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    气相色谱-电子捕获检测器法同时测定土壤中2,4-二硝基甲苯、2,4,6-三硝基甲苯和黑索金的含量

    Simultaneous Determination of 2,4-Dinitrotoluene, 2,4,6-Trinitrotoluene and Hexogen in Soil by Gas Chromatography with Electron Capture Detector

    • 摘要: 为实现土壤中2,4-二硝基甲苯、2,4,6-三硝基甲苯、黑索金的同时、快速、准确测定,进行了题示研究。采集土壤样品,于−50 ℃、真空压力9 Pa下冷冻干燥约40 h。取20 g样品,混匀后采用萃取溶剂体积比1∶1的丙酮-正己烷混合溶液在萃取温度100 ℃、氮气吹扫时间20 s的条件下进行加压流体萃取。于40 ℃将萃取液浓缩至约1 mL,过活化好的硅酸镁小柱,收集流出液,常压氮吹浓缩至约0.5 mL后用体积比1∶1的丙酮-正己烷混合溶液定容至1.0 mL。所得溶液进入气相色谱仪,在DB-5和DB-17色谱柱上以程序升温条件分离目标物,电子捕获检测器检测。结果显示:3种目标物的质量浓度均在一定范围内和峰面积呈线性关系,检出限(3.143 s)分别为2,1,2 μg·kg−1;按照标准加入法进行回收试验,回收率为71.6%~118%,测定值的相对标准偏差(n=6)为1.6%~13%。

       

      Abstract: To achieve simultaneous, rapid, and accurate determination of 2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and hexogen in soil, the study mentioned by the title was conducted. Soil samples were collected and freeze-dried for about 40 h at −50 ℃ and vacuum pressure of 9 Pa. An aliquot (20 g) was taken and homogenized, followed by pressurized fluid extraction using the mixed solution of acetone and n-hexane at volume ratio of 1∶1 as the extractant under extraction temperature of 100 ℃ and nitrogen purge time of 20 s. After the extract was concentrated to about 1 mL at 40 ℃, the solution was passed through the activated magnesium silicate column, and the effluent was collected, and concentrated to about 0.5 mL by nitrogen under atmospheric pressure. The volume of the solution obtained was made up to 1.0 mL with the mixed solution of acetone and n-hexane at volume ratio of 1∶1. The resulting solution was introduced into the gas chromatograph, and target compounds were separated on DB-5 and DB-17 columns under the temperature programmed conditions, and detected using electron capture detector. It was shown that linear relationships between the mass concentrations and peak areas of the 3 target compounds were kept in definite ranges, with detection limits (3.143s) of 2, 1, 2 μg·kg−1, respectively. Test for recovery was performed using the standard addition method, giving recoveries in the range of 71.6%–118%, and RSDs (n=6) of the determined values ranged from 1.6% to 13%.

       

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