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In homogeneity of sediment samples in analysis of hexabromocyclododecane

机译:六溴环十二烷分析中沉积物样品的均质性

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The repeatability test of the analytical method for hexabromocyclododecane (HBCD) was conducted with sediment sample. The maximum HBCD concentration exceeded the minimum by a factor of 90 even though the identical sediment samples were used. Therefore, we examined which step of the analytical method was the factor causing variability. We examined the blank test, and confirmation test of the extraction and purified procedure. From these results, we confirmed that there was nothing wrong with the accuracy of our analytical method. These results indicate that the variability of HBCD concentration in the repeatability test was attributed not to the analytical method, but to the inhomogeneity of the sediment sample. Aluminum, silicon, and organic carbon in sediments were measured to compare the variability of these concentrations with that of HBCD concentration. These concentrations were similar values within identical samples which showed variability in HBCD concentration. HBCD concentration in several samples did not correlate with organic carbon content. These results suggests that sediment samples were homogeneous by itself, and HBCD was heterogeneously distributed in spite of homogeneity of organic carbon in sediment. The sediment sample with variability in HBCD concentration showed different HBCD diastereomer compositions in identical sediment. It implies that the sample contained HBCD derived from different histories or point sources. Even though we increased sample amounts to analyze the homogeneity of the sample, HBCD concentration varied within identical samples if the sample had a hot spot. Past monitoring data may contain overestimation or underestimation of HBCD concentration in sediment.
机译:对沉积物样品进行六溴环十二烷(HBCD)分析方法的重复性测试。即使使用了相同的沉积物样品,六溴环十二烷的最大浓度也超过了最小值的90倍。因此,我们检查了分析方法的哪一步是引起可变性的因素。我们检查了空白试验,以及提取和纯化步骤的确认试验。根据这些结果,我们确认分析方法的准确性没有问题。这些结果表明,在重复性测试中六溴环十二烷浓度的变化不归因于分析方法,而是归因于沉积物样品的不均匀性。测量了沉积物中的铝,硅和有机碳,以比较这些浓度与六溴环十二烷浓度的变异性。这些浓度在相同样品中的相似值,表明HBCD浓度存在差异。一些样品中的六溴环十二烷浓度与有机碳含量不相关。这些结果表明,尽管沉积物中有机碳的均质性,但沉积物样品本身是均质的,六溴环十二烷是不均匀分布的。六溴环十二烷浓度变化的沉积物样品在相同的沉积物中显示出不同的六溴环十二烷非对映体组成。这意味着样品中包含的六溴环十二烷来自不同的历史或点源。即使我们增加了样品量来分析样品的均质性,但如果样品中有热点,六溴环十二烷的浓度在同一样品中也会有所变化。过去的监测数据可能包含对沉积物中六溴环十二烷浓度的高估或低估。

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