Chemically modified rice husk as an effective adsorbent for removal of palladium ions.

Bio-matrix of rice husk and Mobil Composition of Matter No. 41 (MCM-41) was modified with alizarin red S for preconcentration of Pd2+ prior flame atomic absorption spectrometric determination. The prepared bio-matrix (RH@MCM-41@ARS) was characterized by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope, energy dispersive X-ray spectrometer (SEM/EDX) and surface area studies. The impact of different parameters (solution pH, amount of sorbent, contact time, sample volume, initial Pd2+ concentration and diverse ions) on the uptake of Pd2+ were evaluated. The maximum adsorption capacity of Pd2+ onto RH@MCM-41@ARS was 198.2 mg g-1 at optimum conditions. Applying the optimized procedure as a preconcentration step led to limit of detection of 0.13 µg L-1 and dynamic analytical range up to 500 µg L-1. The sorbent was regenerated by 0.5 mol L-1 thiourea for at least 10 cycles without significant reduction of adsorption capacity. The method was applied for preconcentration of Pd2+ from real samples.

Synthesis and application of hydrazono-imidazoline modified cellulose for selective separation of precious metals from geological samples.

A new hydrazono-imidazoline modified cellulose (HIMC) was synthesized for selective recovery of Pt(IV), Pd(II) and Au(III) from geological samples. Cellulose was oxidized by periodate and was further functionalized with hydrazono-imidazoline moieties to afford N-donor chelating fibers. Scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR), X-ray diffraction (XRD), N2 physisorption, elemental analysis, and energy-dispersive X-ray spectroscopy (EDX) were used for characterization. Introducing the hydrazono-imidazoline groups at the surface of cellulose fibers did not alert their ordered structure and crystallinity, as indicated by XRD and SEM results. Factors affecting the adsorption were systematically investigated. Under the optimized conditions, the HIMC sorbent exhibited high adsorption capacities of 105, 88 and 75 mg g-1 for Pt(IV), Pd(II) and Au(III), respectively. Besides, the metal ion adsorption process fitted by pseudo-second-order kinetic model and Langmuir adsorption isotherm. These results highlight the applicability of this carbohydrate-based sorbent for the selective recovery of precious metals from various matrices.

Preparation of lactic acid modified cellulose nanoparticles by microwave heating for preconcentration of copper from blood and food samples.

In this study, nano-sized cellulose modified with lactic acid (MW-Ce-LA) was prepared with the assistant of microwave then used for the adsorption of Cu2+ from real samples. This modified cellulose was characterized by means of FTIR, TEM, XRD, and elemental analysis. ICP-OES was used for determination of Cu2+. The effect of pH, adsorption times, temperature, sorbent dose, and initial adsorbate concentration were studied to detect the ideal adsorption condition. Langmuir model proved to be the best to fit the adsorption isotherm experiments with maximum adsorption capacity of 90.3 mg g-1 Cu2+. Calculated thermodynamic parameters (ΔG° and ΔH°) for adsorption of Cu2+ on MW-Ce-LA suggested exothermic and nonspontaneous character of the adsorption process. The reusability tests indicated regeneration of the prepared adsorbent simply using 1 mol L-1 of HCl. The examined method was used effectively to preconcentrate Cu2+ from water, blood, and food samples.

Solid Phase Extraction and Preconcentration of Trace Gallium, Indium, and Thallium Using New Modified Amino Silica.

Amino silica gel functionalized with 2-hydroxy-5 -(2-hydroxybenzylideneamino)benzoic acid was synthesized, characterized and used as adsorbent for the removal of Ga3+, In3+ and Tl3+ from aqueous solution prior to their determination by flame atomic absorption spectrometry. Experimental parameters that affect the separation process were investigated in both batch and column modes. The maximum adsorption capacities of the sorbent are 61.7 mg g-1, 81.3 mg g-1 and 133.0 mg g-1 for Ga3+, In3+ and Tl3+, respectively. The preconcentration factor is 200 and the limits of detection of Ga3+, In3+ and Tl3+ are 4.10 µg L-1, 1.55 µg L-1 and 1.21 µg L-1, respectively. Interference by Al3+ can be masked by the addition of F-; and that of Fe3+ by its reduction to Fe2+ using 10% ascorbic acid. The method was successfully applied for the determination of these ions in water, sediments and liquid crystal display samples.

