Extraction and separation of Co(II) and Ni(II) from acidic sulfate solutions using Aliquat 336

Extraction and separation of Co(II) and Ni(II) from acidic sulfate solutions by solvent extraction technique were studied using different forms of Aliquat 336 diluted with kerosene. The extraction percent of each metal ion was found to increase with increasing pH and extractant concentration. Co(II) was preferentially extracted by different forms of Aliquat 336 over Ni(II) under the same extraction conditions. From analysis of the experimental results, the extraction mechanism of R₄N-forms was proposed with Co(II). It was found that the highest separation factor (S_Co/Ni) value of 606.7 was obtained with 0.36 M R₄N–SCN in kerosene from 2.0 M H₂SO₄ solution at pH 4.8 and shaking time of 20 min. Stripping of the two metal ions from the organic phase was also investigated. Based on the experimental results, a separation method was developed and tested to separate high purity Co(II), Ni(II) and Ln(III) from Ni–MH batteries leached by 2.0 M H₂SO₄. Based on the experimental results, a flow sheet was developed and tested and 0.34 g Co, 1.39 g Ln and 5.2 g Ni were obtained from the leaching process.     

Selective detection of toxic Pb(II) ions based on wet-chemically prepared nanosheets integrated CuO–ZnO nanocomposites

The present study describes a selective detection methodology for hazardous metal ions based on low-dimensional nanosheets (NSs) integrated CuO–ZnO composite materials. A large-scale synthesis of NSs by wet-chemical process is performed using alkaline reducing agents at higher pH medium. The prepared NSs are characterized in terms of their morphological, structural and optical properties, and efficiently applied for the toxic metal ions detection. The detailed structural, compositional, and optical characterization of NSs are evaluated by XRD, FT-IR, XPS, EDS, and UV–vis spectroscopy, which confirmed that the obtained NSs are well-crystalline CuO–ZnO and possessed good optical properties. The CuO–ZnO NS morphology is investigated by FE-SEM, which confirmed that the NS possesses microstructure shape and growth in large-quantity. The analytical application of CuO–ZnO NSs is studied for a selective extraction of toxic lead-divalent [Pb(II)] ions prior to its determination by inductively coupled plasma-optical emission spectrometry (ICP-OES). The selectivity of doped NSs phase is investigated for eight different metal ions, including Cd(II), Cu(II), Hg(II), La(III), Mn(II), Pb(II), Pd(II), and Y(III) under similar experimental conditions. From the selectivity study, it is confirmed that the composite CuO–ZnO NS phase is the most toward Pb(II) ions according to the magnitude of distribution coefficient (K_d) values, such as Pb(II) > Y(III) > Cd(II) > La(III) > Hg(II) > Cu(II) > Mn(II) > Pd(II). The uptake capacity for Pb(II) is experimentally calculated to be ∼82.66 mg g⁻¹.     

Synthesis of magnetite nanoparticles by surfactant-free electrochemical method in an aqueous system

A simple surfactant-free electrochemical method is proposed for the preparation of magnetite nanoparticles using iron as the anode and plain water as the electrolyte. This study observed the effects of certain parameters on the formation of magnetite nanoparticles and their mechanism in the system, including the role of OH^? ions, the distance between electrodes and current density. We found that OH^? ions play an important role in the formation of magnetite nanoparticles. Particle size can be controlled by adjusting the current density and the distance between electrodes. Particle size increases by increasing the current density and by decreasing the distance between electrodes. Particle formation cannot be favored when the distance between electrodes is larger than a critical value. The magnetite nanoparticles produced by this method are nearly spherical with a mean size ranging from 10 to 30 nm depending on the experimental conditions. They exhibit ferromagnetic properties with a coercivity ranging from 140 to 295 Oe and a saturation magnetization ranging from 60 to 70 emu g^?1, which is lower than that of the corresponding bulk Fe₃O₄ (92 emu g^?1). This simple method appears to be promising as a synthetic route to producing magnetite nanoparticles.     

