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The project covers the preparation and characterization of new series of macrocycle compounds derived from phosphinic acid namely, bis-[1,5-diphenylcarbazide-dimethyl phosphinic acid], bis-[1,5-diphenylthiocarbazide-dimethyl phosphinic acid] and bis-[1,6-diphenyl-oxaloyldihaydrazine dimethyl phosphinic acid. These compounds were prepared from the reaction of paraformaldehyde, phosphinic acid with(1,5-diphenylcarbazide),(1,5-diphenylthiocarbazide) and (1,6-diphenyloxoloyldihydrazine) respectively, at the reflux temperature in presence of 6N HCl. The prepared compounds were characterized by elemental microanalysis, melting point, FTIR, 1H, 13C, 31P, 2D 1H-1H, NMR, and Mass spectroscopy. The prepared compounds were used for adsorption from solution of phenol, p-chlorophenol, copper (II), and nickel (II) at different conditions of temperature and ionic strengths. Shapes of the isotherms obtained from the adsorption studies of phenol, p-chlorophenol, copper (II), and nickel (II) on surfaces of these compounds were found to be combatable to the Freundlich equation and were similar to (S Type) according to Giles classification.