Impact of dialyzer membrane flux on metal clearance in hemodialysis patients.

Deficiency of essential trace elements (such as Cu or Zn) and accumulation of potentially toxic trace elements (as Cd or Pb) are both known to have adverse effects in hemodialysis (HD) patients. Up to our knowledge, no studies about the permeability of low and high flux polysulfone membranes on metal ions during hemodialysis are available. Therefore, the aim of the present study was to address this issue. Forty one hemodialysis patients (19 were using high flux polysulfone membrane while the remaining were using low flux one) participated in the study. Blood levels of Cu, Zn, Cd and Pb were determined by graphite furnace atomic absorption spectrometry among HD patients, before and after dialysis session, as well as among matched 40 healthy persons. Blood concentrations of Cu and Zn in the whole hemodialysis group was significantly lower than those of the healthy control group, on the other hand the toxic metals (Cd and Pb) levels were observed to be significantly higher among HD patients compared to the normal persons. Among the hemodialysis group, there were no significant differences between the low and high flux dialyzer groups in terms of pre-dialysis blood levels of Cu, Zn, Cd and Pb. In addition, significantly decreased levels of all metal ions were observed after dialysis sessions using either low or high flux membranes. An exception was Pb which did not show any difference between pre-dialysis and post-dialysis values in the low flux groupIn conclusion Zn and Cu deficiencies should be considered in the treatment of these patients. High flux membranes are more efficient than low flux ones in removing excess Cd and Pb. Therefore, when high flux membranes are used, chelation therapy might not be required for Cd and Pb overload.

Mixed Micelle-mediated Extraction and Separation of Scandium from Yttrium and Some Lanthanide Ions.

A simple mixed-micelle mediated extraction was elaborated for the preconcentration and determination of scandium(III) by inductively coupled plasma optical emission spectrometry. Scandium(III) was complexed with Alizarin Red S and cetyltrimethylammonium bromide at pH 3 to form hydrophobic chelates, which could be extracted with Triton X-114 at room temperature (25°C) in the presence of KI as a salting-out electrolyte. The main parameters of the extraction procedure were investigated in regard to the extraction efficiency of scandium(III). Under the optimum conditions, a linear range of 0.5 - 150 ng mL(-1) and a detection limit of 0.2 ng mL(-1), along with a preconcentration factor of 100, were achieved. Furthermore, the interference of diverse ions accompanying scandium(III) was extensively studied. The obtained results indicate the high selectivity of the proposed procedure. The accuracy of the procedure was verified through recovery experiments on spiked water samples and synthetic mixtures. The procedure was successfully applied to a scandium(III) determination in clay samples.

Cellulose derivatives modified by sodium tellurate and a chromium(III) tellurate complex.

A novel cellulose (Cell) derivative, sodium-tellurato (Cell-TeO(OH)4(ONa)/Cell-Cl), has been synthesized from the reaction of 6-chloro-6-deoxycellulose (Cell-Cl) with telluric acid in the presence of sodium hydroxide. The subsequent reaction of this polymeric material with chromium(III) in aqueous solution yields the [Cr(Cell-TeO3(OH)3/Cell-Cl)(Cell-TeO2(OH)4/Cell-Cl)(H2O)3] complex. The molecular structures and morphology of the new polymer and the Cr(III) complex have been examined using elemental analysis, solid-state (13)C NMR, UV-vis, XRD and FTIR spectroscopy, and SEM-EDX, TGA and magnetic measurements. The results are considered to be consistent with the formulations proposed. The deprotonation constants of the modified cellulose and the stability constant of the Cr(III) complex have been determined by pH-metric measurements.

