Reliable characterization and quality control of manufactured graphene-related 2D materials are essential for defining structure–property relationships and enabling their broader industrial adoption. However, the robust identification and quantification of chemical functional groups in functionalized graphene remain significant analytical challenges. Conventional spectroscopic techniques, including Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and energy-dispersive X-ray spectroscopy (EDX), primarily provide qualitative or elemental information and generally lack the sensitivity and quantitative capability required for metrologically robust assessment of functionalization. Here, we systematically evaluate thermogravimetric analysis (TGA) as a complementary analytical method for probing chemical functional groups in functionalized graphene materials. A series of graphene samples functionalized with oxygen-, sulfur-, and nitrogen-containing groups was investigated, revealing distinct and reproducible mass-loss profiles associated with the thermal decomposition and oxidation of specific functional moieties bound to the graphene framework. Correlation of these thermal signatures with comprehensive structural and chemical characterization enables the assignment, differentiation, and quantification of functional groups with improved reliability. This TGA-based approach offers a cost-effective, scalable, and high-throughput pathway toward quantitative functional group analysis, supporting improved comparability, quality control, and standardization of graphene materials. The methodology provides new insights into graphene functionalization and supports its deployment in biomedical, energy storage, catalysis, sensors, coatings, and nanocomposite applications.
Yap et al. (Thu,) studied this question.