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

Handle URI:
http://hdl.handle.net/10754/581093
Title:
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
Authors:
Patole, Shashikant P. ( 0000-0001-6669-6635 ) ; Simões, Filipa; Yapici, Tahir; Warsama, Bashir H.; Anjum, Dalaver H.; Da Costa, Pedro M. F. J. ( 0000-0002-1993-6701 )
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.
KAUST Department:
Physical Sciences and Engineering (PSE) Division; Analytical Core Lab; Imaging and Characterization Core Lab
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
Issue Date:
21-Oct-2015
DOI:
10.1016/j.talanta.2015.10.053
Type:
Article
ISSN:
00399140
Additional Links:
http://linkinghub.elsevier.com/retrieve/pii/S0039914015304173
Appears in Collections:
Articles; Analytical Core Lab; Advanced Nanofabrication, Imaging and Characterization Core Lab; Physical Sciences and Engineering (PSE) Division

Full metadata record

DC FieldValue Language
dc.contributor.authorPatole, Shashikant P.en
dc.contributor.authorSimões, Filipaen
dc.contributor.authorYapici, Tahiren
dc.contributor.authorWarsama, Bashir H.en
dc.contributor.authorAnjum, Dalaver H.en
dc.contributor.authorDa Costa, Pedro M. F. J.en
dc.date.accessioned2015-10-26T11:04:16Zen
dc.date.available2015-10-26T11:04:16Zen
dc.date.issued2015-10-21en
dc.identifier.citationAn 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 Talantaen
dc.identifier.issn00399140en
dc.identifier.doi10.1016/j.talanta.2015.10.053en
dc.identifier.urihttp://hdl.handle.net/10754/581093en
dc.description.abstractIt 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.en
dc.language.isoenen
dc.publisherElsevier BVen
dc.relation.urlhttp://linkinghub.elsevier.com/retrieve/pii/S0039914015304173en
dc.rightsNOTICE: this is the author’s version of a work that was accepted for publication in Talanta. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Talanta, 21 October 2015. DOI: 10.1016/j.talanta.2015.10.053en
dc.subjectMetrologyen
dc.subjectCarbon nanotubesen
dc.subjectGraphene nanoplateletsen
dc.subjectMicrowave-assisted acid digestionen
dc.subjectMicrowave-assisted fusionen
dc.subjectInductively coupled plasma optical emission spectrometryen
dc.titleAn evaluation of microwave-assisted fusion and microwave-assisted acid digestion methods for determining elemental impurities in carbon nanostructures using inductively coupled plasma optical emission spectrometryen
dc.typeArticleen
dc.contributor.departmentPhysical Sciences and Engineering (PSE) Divisionen
dc.contributor.departmentAnalytical Core Laben
dc.contributor.departmentImaging and Characterization Core Laben
dc.identifier.journalTalantaen
dc.eprint.versionPost-printen
dc.contributor.affiliationKing Abdullah University of Science and Technology (KAUST)en
kaust.authorPatole, Shashikant P.en
kaust.authorSimões, Filipaen
kaust.authorYapici, Tahiren
kaust.authorWarsama, Bashir H.en
kaust.authorAnjum, Dalaver H.en
kaust.authorDa Costa, Pedro M. F. J.en
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