The study focused on the effect of process parameters on the single adsorption of Zinc and Nickel ions using activated carbon from waste Nigerian bamboo.nbsp The bamboo was cut into sizes, washed,nbsp dried and carbonized at 300oC-500oC. The carbonized bamboo was then activated at 800oC using nitric acid.nbsp The effect of process parameters such as particle size, carbon dosage, initial concentration of adsorbate on the single adsorption of Zinc and Nickel ions in aqueous solution was also investigated and were found to significantly affect the adsorption capacity of Zinc and Nickelnbsp ions in solution using activated carbon from waste Nigerian bamboo. For optimum adsorption of Zinc and Nickel ions in solution, particle size of Nigerian bamboo activated carbon less than 150 mm should be used for batch operations. The amount of Nickel ions adsorbed at equilibrium within initial adsorbate concentration of 28mg/L - 223mg/L was 28mg/g - 170mg/g, while The amount of Zinc ions adsorbed at equilibrium within initial concentration of 28mg/L - 227mg/L was 26mg/g - 185mg/gnbsp for carbon dosage of 10g/L .nbsp The results obtained showed that Nigerian Bamboo is highly effective in the single adsorption of Zinc and Nickel ions in solution