Removal of Pb(II) ions from aqueous solution by adsorption using bael leaves (Aegle marmelos)

Biosorption of Pb(II) on bael leaves (Aegle marmelos) was investigated for the removal of Pb(II) from aqueous solution using different doses of adsorbent, initial pH, and contact time. The maximum Pb loading capacity of the bael leaves was 104 mg g^?1 at 50 mg L^?1 initial Pb(II) concentration at pH 5.1. SEM and FT-IR studies indicated that the adsorption of Pb(II) occurs inside the wall of the hollow tubes present in the bael leaves and carboxylic acid, thioester and sulphonamide groups are involved in the process. The sorption process was best described by pseudo second order kinetics. Among Freundlich and Langmuir isotherms, the latter had a better fit with the experimental data. The activation energy E_a confirmed that the nature of adsorption was physisorption. Bael leaves can selectively remove Pb(II) in the presence of other metal ions. This was demonstrated by removing Pb from the effluent of exhausted batteries.     

Preparation of Fe3O4–chitosan nanoparticles used for hyperthermia

The Fe₃O₄–chitosan nanoparticles with core-shell structure have been prepared by crosslinking method. Oleic acid modified Fe₃O₄ nanoparticles were firstly prepared by co-precipitation then chitosan was added to coat on the surface of the Fe₃O₄ nanoparticles by physical absorption. The Fe₃O₄–chitosan nanoparticles were obtained by crosslinking the amino groups on the chitosan using glutaraldehyde. Transmission electron microscopy showed that the Fe₃O₄–chitosan nanoparticles were quasi-spherical with a mean diameter of 10.5 nm. X-ray diffraction pattern and X-ray photoelectron spectra indicated that the magnetic nanoparticles were pure Fe₃O₄ with a cubic inverse spinel structure. The modification using chitosan did not result in a phase change. The binding of chitosan to the Fe₃O₄ nanoparticles was also demonstrated by the measurement of fourier transform infrared spectra and thermogravimetric analysis. Magnetic measurement revealed that the saturation magnetization of the composite nanoparticles was 30.7 emu/g and the nanoparticles were superparamagnetic at room temperature. Furthermore, the inductive heating property of the composite nanoparticles in an alternating current magnetic field was investigated and the results indicated that the heating effect was significant. The Fe₃O₄–chitosan nanoparticles prepared have great potential in hyperthermia.     

Electromagnetic and microwave-absorbing properties of magnetite decorated multiwalled carbon nanotubes prepared with poly(N-vinyl-2-pyrrolidone)

The magnetite (Fe₃O₄) decorated multiwalled carbon nanotubes (MWNTs) hybrids were prepared by an in situ chemical precipitation method using poly(N-vinyl-2-pyrrolidone) (PVP) as dispersant. The structure and morphology of hybrids are characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and transmission electron-microscopy (TEM). The TEM investigation shows that the Fe₃O₄/MWNTs hybrids exhibit less entangled structure and many more Fe₃O₄ particles are attached homogeneously on the surface of MWNTs, which indicated that PVP can indeed help MWNTs to disperse in isolated form. The electromagnetic and absorbing properties were investigated in a frequency of 2–18 GHz. The results show that the Fe₃O₄/MWNTs hybrids exhibit a superparamagnetic behavior and possess a saturation magnetization of 22.9 emu/g. The maximum reflection loss is ?35.8 dB at 8.56 GHz, and the bandwidth below ?10 dB is more than 2.32 GHz. More importantly, a new reflection loss peak occurs at the frequency of 14.6 GHz, which indicates that the Fe₃O₄/MWNTs hybrids have better absorption properties in the high-frequency.     

