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Determination of elemental impurities in poly(vinyl chloride) by inductively coupled plasma optical emission spectrometry

机译:电感耦合等离子体发射光谱法测定聚氯乙烯中的元素杂质

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In this work, a method for poly(vinyl chloride) (PVC) analysis by inductively coupled plasma optical emission spectrometry (ICP-OES) was developed. Samples were digested by microwave-induced combustion (MIC) and thirteen elements (Ba, Cd, Co, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sr, V and Zn) were determined by ICP-OES. Operational conditions of MIC were investigated allowing quantitative determination of all the analytes and suitable results were achieved using a 3 mol L-1 HNO3 solution. Microwave-assisted wet digestion (MAWD) using closed quartz vessels and a single reaction chamber microwave digestion system (MAWD-SRC), were also evaluated for PVC digestion for results comparison. All the evaluated sample preparation methods were considered suitable for PVC digestion but MIC was preferable due to the possibility of using diluted HNO3 instead of concentrated reagents and due to the better digestion efficiency. The residual carbon content (RCC) in digests obtained by MIC was significantly lower in comparison with the values obtained after MAWD and by MAWD-SRC. Accuracy for the proposed method was better than 94% for all analytes by comparison of results with those obtained by neutron activation analysis (NAA). Using MIC, it was possible to digest a relatively high sample mass (500 mg) and up to 8 samples in less time (25 min) in comparison with MAWD and MAWD-SRC (about 60 min for both methods). The efficiency of digestion by MIC was higher 99% and lower limits of detection (as low as 0.1 mu g g(-1)) were obtained avoiding the use of concentrated acids that is of great concern according to the current green chemistry recommendations. (C) 2016 Elsevier B.V. All rights reserved.
机译:在这项工作中,开发了一种通过电感耦合等离子体发射光谱法(ICP-OES)分析聚氯乙烯(PVC)的方法。通过微波诱导燃烧(MIC)消解样品,并通过ICP-OES测定13种元素(Ba,Cd,Co,Cu,Fe,Mg,Mn,Mo,Ni,Pb,Sr,V和Zn)。研究了MIC的操作条件,可以定量测定所有分析物,并使用3 mol L-1 HNO3溶液获得了合适的结果。还评估了使用密闭石英容器和单个反应室微波消解系统(MAWD-SRC)进行的微波辅助湿消解(MAWD)的PVC消解,以进行结果比较。所有评估的样品制备方法均被认为适用于PVC消化,但由于使用稀释的HNO3代替浓缩试剂的可能性以及更好的消化效率,MIC是优选的。与通过MAWD和通过MAWD-SRC获得的值相比,通过MIC获得的消化物中的残余碳含量(RCC)明显较低。通过将结果与通过中子活化分析(NAA)获得的结果进行比较,该方法对所有分析物的准确性均优于94%。与MAWD和MAWD-SRC(两种方法约60分钟)相比,使用MIC可以在较短的时间(25分钟)内消化相对较高的样品质量(500 mg)和最多8个样品。 MIC的消化效率高达99%,并且检出限较低(低至0.1μg(-1)),从而避免了根据当前绿色化学建议而引起关注的浓酸的使用。 (C)2016 Elsevier B.V.保留所有权利。

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