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首页> 外文期刊>Analytical methods >Trace element determination in leather samples using on-line internal standardization, ultrasonic nebulization and axial view-ICP OES
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Trace element determination in leather samples using on-line internal standardization, ultrasonic nebulization and axial view-ICP OES

机译:使用在线内标,超声雾化和轴向观察ICP-OES测定皮革样品中的痕量元素

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摘要

A method has been developed to determine 15 elements in leather samples by ultrasonic nebulization axial view inductively coupled plasma optical emission spectrometry (USN-ICP OES) after calibration by on-line internal standardization (IS). Samples were ground in a lab blender and decomposed following a simple digestion protocol with nitric acid and hydrogen peroxide under microwave heating. Owing to the high chromium content in samples, judicious selection of analytical wavelengths was necessary, as well as the use of internal standardization on-line to compensate for matrix effects caused by sample loading on the nebulizer system and the ICP-source. Low-biased results were obtained by simple external calibration with aqueous standards. Unpredictable plasma-related matrix effects caused signal suppression that cannot be corrected by acid matrix-matched reinforcing of the major role of IS. Even though no reference material for leather samples is commercially available, two certified biological samples were used to estimate the accuracy (dogfish liver and bovine liver) of the proposed procedure. The experimental values achieved showed good agreement with the certified values only if IS was employed throughout. Spike and recovery experiments confirmed that the results of the proposed method were accurate. Fifteen elements were quantified in different leather samples, and indicated the presence of toxic elements, which were mainly Pb, Cd, Zn, V, Ni and Cr.
机译:在通过在线内部标准化(IS)进行校准之后,已经开发出一种方法,通过超声雾化轴向视图电感耦合等离子体发射光谱(USN-ICP OES)测定皮革样品中的15种元素。将样品在实验室混合器中研磨,并按照简单的消解方案在微波加热下用硝酸和过氧化氢分解。由于样品中的铬含量很高,因此有必要明智地选择分析波长,以及使用在线内部标准化来补偿由于样品加载到雾化器系统和ICP离子源上而引起的基质效应。通过使用水标准品进行简单的外部校准可获得低偏差的结果。不可预测的与血浆相关的基质效应导致信号抑制,而该抑制不能通过酸基质匹配增强IS的主要作用来纠正。即使没有用于皮革样品的参考材料,也可以使用两个认证的生物样品来评估所建议程序的准确性(dog鱼肝和牛肝)。仅在始终采用IS的情况下,获得的实验值才与认证值保持良好的一致性。峰值和恢复实验证实了该方法的结果是准确的。在不同的皮革样品中定量了15种元素,表明存在有毒元素,主要是Pb,Cd,Zn,V,Ni和Cr。

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