Synthesis and magnetic characterization of magnetite obtained by monowavelength visible light irradiation

Magnetite (Fe₃O₄) nanoparticles were controllably synthesized by aerial oxidation Fe^IIEDTA solution under different monowavelength light-emitting diode (LED) lamps irradiation at room temperature. The results of the X-ray diffraction (XRD) spectra show the formation of magnetite nanoparticle further confirmed by Fourier transform infrared spectroscope (FTIR) and the difference in crystallinity of as-prepared samples. Fe₃O₄ particles are nearly spherical in shape based on transmission electron microscopy (TEM). Average crystallite sizes of magnetite can be controlled by different irradiation light wavelengths from XRD and TEM: 50.1, 41.2, and 20.3 nm for red, green, and blue light irradiation, respectively. The magnetic properties of Fe₃O₄ samples were investigated. Saturation magnetization values of magnetic nanoparticles were 70.1 (sample M-625), 65.3 (sample M-525), and 58.2 (sample M-460) emu/g, respectively.     

Capture and release of genomic DNA by PEI modified Fe3O4/Au nanoparticles

Polyethylenimine (PEI) modified Fe₃O₄/Au nanoparticles were synthesized in aqueous solution and characterized by photo correlation spectroscopy (PCS) and vibrating sample magnetometer (VSM). The so-obtained Fe₃O₄/Au-PEI nanoparticles were capable of efficient electrostatic capture of DNA. The maximum amount of genomic DNA captured on 1.0 mg Fe₃O₄/Au-PEI nanoparticles was 90 μg. The DNA release behavior was studied and the DNA recovery from Fe₃O₄/Au-PEI nanoparticles approached 100% under optimal conditions. DNA extraction from mammalian cells using Fe₃O₄/Au-PEI nanoparticles was successfully performed. Up to approximately 43.1 μg of high-purity (OD₂₆₀/OD₂₈₀ ratio = 1.81) genomic DNA was extracted from 10 mg of liver tissue. The results indicated that the prepared Fe₃O₄/Au-PEI nanoparticles could be successfully used for DNA capture and release.     

Poly(furfuryl alcohol)-assisted pyrolysis synthesis of ceramic nanoparticles for solid oxide fuel cells

A pyrolysis synthesis method was developed to prepare ceramic nanoparticles for the fabrication of solid oxide fuel cells. Furfuryl alcohol was used as a polymerizable solvent to dissolve metal nitrates and then polymerized into poly(furfuryl alcohol) (PFA). During the pyrolysis at 600 °C, a mixture of nitrates/PFA was converted into ceramic nanoparticles/carbon networks nanocomposite, and the carbon networks act as a barrier to prevent the aggregation of newly formed nanoparticles during particle crystallization. Dispersible nanoparticles with particle sizes ranging from 40 nm to 200 nm were obtained after burning off carbon networks in air. As an example, Ce_0.8Sm_0.2O_1.9 nanoparticles were synthesized to prepare solid oxide fuel cells, and the fuel cells achieved maximum power densities of 444.5, 625.5 and 684 mW cm^?2 at 500 °C, 550 °C and 600 °C, respectively. Our study shows that the pyrolysis synthesis method described here is promising for the effective synthesis of high quality ceramic nanoparticles.     

Efficient purification of His-tagged protein by superparamagnetic Fe3O4/Au–ANTA–Co2 + nanoparticles

Superparamagnetic Fe₃O₄/Au nanoparticles were synthesized and surface modified with mercaptopropionic acid (MPA), followed by conjugating Nα,Nα-Bis(carboxymethyl)-l-lysine hydrate (ANTA) and subsequently chelating Co^2 +. The resulting Fe₃O₄/Au–ANTA–Co^2 + nanoparticles have an average size of 210 nm in aqueous solution, and a magnetization of 36 emu/g, endowing the magnetic nanoparticles with excellent magnetic responsivity and dispersity. The Co^2 + ions in the magnetic nanoparticle shell provide docking site for histidine, and the Fe₃O₄/Au–ANTA–Co^2 + nanoparticles exhibit excellent performance in binding of a His-tagged protein with a binding capacity of 74 μg/mg. The magnetic nanoparticles show highly selective purification of the His-tagged protein from Escherichia coli lysate. Therefore, the obtained Fe₃O₄/Au–ANTA–Co^2 + nanoparticles exhibited excellent performance in the direct separation of His-tagged protein from cell lysate.     

