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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry
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Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

机译:固体进样高分辨率连续谱源石墨炉原子吸收光谱法同时测定含氟聚合物中的铁和镍

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摘要

This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003 nm) and the adjacent secondary line of iron (232.036 nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H-2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300 degrees C, respectively, using only 0.5 L min(-1) H-2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6 ng g(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4 mu g g(-1) for iron and from 37 to 78 ng g(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave induced combustion and no significant statistical difference was observed. (C) 2016 Elsevier B.V. All rights reserved.
机译:本文报道了一种通过直接固体采样的高分辨率连续谱源石墨炉原子吸收光谱法(HR-CS GF AAS)同时测定含氟聚合物中铁和镍的方法的开发。为了同时进行测量,在同一光谱窗口中同时监测了镍的主共振线(232.003 nm)和相邻的铁的次要线(232.036 nm)。所提出的方法用全氟烷氧基(PFA)样品进行了优化,并用于测定氟化乙烯丙烯(FEP)和改性聚四氟乙烯(PTFE-TFM)样品中的铁和镍。仔细研究了热解和雾化温度,以及使用Pd和H-2(在热解过程中)作为化学改性剂。在热解过程中仅使用0.5 L min(-1)H-2作为化学改性剂,两种分析物的热解和雾化的折衷温度分别达到800和2300摄氏度。通过使用包含两种分析物的单一溶液,使用水性标准液进行校准曲线。铁和镍的检出限分别为221和9.6 ng g(-1)。所有样品中的分析物浓度,铁的范围为3.53至12.4μg g(-1),镍的范围为37至78 ng g(-1),相对标准偏差小于19%。通过将这些结果与通过微波诱导的燃烧消解样品后通过电感耦合等离子体质谱法获得的结果进行比较来评估准确性,并且未观察到明显的统计学差异。 (C)2016 Elsevier B.V.保留所有权利。

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