利用气液相色谱法评估鉴定车用汽油的法医技术的可靠性

G. Bebeshko, G. G. Omel’yanyuk, O. V. Samoilova, A. I. Usov
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引用次数: 0

摘要

提出了一种新方法来解决石油产品、燃料和润滑剂的法医检验问题,即确定车用汽油是否属于共同/不同的鉴定组合。利用色谱法确定受控参数的定量结果以及随后根据既定标准对成对比较样品的结果进行评估的方法来鉴定汽油。选定以下参数作为控制指标:研究辛烷值 (RON)、碳氢化合物组(石蜡、异构烷烃、炔烃、环烷烃、烯烃)和含氧化合物的浓度。它们的测定采用标准化方法进行。我们使用了 Chromatek-Crystal 5000 系列的硬件和软件组合,包括 Chromatek-DHA 数据处理程序。就专家提出的问题确定了估计标准或决策规则,以便将汽油归类为一个产品名称(通用集)、一种生产技术(组集)或一个共同的原产地(一个生产批次、储罐等)。该方法的可靠性通过由三个阶段组成的验证程序进行评估。我们使用了 2022 年 6 个月期间在莫斯科各区四家石油公司加油站收集的 AI-92 车用汽油。在第一阶段,执行人员在不同时间分别分析了四个汽油样品(之前属于同一体积的样品)中的 12 个等分样品。结果表明,所建议方法的质量指标(重复性和再现性的标准偏差、扩大的不确定性、重复性和再现性的极限)中的每一个确定的控制指标都没有超过标准方法所规定的允许误差。在实验的第二阶段,执行人员将每个生产商(一种生产技术)的 12 个测试样品分成四组,每组有三个不同生产时间(不同批次)的样品。通过比较组内各组样品之间相同受控指标测量值的差异和各组之间平均指标的差异,承包商确定了使用相同技术生产的汽油、使用相同技术生产但生产时间不同(不同批次)的汽油,以及具有共同来源(以前属于同一批次)的汽油,概率为 95%。验证研究的结论与样品的原始数据相吻合,这证实了所制定的比较标准的正确性。在第三阶段(盲测),表演者检查了 7 个汽油样品,但没有向他提供这些样品的成分 和特性信息。盲测结果令人满意。因此,验证结果表明,该方法适用于解决与车用汽油有关的法医鉴定问题,执行人员的能力足以实施该方法。
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Assessing the reliability of the forensic technique for the identification study of motor gasoline using gas-liquid chromatography
A new approach to solving the problems of forensic examination of petroleum products, fuels and lubricants associated with establishing whether motor gasoline belongs to a common/different identification set is proposed. A methodology for the identification of gasoline using quantitative results of chromatographic determination of controlled parameters and subsequent evaluation of the results in pairwise compared samples according to the established criteria. The following parameters were selected as controlled indicators: values of research octane number (RON), concentrations of hydrocarbon groups (paraffins, isoparaffins, arenes, naphthenes, olefins) and oxygenates. Their determination was carried out using standardized methods. We used the hardware and software complex of a Chromatek-Crystal 5000 series, including the Chromatek-DHA data processing program. Estimated criteria or decision- making rules regarding the issues posed to an expert were determined to classify gasoline under one product name (generic set), one production technology (group set) or a common source of origin (one production batch, storage tank, etc.). The reliability of the method was assessed using a validation procedure consisted of three stages. We used a collection of AI-92 motor gasoline, selected at gas stations of four oil companies during six months of 2022 in various districts of Moscow. At the first stage, the performer analyzed 12 aliquots of each of four gasoline samples (samples that previously belonged to the common volume) at different times. It was established that the quality indicators of the proposed methodology (standard deviation of the repeatability and reproducibility, expanded uncertainty, limits of the repeatability and reproducibility) for each of the determined controlled indicators did not exceed the permissible errors established by standardized methods. At the second stage of the experiment, the performer combined 12 test samples into four groups from each manufacturer (one production technology) with three samples of different production times (different batches). By comparing the discrepancies in the measured values of the same controlled indicators between pairs of samples within groups and the discrepancy in average indicators between pairs of groups, the contractor identified gasolines manufactured using the same technology; gasolines produced by the same technology, but at different times (different batches) and, with a probability of 95%, gasolines having a common source of origin (previously belonging to a common volume). The conclusions of the validation study matched the original data on the samples, which confirmed the correctness of the developed comparison criteria. At the third stage (blind test), the performer examined seven gasoline samples of, information about the composition and properties of which was not provided to him. The results of the blind test were considered satisfactory. Thus, the validation results indicate the suitability of the methodology for solving forensic identification problems in relation to motor gasoline and the competence of the performer sufficient for implementation of the methodology.
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