Synthesis,characterization and microwave absorption properties of Fe3O4/Co core/shell-type nanoparticles

Co coated Fe₃O₄ core/shell-type nanoparticles were fabricated by hydrothermal technique and electroless plating process. X-ray powder diffraction (XRD), X-ray fluorescence spectrometer (XRF) and transmission electron microscope (TEM) were employed to investigate the crystal structure, element composition and morphology of the prepared nanoparticles. Vibrating sample magnetometer (VSM) and vector network analyzer were used to measure the magnetic properties and electromagnetic parameters of pure Fe₃O₄ and Fe₃O₄/Co core/shell-type nanoparticles, then reflection losses (RL(dB)) were calculated in the frequency range of 2–18 GHz. Magnetic studies revealed typical ferromagnetic behavior for the pure Fe₃O₄ and Fe₃O₄/Co core/shell-type nanoparticles with their saturation magnetization (M_s = 63.1 and 72.4 emu/g) and coercivity (H_c = 99.5, and 165.4 Oe), respectively. Due to the existence of the core/shell structure, the electromagnetic characteristic of the Fe₃O₄/Co nanoparticles exhibit better microwave absorption performance than the pure Fe₃O₄ in the range of 2–18 GHz, such as more powerful absorbing property and wider frequency band of microwave absorption.     

Surface-functionalized pomelo peel-derived biochar with mercapto-1,2,4-triazloe for selective elimination of toxic Pb (II) in aqueous solutions

A novel biochar adsorbent (GP-AMT) is prepared by functionalizing biochar derived from pomelo peel to eliminate Pb (II) from water. GP-AMT was characterized by FTIR, SEM, BET, TGA and XPS. GP-AMT has a large specific area and is multiaperture. The adsorption performance was studied. At the pH = 5, the maximum uptake amount of Pb(II) on GP-AMT reached 420 mg/g. The sorption behavior of GP-AMT obeys with Langmuir and pseudo second-order formula, which shows that the adsorbing property of GP-AMT is uniform chemical sorption. Thermodynamic studies attested that the sorption was an irreversible endothermic course. GP-AMT demonstrated excellent selectivity and reproducibility. After 5 cycles, it still has an excellent sorption property. XPS and zeta potential analysis revealed that the adsorbing nature of GP-AMT for heavy metal ions was coordination and ion exchange. In conclusion, surface modification of biochar can significantly improve its sorption capacity, selectivity and regenerative ability for Pb(II), and reduce the pomelo peel waste pollution.     

Synthesis and characterization of amino acid containing Cu(II) chelated nanoparticles for lysozyme adsorption

Immobilized metal ion affinity chromatography (IMAC) is a useful method for adsorption of proteins that have an affinity for transition metal ions. In this study, poly(hydroxyethyl methacrylate-methacryloyl-l-tryptophan) (PHEMATrp) nanoparticles were prepared by surfactant free emulsion polymerization. Then, Cu(II) ions were chelated on the PHEMATrp nanoparticles to be used in lysozyme adsorption studies in batch system. The maximum lysozyme adsorption capacity of the PHEMATrp nanoparticles was found to be 326.9 mg/g polymer at pH 7.0. The nonspecific lysozyme adsorption onto the PHEMA nanoparticles was negligible. In terms of protein desorption, it was observed that adsorbed lysozyme was readily desorbed in medium containing 1.0 M NaCl. The results showed that the metal-chelated PHEMATrp nanoparticles can be considered as a good adsorbent for lysozyme purification.     

