title: Elemental Quantification and Residues Characterization of Wet Digested Certified and Commercial Carbon Materials.
abstract: Inductively coupled plasma optical emission spectroscopy (ICP-OES) is a common, relatively low cost, and straightforward analytical technique for the study of trace quantities of metals in solid materials, but its applicability to nanocarbons (e.g., graphene and nanotubes) has suffered from the lack of efficient digestion steps and certified reference materials (CRM). Here, various commercial and certified graphitic carbon materials were subjected to a "two-step" microwave-assisted acid digestion procedure, and the concentrations of up to 18 elements were analyzed by ICP-OES. With one exception (Sm), successful quantification of all certified elements in the two reference nanocarbons studied was achieved, hence validating the sample preparation approach used. The applicability of our "two-step" protocol was further confirmed for a commercial single-walled carbon nanotube sample. However, the digestion was markedly incomplete for all other commercial materials tested. Where possible, the digestion residues of the carbon materials analyzed (CRM included) were characterized to understand the structural changes that take place and how this may explain the challenge of disintegrating graphitic carbon. In this respect, it was found that solid state nuclear magnetic resonance holds considerable promise as a nonlocalized, easily interpretable, and reliable tool to access the efficient disintegration of these materials.
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Filipa R F
authors: FR
authors: Simoes
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Nitin M
authors: NM
authors: Batra
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Bashir H
authors: BH
authors: Warsama
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Christian G
authors: CG
authors: Canlas
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Shashikant
authors: S
authors: Patole
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Tahir F
authors: TF
authors: Yapici
authors: Physical Science and Engineering Division, ‡Analytical Core Laboratory, and §Imaging and Characterization Laboratory, King Abdullah University of Science and Technology (KAUST) , Thuwal 23955-6900, Saudi Arabia.
authors: Pedro M F J
authors: PM
authors: Costa