X-rayphotoelectronspectroscopy(XPS)wasadoptedtoelucidatesorptionmechanismofphenolandp-nitrophenolontoaweaklyanionexchangerD301.ThedistributionofspecificformsoftertiaryaminogrouponD301wasobtainedandeffectoffreetertiaryaminogrouponphenolsorptionontoD301wasdiscussed.TheresultindicatedthatthepercentoftheprotonatedtertiaryaminegrouponpolymericmatrixwasmuchlowerthanthereferencecompoundN,N-dimethylbenzylamineatanidenticalpHvalueinsolutionduetothemuchloweractivitydegreeofhydrogenionininnerresinphasethanintheexternalsolution.LessfreeaminogrouponD301resultsinlesssorptioncapacityofphenolandp-nitrophenolinanacidicsolution.UndertheexperimentalconditionsbothphenolsorptionontoD301canbeexplainedassolidextractionandthedistributioncoefficientvarieslinearlywiththecontentoffreeaminogrouponD301.