Variation with added material in the effects of reactive mechanical grinding and hydriding–dehydriding cycling on the hydrogen-storage properties of Mg

Samples Mg–14Ni–6Fe₂O₃, Mg–14Ni–3Fe₂O₃–3Ti, and Mg–14Ni–2Fe₂O₃–2Ti–2Fe were prepared by reactive mechanical grinding, and their hydrogen storage properties were examined. The activated Mg–14Ni–2Fe₂O₃–2Ti–2Fe had the highest hydriding rate, absorbing 4.14 wt% H for 5 min, and 4.27 wt% H for 10 min, and 4.42 wt% H for 60 min at 573 K under 12 bar H₂. The activated Mg–14Ni–3Fe₂O₃–3Ti had the highest dehydriding rate, desorbing 3.81 wt% H for 20 min, 3.98 wt% H for 25 min, and 4.15 wt% H for 60 min. Mg–14Ni–6Fe₂O₃ dehydrided at n = 4 contained Mg, Mg₂Ni, MgO, and Mg(OH)₂. Mg(OH)₂ is considered to be formed by the reactions of MgH₂ or Mg with water vapor. The effects of reactive mechanical grinding and hydriding–dehydriding cycling are the creation of defects and cracks, and the reduction of Mg particle size. The addition of a larger amount of Ti and/or Fe has stronger effects of reactive mechanical grinding, whereas the addition of a larger amount of Fe₂O₃ has greater effects of hydriding–dehydriding cycling.     

Effect of 10Ce-TZP/Al2O3 nanocomposite particle amount and sintering temperature on the microstructure and mechanical properties of Al/(10Ce-TZP/Al2O3) nanocomposites

A zirconia/alumina nanocomposite stabilized with cerium oxide (Ce-TZP/Al₂O₃ nanocomposite) can be a good substitute as reinforcement in metal matrix composites. In the present study, the effect of the amount of 10Ce-TZP/Al₂O₃ particles on the microstructure and properties of Al/(10Ce-TZP/Al₂O₃) nanocomposites was investigated. For this purpose, aluminum powders with average size of 30 μm were ball-milled with 10Ce-TZP/Al₂O₃ nanocomposite powders (synthesized by aqueous combustion) in varying amounts of 1, 3, 5, 7, and 10 wt.%. Cylindrical-shape samples were prepared by pressing the powders at 600 MPa for 60 min while heating at 400–450 °C. The specimens were then characterized by scanning and transmission electron microscopy (SEM and TEM) in addition to different physical and mechanical testing methods in order to establish the optimal processing conditions. The highest compression strength was obtained in the composite with 7 wt.% (10Ce-TZP/Al₂O₃) sintered at 450 °C.     

Competitive adsorption of Cu(II) and Cd(II) ions on spray-dried chitosan loaded with Reactive Orange 16

Chitosan microspheres cross-linked with glutaraldehyde and containing the reactive dye Orange 16 (RO 16) as a chelating agent were obtained by spray drying technique. These microspheres (CHS-RO 16) were characterized by FTIR, TGA, DSC, SEM and EDX analyses, and tested for metal adsorption. The new adsorbent was used in batch experiments to evaluate the adsorption of Cu(II) and Cd(II) ions in single and binary metal solutions. In single metal solutions, the maximum adsorption capacity for Cu(II), obtained by Langmuir model, was close to 1.69 mmol Cu g^? 1; this means the double of the adsorption capacity for Cd(II) (i.e. 0.80 mmol Cd g^? 1). Adsorption isotherms for binary solutions showed that the presence of Cu(II) decreased Cd(II) adsorption due to a significant competition effect. On the other hand, Cu(II) adsorption hardly changed when the initial concentration of Cd(II) increased: the new adsorbent was selective to Cu(II) against Cd(II). The metal ions were efficiently desorbed from chitosan-RO 16 with aqueous solutions of H₂SO₄.     

