This work investigates the hydrothermal synthesis and characterization of zeolite-4A from kaolin found in Ajebo, Nigeria calcined at 700 and 900°C respectively. The synthesized zeolite-4A was further characterised using X-ray Fluorescence (XRF), Fourier Transform Infrared spectrometer (FTIR), Scanning Electron Microscopy (SEM), X-Ray diffraction (XRD), Brunauer-Emmet-Teller (BET) surface area analysis as well as Differential Thermal Analysis/Thermo-gravimetric (TG). Water adsorption capacity tests were also carried out on the synthesized zeolite-4A. The results from the XRF measurements indicated that the amount of Al₂O₃ and SiO₂ in the studied kaolin was similar to the standard kaolin composition making it a perfect candidate for zeolite-4A synthesis. FTIR showed the characteristic zeolite peaks while XRD confirmed the crystalline nature of the synthesized zeolite-4A. TG studies showed that the zeolite-4A samples were stable up to temperatures of 700°C. This stability as well as the surface area and pore size of 7 Ä makes it potentially suitable for use in water treatment applications. The SEM showed cubic crystals which were typical of the morphology of zeolite-4A with water adsorption capacity of approximately 29%. These results indicate that zeolite- 4A can be synthesized from kaolin found in Ajebo as an inexpensive alternative to traditionally sourced materials and also is suitable for use as adsorption agent.