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Plasma-based determination of inorganic contaminants in waste of electric and electronic equipment after microwave-induced combustion

机译:基于等离子体的微波诱导燃烧后电气和电子设备废物中无机污染物的测定

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A systematic study was performed for the determination of inorganic contaminants in polymeric waste from electrical and electronic equipment (EEE) for achieving an efficient digestion to minimize interferences in determination using plasma-based techniques. The determination of As, Br, Cd, Co, Cr, Cu, Ni, Pb, Sb, and Zn by inductively coupled plasma mass spectrometry (ICP-MS) and also by inductively coupled plasma optical emission spectrometry (ICP DES) was carried out after digestion using microwave-induced combustion (MIC). Arsenic and Hg were determined by flow-injection chemical vapor generation inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). Dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) with ammonia was also used for Cr determination. The suitability of MIC for digestion of sample masses up to 400 mg was demonstrated using microcrystalline cellulose as aid for combustion of polymers from waste of EEEs that usually contain flame retardants that impair the combustion. The composition and concentration of acid solutions (HNO3 or HNO3 plus HCl) were evaluated for metals and metalloids and NH4OH solutions were investigated for Br absorption. Accuracy was evaluated by comparison of results with those obtained using high pressure microwave-assisted wet digestion (HP-MAWD) and also by the analysis of certified reference material (CRM) of polymer (EC680k-low-density polyethylene). Bromine determination was only feasible using digestion by MIC once losses were observed when HP-MAWD was used. Lower limits of detection were obtained for all analytes using MIC (from 0.005 mu g g(-1) for Co by ICP-MS up to 3.120 mu g g(-1) for Sb by ICP OES) in comparison to HP-MAWD due to the higher sample mass that can be digested (400 mg) and the use of diluted absorbing solutions. The combination of HNO3 and HCl for digestion showed to be crucial for quantitative recovery of some elements, as Cr and Sb. In addition, suitable agreement of Cr to CRM value was only obtained by mixing NH4Cl to samples before combustion. No statistical difference (95% confidence level) was observed between the results obtained for As, Cd, Co, Cr, Cu, Hg, Ni, Pb, Sb, and Zn by MIC and HP-MAWD methods. Agreement with certified values was better than 96% using MIC for all inorganic contaminants. Particularly for Br, MIC was the method of choice for digestion due to the possibility of using diluted alkaline solutions for analyte absorption. Based on the obtained results, MIC can be considered as a suitable method for digestion of polymers from waste of EEEs for further plasma based determination of inorganic contaminants. (C) 2014 Elsevier B.V. All rights reserved.
机译:进行了系统的研究,以确定电气和电子设备(EEE)聚合废料中的无机污染物,以实现有效的消化,从而最大程度地减少基于等离子体技术的测定干扰。通过电感耦合等离子体质谱法(ICP-MS)和电感耦合等离子体发射光谱法(ICP DES)进行As,Br,Cd,Co,Cr,Cu,Ni,Pb,Sb和Zn的测定使用微波诱导燃烧(MIC)消化后。砷和汞通过流动注射化学蒸气产生电感耦合等离子体质谱法(FI-CVG-ICP-MS)测定。含氨的动态反应池电感耦合等离子体质谱(DRC-ICP-MS)也用于测定Cr。使用微晶纤维素作为助燃剂,可以将EEE废料中的聚合物燃烧,这种MIC适于消化高达400 mg的样品,证明这些物质通常含有会阻碍燃烧的阻燃剂。评估了酸性溶液(HNO3或HNO3加HCl)的金属和准金属的成分和浓度,并研究了NH4OH溶液对Br的吸收。通过将结果与使用高压微波辅助湿消化(HP-MAWD)的结果进行比较,并通过对聚合物(EC680k-低密度聚乙烯)的认证参考材料(CRM)进行分析,来评估准确性。一旦使用HP-MAWD观察到损失,溴的测定只有通过MIC消解才可行。与HP-MAWD相比,使用MIC的所有分析物的检测下限均较HP-MAWD低(通过ICP-MS从Co的0.005 mu gg(-1)到通过ICP OES的Sb的3.120 mu gg(-1))。可以消化的样品质量更高(400 mg),并使用稀释的吸收溶液。 HNO3和HCl的消化组合对于某些元素(如Cr和Sb)的定量回收至关重要。另外,只有通过在燃烧前将NH4Cl混合到样品中,才能使Cr与CRM值达到合适的一致性。通过MIC和HP-MAWD方法获得的As,Cd,Co,Cr,Cu,Hg,Ni,Pb,Sb和Zn的结果之间未观察到统计学差异(95%置信度)。对于所有无机污染物,使用MIC的认证值均优于96%。特别是对于Br,由于可以使用稀释的碱性溶液吸收分析物,因此MIC是消解的首选方法。基于获得的结果,MIC可被认为是从EEE废料中消化聚合物以进一步基于等离子体测定无机污染物的合适方法。 (C)2014 Elsevier B.V.保留所有权利。

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