This work explores the synthesis and characterization of two novel nanocomposites that can be used in various applications, such as aqueous solution adsorption of pollutants. The first nanocomposite consists of tin (Sn)-doped titanium dioxide (TiO2) on activated carbon, while the other one consists of polypyrole (PPy), chitosan (CS), and Sn-doped TiO2. A contrast was made of their effective adsorbent materials for the removal of Cibacron Brilliant Yellow dye from aqueous solutions. Different analytical techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray analysis (EDX), and Fourier transform - infrared (FT-IR) were used to analysis the nanocomposite samples. SEM images show that the average particle diameter of PPy-CS/Sn-doped TiO2 NC is 75 ± 3 nm, while Sn-doped TiO2/AC particles have an average diameter of 40 ± 2 nm. The greater PPy-CS/Sn-doped TiO2 nanocoposite particle diameter indicates that the polymers cover the Sn-doped TiO2 nanoparticles, which leads to higher in the diameter of the particles. The adsorption efficiency of Sn-doped TiO2/AC was higher than that of PPy-CS/Sn-doped TiO2 sample due to its smaller particle size which resulted in a higher surface area which provides more adsorption sites. However, both samples showed remarkable adsorption capacity, where the adsorption capacity of Sn-doped TiO2/AC and PPy-CS/Sn-doped TiO2 were 104 and 103 mg/g, respectively.