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      Determination of Metallic Impurities in Carbon Nanotubes by Glow Discharge Mass Spectrometry

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      ACS Omega
      American Chemical Society

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          Abstract

          A method for the rapid assessment of metallic impurities in carbon nanotubes (CNTs) by pin-cell source geometry glow discharge mass spectrometry (GDMS) is presented. Pins were prepared by pressing CNT powder onto an indium substrate. GDMS analysis was performed using high-carbon-content nanotube and coal-certified reference materials for calibration purposes. This approach enables the calibrated measurement of 41 elemental impurities in CNTs. The method was validated by the analysis of NIST SRM 2483 single-wall CNTs (raw soot) with good agreement with the certified values. The proposed measurement approach could also be applied not only for CNTs but also for the assessment of precursor materials used in the synthesis of CNTs and for quality control during the entire manufacturing process. The ability to assess the presence of all metallic impurities in a simple, reliable, high-throughput manner will allow the industry to real-time monitor any changes in the product process, access its toxicity, and environmental impact. As sample preparation is maintained to a minimum, this allows the determination of metallic impurities at concentration levels that are usually not attainable by most techniques.

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          Most cited references44

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          Helical microtubules of graphitic carbon

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            A green approach to the synthesis of graphene nanosheets.

            Graphene can be viewed as an individual atomic plane extracted from graphite, as unrolled single-walled carbon nanotube or as an extended flat fullerene molecule. In this paper, a facile approach to the synthesis of high quality graphene nanosheets in large scale through electrochemical reduction of exfoliated graphite oxide precursor at cathodic potentials (completely reduced potential: -1.5 V) is reported. This method is green and fast, and will not result in contamination of the reduced material. The electrochemically reduced graphene nanosheets have been carefully characterized by spectroscopic and electrochemical techniques in comparison to the chemically reduced graphene-based product. Particularly, FTIR spectra indicate that a variety of the oxygen-containing functional groups have been thoroughly removed from the graphite oxide plane via electrochemical reduction. The chemically converted materials are not expected to exhibit graphene's electronic properties because of residual defects. Indeed, the high quality graphene accelerates the electron transfer rate in dopamine electrochemistry (DeltaE(p) is as small as 44 mV which is much smaller than that on a glassy carbon electrode). This approach opens up the possibility for assembling graphene biocomposites for electrocatalysis and the construction of biosensors.
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              Gram-scale production of graphene based on solvothermal synthesis and sonication.

              Carbon nanostructures have emerged as likely candidates for a wide range of applications, driving research into novel synthetic techniques to produce nanotubes, graphene and other carbon-based materials. Single sheets of pristine graphene have been isolated from bulk graphite in small amounts by micromechanical cleavage, and larger amounts of chemically modified graphene sheets have been produced by a number of approaches. Both of these techniques make use of highly oriented pyrolitic graphite as a starting material and involve labour-intensive preparations. Here, we report the direct chemical synthesis of carbon nanosheets in gram-scale quantities in a bottom-up approach based on the common laboratory reagents ethanol and sodium, which are reacted to give an intermediate solid that is then pyrolized, yielding a fused array of graphene sheets that are dispersed by mild sonication. The ability to produce bulk graphene samples from non-graphitic precursors with a scalable, low-cost approach should take us a step closer to real-world applications of graphene.
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                Author and article information

                Journal
                ACS Omega
                ACS Omega
                ao
                acsodf
                ACS Omega
                American Chemical Society
                2470-1343
                25 August 2021
                07 September 2021
                : 6
                : 35
                : 22717-22725
                Affiliations
                Metrology, National Research Council Canada , Ottawa, Ontario K1A 0R6, Canada
                Author notes
                Author information
                https://orcid.org/0000-0002-1167-6474
                https://orcid.org/0000-0002-2377-2615
                Article
                10.1021/acsomega.1c03013
                8427626
                89a26bd5-1198-42a6-9acb-5e7f63829d71
                Crown © 2021. Published by American Chemical Society

                Permits non-commercial access and re-use, provided that author attribution and integrity are maintained; but does not permit creation of adaptations or other derivative works ( https://creativecommons.org/licenses/by-nc-nd/4.0/).

                History
                : 08 June 2021
                : 06 August 2021
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                ao1c03013

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