Adsorption behaviour of tri-n-butyl phosphate (TBP) from aqueous solution (dilute HN03) on Amberlite XAD-4 has been investigated experimentally. Factors affecting the adsorption rates and breakthrough curves have been studied in batchwise and semicontinuous fixed bed adsorber. The adsorption isotherm of TBP on Amberlite XAD-4 resin have also been determined and the Freundlich model of adsorption is used to describe adsorption equilibrium. For the case of nonlinear equilibrium a simplified method proposed by Chi Tein is used to estimate intraparticle diffusion coefficient. The intraparticle diffusion coefficient is found to be in the range of 10-8cmZ~s-'. Results of fixed bed column are used to estimate mass transfer zone (MTZ) length, length of unused bed (LUB), breakthrough capacity corresponding to fixed value of effluent concentration (5 mg/l of TBP) and degree of saturation of bed at breakthrough. The MTZ length was found to vary from 21.8 cm to 37.3cm when flow rate changed from 13.5 mllmin to 52 mllmin, whereas column utilization ranged from 65.1% for the lowest flow rate to 43.5% for the highest flow rate.