An investigation of morphology w.r.t. Fourier transform infrared spectroscopy (FT-IR), energy dispersive Xray fluorescence (EDXRF), scanning electron microscope (SEM), Mössbauer spectra (MS), X- ray diffraction (XRD) study based on resin column experiment has been performed for ascertaining breakthrough point in a resin loaded column for metal ions present in front stage generated nuclear effluent. Effect of chelation (FT-IR study) of different elements such as Cu(II), Sr(II), Gd(III), U(VI) on polyhydroxamate resin leads to prominent colouration (green for Cu), upper layer deposition (Sr), or loosely bound Gd or strongly bound U or Fe (Mössbauer and XRD studies) onto resin has been investigated during passing of Rad-effluents. In this regard, metal ions were analysed by inductively coupled plasma mass spectroscopy (ICP-AES) and confirmed by EDXRF. A vertical glass column chromatography with resin bed diameter 38 mm and height 350 mm produced the “S” shape break through curve. The high capacity of resin was attributed to corrugate and symmetrically folded tunnelled structure derived from SEM.