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Synthesis, characterization and intercalation of Zeolite A from Nigerian Ahoko kaolin for adsorption studies of Methylene blue (MB)were studied. The Zeolite A was synthesized from Nigerian Ahoko kaolin (NAK) using hydrothermal technique and was intercalated by hexamethyltetraamine (HMTA). The synthesized zeolite A (SZA) and intercalated zeolite A (IZA) were characterized using X- Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Braunauer Emmet Teller (BET) and Fourier Transform Infrared spectroscopy (FT-IR) analyses.The XRD reveal zeolite A peaks including several peaks depicting presence of minerals like quartz, mica, calcium and iron.The surface area of SZA and IZA were found to be 21.11m2/g and 21.47m2/g, respectively based on BET analysis. The effects of initial concentration, adsorbent dosage, pH and temperature with contact time were studied for SZA and IZA to examine their performance as an adsorbent. The adsorption rates increased with increase pH,temperature, initial concentration and adsorbent dosage for both SZA & IZA. The intercalation also positively increases the adsorption capacity of the parent material.