The synthesis of needle/fibrous particles of analogue of heulandite with particle diameter of 0.08 μm, length 4–8 μm and high specific surface area (478 m 2 g −1) with cation exchange capacity (3.27 mequiv g −1) have been achieved. The heulandite needles were obtained by using inorganic salts as a source for silicon and aluminum in the hydrothermal synthesis of the material. Alkalinity of the medium played an important role in the formation of heulandite fibers, as it affects the nucleation rate of zeolite synthesis. The analogue of heulandite was characterized using spectroscopic, thermal analysis, scanning and adsorption techniques. After mechanical grinding of crystals of heulandite, obtained powder was used for the study of radionuclide recovery from aqueous waste. The adsorption experiments were carried out under batch process with, pH of medium, amount of sorbent, time of contact between sorbate and sorbent, metal ion concentration and temperature as the variables. The adsorption was strongly dependent on pH of the medium and the uptake of all the metal ions increased from pH 1.0 to 9.0 and the maximum sorption was noticed in the pH range of 5.0–7.0. The optimum condition for these metal ions (Th(IV), Eu(III), Sm(II), and Fe(III)) sorption on self synthesized analogue of heulandite was; 0.001 N metal ion concentration, equilibration time of 4 h, 100 mg sorbent dose and 313–323 K temperature. This sorption process is fit to both Langmuir and Freundlich sorption isotherm. Thermodynamic studies predict the endothermic and spontaneous nature of the same.
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