An attempt was made for understanding the sorption behaviour of different actinide ions Pu4+, PuO22+, Am3+, Np4+, and NpO22+ on carbonate treated exhausted coffee powder (CTCP). Very efficient sorption of Pu4+ over other actinide ions from aqueous acidic medium was observed. Almost 4 h were required for achieving equilibrium. Experimental results for Pu+4 were fitted into different sorption isotherm model: Langmuir isotherm, Freundlich isotherm, D.R, isotherm and Temkin isotherm. Based on the linear regression, it was found that, Freundlich isotherm was predominantly operative. Pseudo 2nd order kinetics was found to be effective for the sorption of Pu+4. More than 80 % of loaded Pu4+ was found to desorb by 0.25 M oxalic acid solution. CTCP exhibited relatively good radiation stability. Sorption of Pu+4 on CTCP was exothermic, and spontaneous in nature. The sorption process was simple, cost effective and environmentally benign, as it did not involve any sophisticated, multi-step, sorbent synthesis.

Zirconium phosphosilicate (ZPS) has been prepared by gelation route for its ion exchange applications. ZPS was characterised by X-ray diffraction technique (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), Fourier transformed Infrared Spectrometry (FTIR) and surface area analysis. K+ ion exchange behaviour was studied by pH titration. The material was found to extract Pu selectively over U from different mineral acids. Pu sorption behaviour on ZPS packed column was also been carried out. The pore volume was evaluated as 0.1336 mL g(-1). The FTIR revealed the presence of -Oil and PO(4)(3- )groups on the surface of the material, while the SEM image indicates the irregular morphology and size of the sorbent. Different isotherm model: Langmuir, Freundlich, Dubinin-Rodushkevich and Temkin were used to understand the nature of sorption, while Lagergren 1st order, Intrapartide diffusion and pseudo 2nd order kinetics were used for modelling sorption kinetics. Suitable elution method was used for quantitative stripping of plutonium from sorbent. The radiolytic stability of the sorbent was evaluated upto 1500 kGy. A comparative evaluation of the sorption process has also been carried out with that reported in literature.

Titania–silica microspheres have been prepared by sol–gel process. Internal gelation route, which use hexamethylenetetramine as the source of ammonia was used for the preparation spherical gel particles. A cationic surfactant, cetrimide was added in the feed broth for introducing meso-porosity in the gel network. Further paraffin oil emulsion was incorporated in the feed broth before gelation for the formation of larger pores in the gel network. The spherical gel particles thus obtained were washed and heat treated under controlled conditions to remove the entrapped surfactant, paraffin oil and other organic compounds resulting in highly porous intact titania–silica microspheres. The material was characterized by surface area, porosity and by SEM photomicrographs. The ion exchange property of this material was studied using the sorption of plutonium on this material from carbonate medium by distribution coefficient studies and ion exchange column loading and elution experiments.

A sol–gel based hybrid process was developed by manipulating different techniques in sol–gel process to synthesize γ-alumina and (CuO, CuO + ZnO) doped γ-alumina spherical particles. Catalysts having spherical geometry have an important advantage over powders or pellets which are impervious to fluids, when packed in a reactor. Boehmite sol was used as alumina precursor for synthesizing porous γ-alumina and doped materials. γ-alumina particles having 5 wt% CuO, 4 wt% CuO + 1 wt% ZnO, 3 wt% CuO + 2 wt% ZnO and 2 wt% CuO + 3 wt% ZnO were prepared by adding required amounts of Cu(NO3)2 and Zn(NO3)2 solutions prior to gelation of the sol. Methanol dehydration studies were carried out by employing these synthesized catalysts. Hundred percent conversion of methanol to dimethyl ether was observed with (4 wt% CuO + 1 wt% ZnO)-γ-alumina and (5 wt% CuO)-γ-alumina microspheres at 325 and 350 °C, respectively.

Internal gelation process was employed for preparation of 0.3–1 mm sized microspheres of titania for their application in ion exchange columns. The conventional internal gelation process was modified by adding surfactant and oil emulsion in the feed broth, which introduced large pores in the structure of the material. The effects of concentration of hydrochloric acid, titanium, surfactant and hexamethylenetetramine to titanium ratio in the feed broth and temperature of calcination on the surface characteristics of the final product were studied. The conditions of preparation were optimized to obtain physically stable porous microspheres suitable for various applications. The resultant material was characterized by pore size distribution, pore volume, thermogravimetry, X-ray diffraction and SEM analyses. Ion exchange behaviour of the material was then studied by pH titration.

Polyacrylhydroxamic acid resin synthesized by functionalization of polyacrylamide with hydroxylamine has been investigated for the sorption of plutonium(IV) from carbonate medium, aiming at its application for the removal of plutonium from alkali wash effluent generated during purification of TBP in PUREX process. Batch experiments have been carried out to determine distribution coefficient of plutonium(IV) between this exchanger and various compositions of carbonate medium. Effect of the concentration of sodium carbonate, sodium bicarbonate and pH of the solution on the distribution coefficient have been studied to optimize the conditions for the uptake of Pu(IV) by this exchanger. Column experiments were carried out to determine the practical capacity of the exchanger for plutonium. Elution studies were also carried out to recover the loaded plutonium from the ion exchange column The exchanger displayed good exchange capacity for Pu(IV) from feed solution simulating the conditions of carbonate wash effluent generated in PUREX process. The exchanger also exhibited fast elution of Pu, suggesting the feasibility of using it for the recovery of Pu from carbonate based wash effluent.

Mesoporous γ-alumina samples were prepared by the sol–gel process from the boehmite sol having different template solutions. Copper doped material was also prepared from sol containing template solution along with copper nitrate. Studies were performed to understand the influence of templates on the morphology of the synthesized samples particularly with respect to specific surface area and porosity. Synthesized samples were used to study sorption of Pu(IV) from nitric acid–oxalic acid solutions. Distribution ratios (D) for Pu(IV) were determined using the γ-alumina samples with an objective to employ these for the recovery of Pu.

Porous zirconia spherical particles have been prepared by internal gelation process. During preparation of these spherical particles, a cationic surfactant, cetrimide was added in the feed broth to increase the surface area and porosity of the particles. The sorption behavior of plutonium was investigated on this material from different complexing aqueous media from the recovery point of view. Distribution ratio studies have been carried out to investigate the effect of varying concentrations of oxalic acid, phosphoric acid, sulphuric acid, nitric acid, sodium carbonate and sodium bicarbonate to optimize the conditions of sorption of plutonium on this ion exchange material.

A modified internal gelation process for the preparation of porous zirconia microspheres has been developed. The conventional method has been modified by adding a surfactant in the feed broth. The effects of variation of surfactant concentration, washing techniques and temperature of calcination on the pore volume and the surface area of the microspheres have been studied. The conditions were optimized to obtain porous stable microspheres suitable for various applications. The microspheres were characterized by surface area analysis, pore volume analysis, thermogravimetric analysis and X-ray diffraction. The ion exchange behavior was studied using pH titration.