Quantifying the Epoxide Group and Epoxide Index in Graphene Oxide by Catalyst-Assisted Acid Titration

Graphene oxide (GO), having diverse oxygen functional groups, including carboxyl, hydroxyl, carbonyl, and epoxy groups, is a significant graphene-related 2D material (GR2M) essential for various applications. The quantification of these functional groups traditionally utilizes Boehm acid titration, which, however, does not account for epoxy groups crucial for these applications. Presently, there exists no analytical method enabling quantitative assessment of the concentration of epoxy groups in GO available in the market in different forms such as powders, pastes, and dispersions. This paper presents a new approach employing catalyst-assisted acid-water-based titration to quantify epoxy groups in GO materials. The method's efficacy was validated using a well-characterized reference GO sample and tested on commercially produced GO powders, yielding epoxy group concentrations ranging from 1.15 ± 0.047 to 1.37 ± 0.051 mmol/g with high precision and reproducibility. The method introduces two new quality parameters, including the epoxide index (EI) and the equivalent epoxide weight (EEW) not implemented for GO before. Control measurements with a commercial epoxide material of known epoxide content demonstrated excellent agreement by using the proposed approach. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were used for comparative characterizations of epoxide groups in GO samples during titrations.