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    An evaluation of microwave-assisted fusion and microwave-assisted acid digestion methods for determining elemental impurities in carbon nanostructures using inductively coupled plasma optical emission spectrometry

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    Type
    Article
    Authors
    Patole, Shashikant P. cc
    Simões, Filipa
    Yapici, Tahir
    Warsama, Bashir H.
    Anjum, Dalaver H. cc
    Da Costa, Pedro M. F. J. cc
    KAUST Department
    Analytical Chemistry Core Lab
    Electron Microscopy
    Imaging and Characterization Core Lab
    Inorganics
    Material Science and Engineering Program
    Physical Science and Engineering (PSE) Division
    Date
    2015-10-25
    Online Publication Date
    2015-10-25
    Print Publication Date
    2016-02
    Permanent link to this record
    http://hdl.handle.net/10754/581093
    
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    Abstract
    It is common for as-prepared carbon nanotube (CNT) and graphene samples to contain remnants of the transition metals used to catalyze their growth; contamination may also leave other trace elemental impurities in the samples. Although a full quantification of impurities in as-prepared samples of carbon nanostructures is difficult, particularly when trace elements are intercalated or encapsulated within a protective layer of graphitic carbon, reliable information is essential for reasons such as quantifying the adulteration of physico-chemical properties of the materials and for evaluating environmental issues. Here, we introduce a microwave-based fusion method to degrade single- and double-walled CNTs and graphene nanoplatelets into a fusion flux thereby thoroughly leaching all metallic impurities. Subsequent dissolution of the fusion product in diluted hydrochloric and nitric acid allowed us to identify their trace elemental impurities using inductively coupled plasma optical emission spectrometry. Comparisons of the results from the proposed microwave-assisted fusion method against those of a more classical microwave-assisted acid digestion approach suggest complementarity between the two that ultimately could lead to a more reliable and less costly determination of trace elemental impurities in carbon nanostructured materials. Graphical abstract A method for the complete digestion of carbon nanostructures has been demonstrated. Photographs (on the left side) show zirconium crucibles containing SWCNTs with flux of Na2CO3 and K2CO3, before and after microwave fusion; (on the right side) the appearance of the final solutions containing dissolved samples, from microwave-assisted fusion and microwave-assisted acid digestion. These solutions were used for determining the trace elemental impurities by ICP‒OES.
    Citation
    An evaluation of microwave-assisted fusion and microwave-assisted acid digestion methods for determining elemental impurities in carbon nanostructures using inductively coupled plasma optical emission spectrometry 2015 Talanta
    Publisher
    Elsevier BV
    Journal
    Talanta
    DOI
    10.1016/j.talanta.2015.10.053
    PubMed ID
    26653428
    Additional Links
    http://linkinghub.elsevier.com/retrieve/pii/S0039914015304173
    ae974a485f413a2113503eed53cd6c53
    10.1016/j.talanta.2015.10.053
    Scopus Count
    Collections
    Articles; Analytical Chemistry Core Lab; Imaging and Characterization Core Lab; Physical Science and Engineering (PSE) Division; Material Science and Engineering Program

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