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Analysis method for PCBs in reclaimed oil using a fast-GC triple stage quadrupole mass spectrometer with the 13-component quantitation method

机译:使用13组分定量法的快速GC三级四极杆质谱仪分析再生油中的PCB

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摘要

It is necessary for companies supplying reclaimed oil to analyze polychlorinated biphenyls (PCBs), because there is a possibility of the presence of contaminants due to trace-level PCBs in the reclaimed oil. However, common analysis methods of PCBs are time-consuming and complicated. Fast-GC triple stage quadrupole mass spectrometer with the 13-component quantitation method is an official method for analyzing PCBs in insulating oil in Japan. This method is extremely fast and simplified. The purpose of this study involves an investigation of the aforementioned fast and simple method for potential use in the analysis of reclaimed oil. Furthermore, it was attempted to combine the method with sample preparation involving only hexane dilution. The effect of sample dilutions corresponding to 100, 300, and 500 times was evaluated for reducing the matrix effect. The matrix effect was suppressed at a dilution ratio equal to or exceeding 300 times. Calibration curves of four points, namely 0.01, 0.05, 0.1, and 0.5 ng/mL, (ignored origin) by using an internal standard method were prepared for the 13 components. The square of regression coefficient (R2) values of all calibration curves exceeded 0.997. This method was adopted for the analysis of reclaimed oil containing 0.5 μg/mL PCBs, which corresponds to the judgment criteria, and accurate quantitation (accuracy value, 94.0–102%) and good repeatability (%RSD, 3.6%) were obtained. Furthermore, the required sensitivity was maintained even when 800 samples were analyzed without a cleaning ion source and an exchanging analysis column.
机译:供应再生油的公司有必要对多氯联苯(PCB)进行分析,因为再生油中可能会存在痕量PCB导致污染物的存在。但是,常见的PCB分析方法既费时又复杂。采用13组分定量法的Fast-GC三级四极杆质谱仪是日本分析绝缘油中PCBs的官方方法。此方法非常快速且简化。这项研究的目的涉及对上述快速,简单方法的研究,以用于再生油的分析。此外,尝试将该方法与仅涉及己烷稀释的样品制备相结合。为了减少基质效应,评估了对应于100、300和500倍的样品稀释液的影响。当稀释倍率等于或超过300倍时,基质效应被抑制。使用13种组分通过内标法制备了四个点的校正曲线,即0.01、0.05、0.1和0.5ng / mL(忽略来源)。所有校准曲线的回归系数(R 2 )值的平方均超过0.997。该方法被用于分析含0.5μg/ mL PCBs的再生油,这符合判断标准,并获得了准确的定量(准确度值,94.0–102%)和良好的重复性(%RSD,3.6%)。此外,即使在不使用清洁离子源和交换分析柱的情况下分析800个样品时,也可以保持所需的灵敏度。

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