Determination of Cu(2+), Zn(2+) and Pb(2+) in biological and food samples by FAAS after preconcentration with hydroxyapatite nanorods originated from eggshell.

Hydroxyapatite nanorods (HAPNRs) were prepared from recycled eggshell by using precipitation method. The structure of the HAPNRs was physicochemically and morphologically characterized by X-ray diffraction, transmission electron microscopy and Fourier transform infrared spectroscopy. The resulting HAPNRs were used for solid phase extractive preconcentration of Cu(2+), Zn(2+) and Pb(2+) prior to its determination by flame atomic absorption spectrometry. Experimental variables that influence the quantitative extraction of metal ions were optimized by both batch and column methods. The analytes were quantitatively sorbed on the matrix between pHs6 and 9. The maximum sorption capacity of the HAPNRs has been found to be 2.43, 2.37 and 2.53 mmol g(-1) for Cu(2+), Zn(2+) and Pb(2+), respectively, with the preconcentration factor of 250. The 3σ detection limit and 10σ quantification limit for Cu(2+), Zn(2+) and Pb(2+) were found to be 0.72, 0.55 and 5.12 µg L(-1) and 2.40, 1.83 and 17.06 µg L(-1), respectively. The calibration curves were linear up to 250 µg L(-1) for Cu(2+), 300 µg L(-1) for Zn(2+) and 400 µg L(-1) for Pb(2+). Accuracy of the proposed method was verified using certified reference materials (NCS ZC85006 Tomato, Seronorm Trace Elements Whole Blood L-1, Seronorm Trace Elements Whole Blood L-3 and Seronorm Trace Elements Urine). The present method was successfully applied to the analysis of these metal ions in sea water, biological and food samples.

Selective preconcentration of uranyl ion by silica gel phases modified with chelating compounds as inorganic polymeric ion exchangers.

Four chemically modified chelating silica gel phases (I - IV) with ion exchange groups were tested for their potential capability to selectively bind, extract and preconcentrate uranyl ions (UO(2)(2+)) from different aqueous solutions as well as ore samples. Factors affecting such determination processes were studied and optimized. These included the pH of the contact solution, the mass of the silica gel phase extractant, the stirring time during the application of a static technique and the eluent concentration for desorption of the surface-bound uranyl ion and interfering anions and cations. All these factors were evaluated on the basis of determinations of the distribution coefficient value (K(d)) and the percent recovery (R%). Percent recovery values of 91% for silica phase (II) and 93% for silica phase (IV) were identified in the optimum conditions. The proposed preconcentration method was further applied to uranium ore samples as well as granite samples. The determined percentage and ppm values are in good agreement with the standard assigned ones. The structure of the synthesized silica gel phases (I - IV) and their uranyl bound complexes were identified and characterized by means of infrared analysis, thermal analysis (TGA) and potentiometric titration.

Separation and preconcentration of gallium(III), indium(III), and thallium(III) using new hydrazone-modified resin.

Ga(III), In(III) and Tl(III) ions in the presence of different sulfate salts have been successfully separated using 1-(3,4-dihydroxybenzaldehyde)-2-acetylpyridiniumchloride hydrazone (DAPCH) loaded on Duolite C20 in batch and column modes. The obtained modified resin as well as the metal complexes was characterized by elemental analysis and infrared spectra. The extraction isotherms were determined at different pH values. Ga(III) and In(III) are sorbed from aqueous solution at pH 2.5 - 3.0 while Tl(III) is sorbed at 2.0. The stripping of the adsorbed ions can be carried out using different concentrations of HCl as eluent. The saturation sorption capacities of Ga(III), In(III) and Tl(III) were 0.82, 0.96 and 0.44 mmol g(-1), where the preconcentration factors are 150, 150 and 100, respectively. The metal(III):Duolite C20-DAPCH ratio was 1:2 for Tl(III) and 1:1 for In(III) and Ga(III). The loaded resin can be regenerated for at least 50 cycles. The utility of the modified resin was tested in aqueous samples and the results show an RSD value of < 5% reflecting their accuracy and reproducibility.