Dimethyldichlorosilane (DMDCS) driven silane coupling is enabled by productive immobilization of an azo-dye to inorganic carrier through m-nitro aniline as a bridging component. The material has been utilized for the selective sample cleanup of zinc(II), cadmium(II), and mercury(II), respectively, extracted as [Zn-5(OH)(6)(H2O)(2)](4+), [Cd-4(OH)(4)(H2O)(3)](4+), and [Hg-4(OH)(3)(H2O)(2)](5+). The corresponding luminescent nanomaterial was used for selective detection of mercury(II) at trace level (LOD >= 0.04 X 10(-5) M) amid a matrix of possible interferences. Breakthrough capacity (BTC) and preconcentration factor (PF) for the respective metal ions (BTCZinc(II), 600; BTCCadmium(II), 460; BTCMercury(II), 540 mu M g(-1); and PFZinc(II), 197; PFCadmium(II), 148; PFMercury(II), 145) were found to be excellent. Sequential separation of zinc(II), cadmium(II), and mercury(II) was achieved by employing selective eluents (mineral acids of very low concentration, 5 X 10(3) mu M). BTC (530 +/- 70 mu M g(-1)) was found to be the product of the amount of extractor frontier orbitals (132 mu M g(-1)) and polynuclear state of sorbed species, x (i.e., BTC = {amount of HOMO}x x; x = 4 for cadmium(II), mercury(II); and x = 5 for zinc(II)). Along with these analytical qualities, ease of synthesis, high level of reusability (<= 2700 cycles @ 95% exchange capacity), and chemical stability (post treatment BTC with 8 M HNO3, 8 M HCI, and 5 M H2SO4 was <= 95%) is an insignia of the material.