加速溶剂萃取-气相色谱法测定化工园区土壤中石油烃(C_(10)~C_(40))的含量  

Determination of Petroleum Hydrocarbons(C_(10)-C_(40))in Soil of Chemical Industrial Park by Gas Chromatography with Accelerated Solvent Extraction

作　　者：李超群 蒋敬思 刘立平 赵锦华 吴宗源 任颖俊 LI Chaoqun;JIANG Jingsi;LIU Liping;ZHAO Jinhua;WU Zongyuan;REN Yingjun(Changsha Mineral Resources Inspection Center of Ministry of Natural Resources,Changsha 410007,China;Central South University of Forestry and Technology,Changsha 410004,China)

机构地区：[1]自然资源部长沙矿产资源检测中心,长沙410007 [2]中南林业科技大学,长沙410004

出　　处：《理化检验(化学分册)》2025年第2期176-181,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国土资源部公益性行业专项基金资助项目(201411107-3)。

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(C_(10)~C_(40))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(C_(10)~C_(40))的质量浓度在31~6200 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(C_(10)~C_(40)),最高检出量为540 mg·kg^(-1)。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-nhexane 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(C_(10)~C_(40))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(C_(10)~C_(40))and total peak area within the retention time window of 5.09-32.78 min was kept in the range of 31-6200 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%^(-1)02%,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(C_(10)~C_(40))were detected in 46 samples,with the highest detection amount of 540 mg·kg−1.

关 键 词：石油烃(C_(10)~C_(40)) 加速溶剂萃取 气相色谱法 土壤 化工园区 

分 类 号：O657.7[理学—分析化学]