多溴联苯醚提取方法的优化与应用

N. Stojić, M. Pucarević, D. Prokić, S. Štrbac, Anastasija Joksimović
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引用次数: 0

摘要

采用32因子试验设计(DOE)确定了8种多溴联苯醚(PBDEs)的最佳提取工艺。自变量分为三个层次编码,在初步实验结果的基础上选取自变量的实际值。DOE包括9组,在中心点有3个重复。采用二阶多项式模型进行响应预测。优化提取时间、溶剂比、纯化比和仪器参数后,对24个潜在污染地点(垃圾填埋场、前组组场、二次原料堆放场和汽车废弃物)土壤表层样品进行了优化。采用气相色谱-电子捕获检测(GC-ECD)法测定多溴二苯醚。五种浓度水平下BDE同源物的回收率在80% ~ 115%之间。在绝对干燥土壤中,多溴二苯醚的总浓度在4.4 ~ 729g kg-1之间。通过对各变量参数的实验值与预测值的比较,验证了实验的适用性。
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Optimisation and application of polybrominated diphenyl ethers extraction method
The optimal conditions for the extraction of eight polybrominated diphenyl ethers (PBDEs) were determined using 32 factorial design of experiments (DOE). The independent variables were coded at three levels and their actual values were selected on the basis of the preliminary experimental results. DOE consisted of nine runs with three replicates at the central point. A second-order polynomial model was used for predicting the response. After the optimization of the duration of extraction, the ratio of solvents and purification and instrumental parameters, the optimized conditions were applied on the samples taken from the surface layer of soil from 24 potentially contaminated locations (landfills, ex marshalling yard, dump of secondary raw materials and automotive waste). The gas chromatographic analysis with electron capture detection (GC-ECD) was used for the determination of PBDEs. The recovery values of BDE congeners at five concentration levels ranged between 80% and 115%. The total PBDEs concentrations ranged from 4.4 to 729 ?g kg-1 of absolutely dry soil. The suitability of the experiment was proved by comparing the experimental and predicted values of the variable parameters.
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