Yap, P L; Farivar, F; Jämting, Å K; Coleman, V A; Gnaniah, S; Mansfield, E; Pu, C; Landi, S M; David, M V; Flahaut, E; Aizane, M; Barnes, M; Gallerneault, M; Locatelli, M D; Jacquinot, S; Slough, C G; Menzel, J; Schmölzer, S; Ren, L; Pollard, A J; Losic, D (2023) International Interlaboratory Comparison of Thermogravimetric Analysis of Graphene-Related Two-Dimensional Materials. Analytical Chemistry, 95 (12). pp. 5176-5186. ISSN 0003-2700

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Abstract

Graphene related 2D materials (GR2Ms) are transitioning from academic research labs into industrial sectors with many developed products now on the market. Characterization of the GR2M properties and their quality control are critical, with a need for analytical methods for reliable, reproducible, and accurate measurements. To facilitate industrial growth using GR2Ms, several measurement standards are either published or under development within the ISO 229 and IEC 113 standardization committees. Towards this effort, this work presents the results of an international interlaboratory comparison (ILC), conducted under Versailles Project on Advanced Materials and Standards (VAMAS) Technical Working Area (TWA) 41 “Graphene and Related 2D Materials” to quantitatively assess the interlaboratory performance (reproducibility and confidence) of thermogravimetric analysis (TGA) as a reliable method to characterize key thermal properties and qualitative and quantitative analytical parameters of GR2Ms. “Real-life” commercially-available samples of a relevant range of GR2Ms, such as pristine few-layer graphene (FLG), graphene oxide (GO) and reduced graphene oxide (rGO) were used for this study. The method performance was evaluated by series of TGA measurements of selected parameters including the determination of GR2M physical properties (thermal stability and the peak or maximum temperature (Tp) for each decomposition step), the qualitative (number of mass loss steps) and the quantitative compositional analysis (moisture, residue, carbon and oxygen elements in graphene). TGA measurements were performed using a provided measurement protocol, and the same types (3) of GR2M samples by 12 participants across academia, industry (including instrument manufacturers), and national metrology institutes. The collected and processed data of TGA measurements were compared to evaluate their statistical performance using the distribution of the Mandel's k (within participants’ consistency) and h (between participants’ consistency) values. The obtained results and performance statistics from this work confirmed the suitability of TGA to be used as a reliable analytical method for characterization and quality control of GR2Ms.

Item Type:	Article
Keywords:	TGA, VAMAS, Graphene
Subjects:	Advanced Materials > Thermal Analysis of Materials
Divisions:	Materials and Mechanical Metrology
Identification number/DOI:	10.1021/acs.analchem.2c03575
Last Modified:	03 Sep 2026 14:50
URI:	https://eprintspublications.npl.co.uk/id/eprint/10504