Determination of Petroleum Hydrocarbons(C10—C40)in Soil by Gas Chromatography with Pressurized Fluid Extraction and Magnesium Silicate Column Purification
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%.
NETL
NSTL
万方数据
