加压流体萃取-硅酸镁柱净化-气相色谱法测定土壤中石油烃(C10~C40)的含量  

Determination of Petroleum Hydrocarbons(C10—C40)in Soil by Gas Chromatography with Pressurized Fluid Extraction and Magnesium Silicate Column Purification

作　　者：王艳丽 陈晨 赵志强 崔连喜 杨华 WANG Yanli;CHEN Chen;ZHAO Zhiqiang;CUI Lianxi;YANG Hua(Tianjin Eco-Environmental Monitoring Center,Tianjin 300191,China)

机构地区：[1]天津市生态环境监测中心,天津300191

出　　处：《理化检验（化学分册）》2024年第6期589-592,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家环境保护标准资助项目(2017-5)。

摘　　要：取10.0 g土壤样品,加入约10 g硅藻土,混匀,脱水,研磨后进行加压流体萃取。以体积比1∶1的正己烷-丙酮混合溶液作提取溶剂,在温度100℃,压力11.70 MPa下静态提取5 min,循环提取2次。浓缩提取液后过活化好的硅酸镁净化柱,收集流出液。用7 mL体积比9∶1的正己烷-丙酮混合溶液洗涤浓缩装置,清洗液过硅酸镁净化柱。合并流出液,浓缩后进入气相色谱仪。在HP-5MS色谱柱上以升温程序分离样品中的石油烃(C10~C40)。结果显示:石油烃(C10~C40)的质量浓度在248~9300 mg·L^(−1)内和峰面积呈线性关系,检出限(3.143s)为2.4 mg·kg^(−1);加标回收率为93.5%~103%,石油烃土壤质控样品中石油烃(C10~C40)的测定值在认定值范围内,测定值的相对标准偏差(n=6)为7.1%~8.8%。An aliquot(10.0 g)of the soil sample was taken,and 10 g of diatomite was added.After mixing,dehydration and grinding,the mixture was treated by pressurized fluid extraction.Static extraction was performed twice with the mixed solution of n-hexane and acetone at volume ratio of 1∶1 as extractant at temperature of 100℃,pressure of 11.70 MPa,and extraction time of 5 min.The extract was concentrated,and passed through the activated magnesium silicate purification column,and the effluent was collected.The concentration device was washed by 7 mL of the mixed solution of n-hexane and acetone at volume ratio of 9∶1,and the washing solution was passed through the activated magnesium silicate purification column.The effluent was combined and concentrated,and the resulting solution was introduced into the gas chromatograph.Petroleum hydrocarbons(C10-C40)in the sample were separated by the heating program on the HP-5MS chromatographic column.It was shown that linear relationship between values of the mass concentration and peak area of petroleum hydrocarbons(C10-C40)was kept in the range of 248-9300 mg·L^(−1),with detection limit(3.143s)of 2.4 mg·kg^(−1).The spiked recoveries were in the range of 93.5%-103%,and the determined values of petroleum hydrocarbons(C10-C40)in soil quality control samples were within the certified value range,with RSDs(n=6)of the determined values in the range of 7.1%-8.8%.

关 键 词：土壤 石油烃(C10~C40) 加压流体萃取 气相色谱法 

分 类 号：O657.7[理学—分析化学]