Novel Hybrid Nanoparticles: Synthesis, Functionalization, Characterization, and Their Application in the Uptake of Scandium (III)Ions from Aqueous Media (original) (raw)
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Separation and Purification Technology, 2018
Comparative and synergistic solvent extraction of Sc(III) using two phosphoric acidic reagents such as di-(2-ethyhexyl) phosphoric acid and 2,4,4,tri-methyl,pentyl-phosphinic acid was investigated. Slope analysis method suggests a cation exchange reaction of Sc(III) with both extractants at a molar ratio of extractant: Sc(III) = 2.5:1 at equilibrium pH< 1.5. The plot of log D vs. log [Extractant] yield the slope (n) value as low as 1.2-1.3 and as high as n=7 at low and high extrcatant concentration level, respectively. Extraction isotherm study predicted the need of 2 stages at A: O=1:4 and A: O=1:3 using 0.1 M D 2 EHPA and 0.1 M Cyanex 272, respectively. Stripping of Sc (III) was carried out at varied NaOH concentration to ascertain the optimum stripping condition for effective enrichment of metal. The predicted stripping condition (2-stages with A: O=1:3 and 1:4 for D 2 EHPA and Cyanex 272, respectively) obtained from Mc-Cabe Thiele plot was further validated by 6-cycles CCS study. An actual leach solution of Mg-Sc alloy bearing 1.0 g/L of Sc (III), 2.5 g/L of Mg and 0.2 M HCl was subjected for selective separation of Sc at the optimum condition. The counter current simulation (CCS) study for both extraction and stripping of actual solution resulted quantitative separation of Sc with ~12 fold enrichment. The organic phase before and after loading of Sc (III) along with the diluents was characterized by FTIR to ascertain the phase transportation of Sc (III).
Extraction of scandium ions by new aminophosphinyl extractants
Russian Journal of General Chemistry, 2009
Extraction of Sc(III) ions by new aminophosphinyl compounds containing one or two methylenediorganylphosphinyl groups at the nitrogen atom was studied with a target of the development of effective and selective extractants of trace elements. The selection of extractants was due to their high hydrolytic stability in the acid media, commonly used at the extraction of metal ions in the industrial hydrometallurgical processes. The study of extraction of hydrogen chloride and nitric acids with the selected aminophosphinyl compounds allowed a discovery of substances with the low basicity, which were characterized by the low coefficient of the acids extraction. Highly effective extractants of Sc(III) were found possessing high coefficients of extraction and high degree of selectivity in the separation of Sc(III) ion from the ions of satellite metals.
Liquid–liquid extraction of scandium with nalidixic acid in dichloromethane
Journal of Radioanalytical and Nuclear Chemistry, 2012
The extraction behavior of nalidixic acid (HNA) in CH 2 Cl 2 has been studied for various di-and trivalent metal ions such as Cu(II), Fe(II), Ni(II), Mn(II), Sb(II), Co(II), Sc(III), Y(III), Nd(III) and Eu(III) from aqueous buffer solutions of pH 1-7 with 0.1 mol dm -3 nalidixic acid in dichloromethane. Separation factors of Sc(III) from these metals has shown that its clean separation is possible at pH 3.4-4. The parameters affecting the extraction of Sc(III) were optimized. The composition of the extracted adduct was determined by slope analysis method that came out to be Sc(NA) 3 . Extraction of Sc(III) was studied in the presence of various cations and anions. Among the anions studied only fluoride, citrate and oxalate have significant interference whereas, Fe(III) has reduced the extraction to 53% that can be removed by using ascorbic acid as reducing agent. The proposed extraction system proved good stability up to six extraction-stripping stages for the extraction of Sc(III).
