Activated coal fly ash (FA) treated with NaOH and hexadecyltrimethylammonium bromide (HDTMABr) was used as adsorbent for removal of cadmium(II) ions and rhodamine B (RB) from an aqueous solution. Characterization of fly ash and FA-HDTMABr were done using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and X-ray diffraction (XRD). The sorption equilibrium in the system were analysed using isotherm models, such as Freundlich, Langmuir, generalized Langmiur-Freundlich, Redlich-Peterson, Jovanović, extended Jovanović, Tóth, Fumkin-Fowler-Guggenheim, Fowler-Guggenheim-Jovanović-Freundlich, Temkin, Dubinin-Radushkevich, Halsey, Brunauer, Emmett and Teller. The evaluation of the fit of the isotherms studied experimentally was carried out by means of the reduced chi-square test and the coefficient of determination. The maximum monolayer adsorption capacity of the FA-HDTMABr was found to be 744 mg·g−1 and 666 mg·g−1 for Cd(II) and RB, respectively. The PFO, PSO, Elovich mass transfer, liquid film diffusion and intra-particle diffusion models were analysed. Sorption kinetics data were well fitted by the PSO model. The Elovich and intra-particle model also revealed that there are two separate stages in the sorption process, namely, external diffusion and inter-particle diffusion.