The functionalization of pristine CNTs is necessary for carbon nanotubes (CNTs) to be fully utilized, with the aim of increasing the nanotube reactivity and solubility in aqueous solutions. In this study, multi-walled carbon nanotubes (MWCNTs) were functionalized with a carboxylic group as this was an important step prior to application. The carboxylic group-functionalization was conducted through acid treatment, using sulphuric and nitric acids mixed at a ratio of 3:1 (v/v) and sonication for 30 min under different temperatures and time durations. The functionalization conditions of 50ºC x 5 h and 60ºC x 3 h were identified to be most suitable for introducing a carboxylic group onto the nanotube surfaces. The percentage of total weight loss due to the carboxylic group on the MWCNTs treated at 50ºC x 5 h and 60ºC x 3 h obtained from the thermogravimetric analysis was 13.26% and 13.76%, respectively. For both samples, peaks corresponding to the carboxylic group were identified in the FT-IR spectra. The changes in the morphology of the treated MWCNTs were also observed under SEM analysis.