Recovery of scandium(III) from diluted aqueous solutions by a supported ionic liquid phase (SILP
The adsorption of scandium from diluted, acidic solutions by a supported ionic liquid phase (SILP) was investigated, as part of a process for recovery of scandium from bauxite residue (red mud). Both dry impregnation and covalent linking were studied for the SILP preparation. The SILP betainium sulfonyl(trifluoromethanesulfonylimide) poly(styrene-co-divinylbenzene) [Hbet-STFSI-PS-DVB] was prepared by covalent linking of the ionic liquid to the resin and this resulted in an adsorbent suitable for scandium recovery. For a chloride feed solution, the effects of pH, contact time, adsorption capacity, desorption, reusability of adsorbent and the influence of Fe(III), Al(III) and Ca(II) on the Sc(III) adsorption were studied. The adsorption of Sc(III) from nitrate and sulfate feed solution under optimal conditions was studied as well. The adsorption kinetics followed a pseudo-second order kinetic model. Equilibrium studies at room temperature showed that the experimental data could be well fitted by the Langmuir isotherm model. The stripping of Sc(III) from the loaded SILP was achieved with 1 M sulfuric acid. The SILP was stable and could be reused for seven adsorption/desorption cycles without significant losses in its adsorption efficiency for Sc(III).
Solid-Phase Extraction of Antimony Using Chemically Modified SiO2-PAN Nanoparticles
Journal of AOAC INTERNATIONAL, 2010
A new analytical method using 1-(2-pyridylazo)-2-naphthol (PAN)-modified SiO2 nanoparticles as solid-phase extractant has been developed for the preconcentration of trace amounts of Sb(III) in different water samples. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions, and effects of interfering ions for the recovery of the analyte were investigated. The adsorption capacity of nanometer SiO2-PAN was found to be 186.25 mol/g at optimum pH and the LOD (3) was 0.60 g/L. The extractant showed rapid kinetic sorption. The adsorption equilibrium of Sb(III) on nanometer SiO2-PAN was achieved in 10 min. Adsorbed Sb(III) was easily eluted with 4 mL 2 M hydrochloric acid. The maximum preconcentration factor was 62.20. The method was applied for the determination of trace amounts of Sb(III) in various water samples (tap, mineral water, and industrial effluents).
Heavy metal ions extraction from aqueous media using nanoporous silica
Chemical Engineering Journal, 2011
Nanoporous silica (NP) was synthesized and modified with thiol moiety [NPSi-SH]. Thermal gravimetric analysis (TGA) of [NPSi-SH] proved its high thermal stability in the temperature range of 25-600 • C. Structural identification of surface modification of [NPSi-SH] was also confirmed on the basis of surface coverage value from the study of thermal desorption method and FT-IR as well as electron impactmass spectrometry (EI-MS) by the direct insertion probe. A study was performed to explore the metal adsorption, chelating and selectivity properties of [NPSi-SH] toward a series of di-and tri-valent toxic and nontoxic metal ions via determination of the metal capacity and distribution coefficient values. The incorporated selectivity characters of [NPSi-SH] were studied based on determination of the distribution coefficient and separation factor and the results have strongly referred to high affinity toward binding and up-take of anionic and cationic Hg(II) species in all the studied pH range (1.0-7.0). Also, The proposed mechanisms of adsorption of Hg(II) were suggested at different pH. The selective removal and extraction of Hg(II), via micro-column packed with [NPSi-SH], versus other toxic and nontoxic metal ions from drinking tap water samples were also explored. Excellent percentage extraction values of Hg(II) were characterized as 98.1 ± 4.0%, 98.0 ± 4.0% and 97.7 ± 3.0% from water samples buffered to pH 1.0, 2.0 and 7.0 respectively. The other tested metal ions were found to exhibit percentage extraction values of 94.0 ± 5.0% for Cd(II), 93.6 ± 4.0% for Cu(II) and 90.5 ± 5.0% for Zn(II) from pH 7.0 water samples. Different important analytical factors were applied to compare and show superiority of synthesized [NPSi-SH] phase with other previously reported silica gel phases-loaded-thiol [Si-SH].
Analytical Sciences, 2006
Two new chelating materials (Si-DDE-o-HB, and Si-DDS-o-HB) were synthesized by modifying the activated silica gel phase with Schiff bases of 4,4′-diaminodiphenylether (DDE)/4,4′-diaminodiphenylsulfone (DDS) and ohydroxybenzaldehyde (o-HB). The synthesized materials were characterized by FTIR and BET surface area measurement techniques. The extraction of metal ions such as Zn 2+ , Mn 2+ and Cr 3+ by the chelating material Si-DDE-o-HB was found to be higher than that by Si-DDS-o-HB. The order of metal sorption was found to be Zn 2+ > Mn 2+ > Cr 3+. The correlation coefficients for Freundlich and Langmuir adsorption isotherms were compared for the sorption of Zn 2+ onto the chelating material. The loading and elution of the metal ion solution was examined at optimum pH 7.5 and 0.5 cm 3 min-1 flow rate of the solution using a column technique. The preconcentration factor for the elution of Zn 2+ using dilute HNO3 was found to be 66.2 with a breakthrough volume of 15 cm 3. The data obtained for the preconcentration of Zn 2+ by the column technique suggested that the material Si-DDE-o-HB can find industrial applications.
