysis of simulated samples attained to 86.9%,and average values of RSD′s (n=5) found was 3.6%.As compared with several other methods of extraction,including the soxhlet extraction,open or closed vessel microwave assisted extraction and direct or indirect ultrasonic agitation extraction,the present method was proved to have higher capacity and efficiency as well as better repeatability.

       

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