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    加速溶剂萃取-气相色谱法测定化工园区土壤中石油烃(C10~C40)的含量

    Determination of Petroleum Hydrocarbons (C10-C40) in Soil of Chemical Industrial Park by Gas Chromatography with Accelerated Solvent Extraction

    • 摘要: 样品参照标准处理后,分取约10 g,加入约8 g灼烧后的硅藻土,混合均匀,以体积比1∶1的丙酮-正己烷混合液进行加速溶剂萃取,萃取液浓缩至约1 mL后依照HJ 1021—2019净化。净化液进入气相色谱仪,其中的石油烃(C10~C40)在HP-5色谱柱上以升温程序分离,外标法定量。结果显示:石油烃(C10~C40)的质量浓度在31~6 200 mg·L−1内和保留时间窗5.09~32.78 min内的总峰面积呈线性关系,检出限(3.143s)为3.93 mg·kg−1;按照标准加入法进行回收试验,回收率为96.8%~102%,测定值的相对标准偏差(n=6)为8.2%~9.0%,有证标准物质测定值的相对误差为-9.7%。方法用于化工园区15个采样点的50个土壤样品的分析,在46个样品中检出了石油烃(C10~C40),最高检出量为540 mg·kg−1

       

      Abstract: After processing the sample according to the standard, about 10 g of the sample was taken, and 8 g of the burned diatomaceous earth was added. The mixture was mixed evenly, and accelerated solvent extraction was performed with acetone-n-hexane mixed solution at a volume ratio of 1∶1. The extract was concentrated to about 1 mL and purified according to HJ 1021—2019. The purified liquid was introduced into the gas chromatograph, and the petroleum hydrocarbons (C10-C40) were separated by the heating program on HP-5 chromatographic column, and quantified by the external standard method. It was shown that linear relationship between values of the mass concentration of petroleum hydrocarbons (C10-C40) and total peak area within the retention time window of 5.09-32.78 min was kept in the range of 31-6 200 mg·L−1, with detection limit (3.143s) of 3.93 mg·kg−1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 96.8%-102%, and RSDs (n=6) of the determined values in the range of 8.2%-9.0%. The relative error of the determined value of certified reference material was −9.7%. The proposed method was used for the analysis of 50 soil samples from 15 sampling points in the chemical industrial park. Petroleum hydrocarbons (C10-C40) were detected in 46 samples, with the highest detection amount of 540 mg·kg−1.

       

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