Materials Science and Engineering: C, 2013
Silica chemically bonded N-propyl kriptofix 21 Silica chemically bonded N-propyl kriptofix 22 Solid phase extraction Silica gel chemically bonded N-propyl kriptofix 21 (SBNPK 21) and N-propyl kriptofix 22 (SBNPK 22) and subsequently immobilized with palladium nanoparticles (PNP-SBNPK 21 and PNP-SBNPK 22) to produce two new complexing lipophilic materials. Then these novel sorbents were applied for the enrichment of some metal ions and their subsequent determination by flame atomic absorption spectroscopy (FAAS). The influences of the variables including pH, amount of solid phase, sample flow rate, eluent conditions and sample volume on the metal ion recoveries were investigated. The detection limit of proposed method was in the interval 2.1-2.3 and 1.7-2.8 ng mL −1 for PNP-SBNPK 21 and PNP-SBNPK 22 respectively, while the preconcentration factor was 80 for two sorbents. The relative standard deviations of recoveries were between 1.23-1.31 and 1.28-1.49 for PNP-SBNPK 21 and PNP-SBNPK 22 respectively. The method has high sorption-preconcentration efficiency even in the presence of various interfering ions. Due to the reasonable selectivity of proposed method, the relative standard deviation of recoveries of all understudied metal ions in some complicated matrices was less than 3.0%.
Separation Science and Technology, 2018
The Mg-Sc alloy leach solution bearing 2.5 g/L Sc(III), 25.0 g/L Mg(II) and 0.5 M HCl was subjected to investigate for separation of Sc(III) by hollow fibre liquid membrane (HFLM) followed by its recovery through oxalate precipitation route. Ionic liquid (IL) R 4 ND derived from commercial organo-phosphoric acid (D 2 EHPA) and aliquot-336 was used as carrier in this study. Equilibrium study ensures on extraction of Sc(III) as ScCl 3 with association of 3 mole of R 4 ND in the extracted phase. The role of chloride and R 4 ND concentration appears to be critical while enhancing the Sc flux (J Sc). The complex formation during extraction of Sc(III) into the carrier phase was confirmed from FTIR analysis. Maximum J Sc of 10.41 × 10-−5 mol/m 2 .s was obtained at the optimum condition: pH 4.0, 0.4 M R 4 ND, flow rate 150 mL/min., 6.0 M NaOH, Feed: Strip = 3:1 and after 90 min. of HFLM continuous run of almost all scandium separation from scrap solution was achieved on yielding threefold enrichment into the strip phase which bears 7.49 g/L of scandium. The stripped solution resulted was precipitated using oxalic acid and substantially calcined to produce Sc 2 O 3. The pure form of Sc 2 O 3 produced in the present work was ensured from XRD analysis.
Improved procedures of Sc(OH)3 precipitation and UTEVA extraction for 44Sc separation
Nuclear medicine review. Central & Eastern Europe, 2019
BACKGROUND 44Sc is becoming attractive as a PET radionuclide due to its decay characteristics. It can be produced from 44Ca present in natural calcium with 2.08% abundance. MATERIALS AND METHODS The targets were mostly prepared from natural CaCO3 or metallic calcium in the form of pellets. After irradiation they were dissolved in 3 M hydrochloric acid and 44Sc was separated from excess of calcium by precipitation of scandium hydroxide using ammonia. Alternatively, targets were dissolved in 11 M hydrochloric acid and 44Sc was separated by extraction chromatography on UTEVA resin. As the next step, in both processes 44Sc was further purified on a cation exchange resin. Initially, the separation procedures were developed with 46Sc as a tracer. Gamma spectrometry with a high purity germanium detector was used to determine the separation efficiency. Finally, the CaCO3 pellet with 99.2% enrichment in 44Ca was activated with protons via 44Ca(p,n)44Sc nuclear reaction. RESULTS Altogether tw...