An intercalibration study on organobromine compounds: Results on polybrominated diphenylethers and related dioxin-like compounds.
An intercalibration study on organobromine compounds: Results on polybrominated diphenylethers and related dioxin-like compounds.
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有机溴化合物的相互校准研究：多溴二苯醚和相关二恶英类化合物的结果。
DOI：
10.1016/j.chemosphere.2005.12.008
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发表时间：
2006
期刊：
影响因子：
8.8
通讯作者：
I. Watanabe
中科院分区：
文献类型：
--
作者：
Shin Takahashi;S. Sakai;I. Watanabe
为评价溴化阻燃剂(如多溴二苯醚)及其相关化合物如多溴和一溴多氯二苯并呋喃(PBDDs/DFS、MoBPCDDs/DFS)分析的准确性和可靠性，对有机溴化合物进行了内部校准研究。本文报道了这些化合物在“混合标准溶液”和“风干沉淀物”中的测定结果。在混合标准溶液中，PBDEs、PBDDs/DFS和MoBPCDDs/DFS的相对标准偏差分别为9%~24%、4%~20%和8%~27%。这项研究的结果比早先的国际实验室间研究报告的结果更好，这是由于分析方法的普遍改进和现有可信标准的增加，特别是对多溴二苯醚。在分析八溴二苯二恶英等溴化程度较高的化合物时，由于注意到相对反应系数的变化，建议参与者优化校准曲线，以适应样品中发现的浓度范围。风干沉淀物的测定结果也比较合理，相对标准偏差分别为10%~38%(PBDEs)、8%~38%(PBDDs/DFS)和17%~36%(MoBPCDDs/DFS)。在沉积物样品中，指出了样品前处理中可能的错误和/或其他化合物/杂质的干扰。在某些色谱条件下，五溴二苯醚BDE100的浓度变化比其他PBDE异构体大，这是因为它在某些色谱条件下分离较差。此外，在多溴联苯并呋喃的分析中也观察到了多溴二苯醚的干扰。提出了在索氏提取过程中加入铜粉时，多溴二苯醚和多溴联苯并呋喃在索氏提取过程中的潜在降解/二次生成。尽管有这些观察，但这项研究的结果比其他实验室间研究报告的结果更好，这是因为向参与者提供了改善结果的建议。与PCDDs/DFS(5-23%RSD)和Co-PCbs(6-24%RSD)的结果相比，大多数有机溴化合物的RSD都很高，表明与常见的氯化二恶英相比，用于分析PBDEs和相关化合物的QA/QC方法还不成熟。
An intercalibration study on organobromine compounds has been conducted to evaluate the accuracy and reliability in the analysis of brominated flame retardants (BFRs) such as polybrominated diphenyl ethers (PBDEs) and their related compounds like polybrominated and monobromo-polychlorinated dibenzodioxins and -furans (PBDDs/DFs, MoBPCDDs/DFs). This paper reports the results for these compounds in ‘Mixed Standard Solutions’ and ‘Air-Dried Sediment’. The relative standard deviations (RSDs) for PBDEs, PBDDs/DFs and MoBPCDDs/DFs in mixed standard solutions ranged from 9% to 24%, 4% to 20% and 8% to 27%, respectively. The results of this study are better than those reported in earlier international interlaboratory studies due to general improvement in analytical methods and an increasing number of available authentic standards, particularly for PBDEs. In the analysis for higher brominated compounds such as octabromodibenzodioxin, the participants were advised to optimize the calibration curves befitting the range of concentrations found in samples because variation of relative response factors was noted. The results for ‘Air-Dried Sediment’ were also reasonable with RSDs from 10% to 38% for PBDEs, 8% to 38% for PBDDs/DFs and 17% to 36% for MoBPCDDs/DFs. In the sediment sample, possible errors in the sample pretreatment and/or interference by other compounds/impurities were indicated. The concentrations of pentabromodiphenylether, BDE100, varied more than the other PBDE isomers due to its poor separation in some chromatographic conditions. In addition, interference by PBDEs was observed in the analysis for PBDFs. Potential degradation/secondary formulation of PBDEs and PBDFs during the Soxhlet extraction were suggested when copper powder was added into the sediment samples. Inspite of these observations, the results in this study are better than those reported in other interlaboratory studies due to the advice given to participants for improving the results. Compared with the results for PCDDs/DFs (5–23% RSDs) and Co-PCBs (6–24% RSDs), the RSDs for most of the organobromine compounds were high, indicating an immature QA/QC approach for the analysis of PBDEs and related compounds in comparison to common chlorinated dioxins.