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Comparison of sample digestion techniques for the determination of trace and residual catalyst metal content in single-wall carbon nanotubes by inductively coupled plasma mass spectrometry

机译:电感耦合等离子体质谱法测定单壁碳纳米管中痕量和残留催化剂金属含量的样品消解技术比较

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摘要

A single-wall carbon nanotube material produced by laser ablation of renewable biochar in the presence of Ni and Co catalyst was characterized for residual catalyst (Co and Ni) as well as trace metal impurity content (Fe, Mo, Cr, Pb and Hg) by isotope dilution ICP-MS following sample digestion. Several matrix destruction procedures were evaluated, including a multi-step microwave-assisted acid digestion, dry ashing at 450 degrees C and microwave-induced combustion with oxygen. Results were benchmarked against those derived from neutron activation analysis and also supported by solid sampling continuum source GF-AAS for several of the elements. Although laborious to execute, the multi-step microwave-assisted acid digestion proved to be most reliable for recovery of the majority of the analytes, although content of Cr remained biased low for each approach, likely due to its presence as refractory carbide. (C) 2014 The Authors. Published by Elsevier B.V. All rights reserved.
机译:通过在Ni和Co催化剂存在下通过激光烧蚀可再生生物碳制得的单壁碳纳米管材料,对残余催化剂(Co和Ni)以及痕量金属杂质含量(Fe,Mo,Cr,Pb和Hg)进行了表征。样品消解后,通过同位素稀释ICP-MS进行分析。评估了几种基质破坏程序,包括多步微波辅助酸消化,450℃下的干灰化和微波诱导的氧气燃烧。将结果与中子活化分析得出的结果进行了基准比较,其中一些元素还得到了固体采样连续体源GF-AAS的支持。尽管执行起来很费力,但是多步微波辅助酸消解法对于大多数分析物的回收是最可靠的,尽管每种方法中Cr的含量仍然偏低,可能是由于其作为难熔碳化物的存在。 (C)2014作者。由Elsevier B.V.发布。保留所有权利。

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