The physicochemical investigations on the associative, micellar and thermodynamic properties of a diblock (PEO) 62 -b-(PBO) 33 copolymer in aqueous medium and its interaction with ionic surfactants were carried out by using surface tensiometry, laser light scattering and steady-state fluorescence spectroscopy. Surface tension and fluorescence measurements were used to find out the critical micelle concentration (CMC) and related thermodynamic parameters of micellization copolymer at various temperatures. The data from dynamic light scattering (DLS) was helpful to obtain the values of hydrodynamic radii (R h ), volume ( h ) and hydrodynamic expansion parameter ( h ) of the copolymer micelle. Likewise, the measurements from static light scattering (SLS) were employed to determine weight-average molar (M w ), association number (N w ), thermodynamic radius (R t ), thermodynamic volume ( t ), anhydrous volume ( a ) and thermodynamic expansion parameter ( t ) of the copolymer micelles in the temperature range of 20-50 o C. Similarly, the interactions between (PEO) 62 -b-(PBO) 33 and two ionic surfactants, sodium dodecyl sulphate (SDS) and hexadecyltrimethylammonium bromide (CTAB), have also been investigated by fluorescence spectroscopy and DLS at 30 o C. Downloaded by [FU Berlin] at 05:19 07 July 2015 2Similarly, the interactions between (PEO) 62 -b-(PBO) 33 and two ionic surfactants, sodium dodecyl sulfate (SDS) and hexadecyl trimethylammonium bromide (CTAB), have also been investigated by fluorescence spectroscopy and DLS in detail.Graphical Abstract: