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A simple method for the selective quantification of polyethylene, polypropylene, and polystyrene plastic debris in soil by pyrolysis-gas chromatography/mass spectrometry

机译:通过热解 - 气相色谱/质谱法选择性地定量聚乙烯,聚丙烯和聚苯乙烯塑料碎片的简单方法

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The lack of adequate analytical methods for the quantification of plastic debris in soil challenges a better understanding of their occurrence and fate in the terrestrial environment. With this proof-of-principle study, we developed a simple and fast method for the selective quantification of the three most environmentally relevant polymers polyethylene (PE), polypropylene (PP), and polystyrene (PS) in soil using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). In order to facilitate the preparation of calibration series and to better account for the heterogeneity of soil matrix, polymers were dissolved in 1,2,4-trichlorobenzene (TCB) at 120 degrees C. Thereby, liquid sample aliquots from up to 4 g of solid sample became amenable to pyrolysis without further preparation. To evaluate the performance of this approach, three reference soils with 1.73-5.16% organic carbon (C-org) were spiked at 50 and 250 mu g g(-1) of each polymer and extracted with TCB. Prior cleanup steps with methanol, flocculation with KAl(SO4)(2), or Fenton digestion were tested for their suitability to reduce potentially interfering C-org. Calibration curves responded linearly (adj. R-2 0.996) with instrumental detection limits of 1-86 ng corresponding to method detection limits of 1-86 mu g g(-1). The measurement repeatability was 3.2-7.2% relative standard deviation. Recoveries of 70-128% were achieved for plastic contents of 250 mu g g(-1) extracted with TCB without prior cleanup from soils with less than 2.5% C-org. A higher C-org particularly interfered with the quantification of PE. The addition of non-target polymers (polyethylene terephthalate, polyvinyl chloride, poly (methyl methacrylate), and tire wear particles) did not interfere with the quantification of the analytes highlighting the selectivity of the method. Further research is needed to determine low plastic contents in soils exceeding 2.5% C-org. With 1-3 h processing time per sample, our method has the potential for routine analyses and screening studies of agricultural systems to be complemented with microspectroscopic techniques for additional information on particle shapes and sizes.
机译:缺乏足够的分析方法来定量土壤中的塑料碎片挑战,更好地了解其在陆地环境中的发生和命运。通过这种原则上的研究,我们开发了一种使用热解 - 气相色谱法/的三种最环保的聚合物聚乙烯(PE),聚丙烯(PP),聚丙烯(PP)和聚苯乙烯(PS)的选择性提供的简单和快速的方法。/质谱(Py-GC / MS)。为了便于校准系列的制备并更好地解释土壤基质的异质性,将聚合物在120℃下溶于1,2,4-三氯苯(TCB)中。因此,液体样品等分试样可从多达4g固体样品在没有进一步制备的情况下均可过热。为了评估这种方法的性能,将具有1.73-5.16%的有机碳(C-ORG)的三种参考土壤以50和250μg(-1)的每种聚合物掺入并用TCB萃取。用甲醇的先前清理步骤,测试用kal(SO 4)(2)或Fenton消化的絮凝以减少潜在干扰C-Org。校准曲线线性(ADJ.R-2> 0.996)响应,具有1-86 ng的仪器检测限,对应于1-86μg(-1)的方法检测限。测量重复性为3.2-7.2%相对标准偏差。对于用TCB提取的250μmg(-1)的塑料含量,实现了70-128%的回收率,而无需从少于2.5%C-ORG的土壤清除。更高的C-org特别干扰PE的定量。添加非靶聚合物(聚对苯二甲酸乙二醇酯,聚氯乙烯,聚(甲基丙烯酸甲酯)和轮胎磨损颗粒)并未干扰分析物的定量,突出了该方法的选择性。需要进一步研究以确定超过2.5%C-Org的土壤中的低塑料含量。每种样品处理1-3小时,我们的方法具有常规分析和农业系统的筛选研究,以互补微型光谱技术,以进行颗粒形状和尺寸的额外信息。

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