Removal and preconcentration of lead (II), copper (II), chromium (III) and iron (III) from wastewaters by surface developed alumina adsorbents with immobilized 1-nitroso-2-naphthol

The potential removal and preconcentration of lead (II), copper (II), chromium (III) and iron (III) from wastewaters were investigated and explored. Three new alumina adsorbents of acidic, neutral and basic nature (I–III) were synthesized via physical adsorption and surface loading of 1-nitroso-2-naphthol as a possible chelating ion-exchanger. The modified alumina adsorbents are characterized by strong thermal stability as well as resistance to acidic medium leaching processes. High metal up-take was found providing this order: Cu(II) > Cr(III) > Pb(II) owing to the strong contribution of surface loaded 1-nitroso-2-naphthol. The outlined results from the distribution coefficient and separation factor evaluations (low metal ion concentration levels) were found to denote to a different selectivity order: Pb(II) > Cu(II) > Cr(III)) due to the strong contribution of alumina matrix in the metal binding processes. The potential applications of alumina adsorbents for removal and preconcentration of Pb(II), Cu(II), Cr(III) from wastewaters as well as drinking tap water samples were successfully accomplished giving recovery values of (89–100 ± 1–3%) and (93–99 ± 3–4%), respectively without any noticeable interference of the wastewater or drinking tap water matrices.     

Umbelliprenin-coated Fe3O4 magnetite nanoparticles: Antiproliferation evaluation on human Fibrosarcoma cell line (HT-1080)

The potential applications of Fe₃O₄ magnetite nanoparticles (MNPs) in nanomedicine as drug delivery systems are well known. In this study we prepared umbelliprenin-coated Fe₃O₄ MNPs and evaluated the antiproliferative effect of combination in vitro. After synthesis of Fe₃O₄ MNPs, particles were characterized by transmission electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction spectroscopy techniques. The natural candidate compound — umbelliprenin— was isolated and identified and umbelliprenin-coated Fe₃O₄ MNPs were prepared, using precipitation method. The surface chemistry of umbelliprenin-coated Fe₃O₄ MNPs as well as their thermal decomposition characteristics was examined using Fourier transform infrared spectroscopy and Thermogravimetric Analyzer equipment, respectively. HT-1080 cells were cultured until the logarithmic phase of growth, and MTT assay was successfully carried out to evaluate the possible cytotoxic effects of umbelliprenin-coated Fe₃O₄ MNPs in viable cells in vitro. The results demonstrated that umbelliprenin has moderate antiproliferative effects with IC₅₀ value of 50 µg/mL. However, the combination of umbelliprenin and Fe₃O₄ MNPs showed the IC₅₀ value of 9 µg/mL. In other words, cell proliferation decreased to the remarkably-low proportion of 45% after treating cells with umbelliprenin-coated Fe₃O₄ MNPs. This suggests that with the aid of nanoparticles as carriers, natural products may have even broader range of medical applications in future.     

New nanocomposite based on poly(lactic-co-glycolic acid) copolymer and magnetite. Synthesis and characterization

The study presents the preparation of the new magnetic nanocomposite based on PLGA and magnetite. The PLGA used to obtain the magnetic nanocomposites was synthesized by the copolymerization of lactic acid with glycolic acid, in the presence of tin octanoate [Sn(Oct)₂] as catalyst, by polycondensation procedure. Magnetite was obtained by co-precipitation from aqueous salt solutions FeCl₂/FeCl₃. The particles size of magnetite was 420 nm, and the saturation magnetization 62.78 emu/g, while the PLGA/magnetite nanocomposite size was 864 nm and the saturation magnetization 39.44 emu/g. The magnetic nanocomposites were characterized by FT-IR, DLS technique, SEM, VSM and simultaneous thermal analyses (TG–FTIR–MS). The polymer matrix PLGA acts as a shell and carrier for the active component, while magnetite is the component which makes targeting possible by external magnetic field manipulation. Based on the gases resulted by thermal degradation of PLGA copolymer, using the simultaneous analysis TG–FTIR–MS, a possible degradation mechanism was proposed.     

High T2-relaxation and biocompatible magnetic nanofluids with poly(amino acid) coating

A facile one-pot method has been developed to prepare poly(amino acid) functionalized, water-stable, biocompatible, and superparamagnetic iron oxide nanoparticles (NPs) with small diameters of ∼10 nm. The obtained biocompatible magnetic nanoparticles capped with polyaspartic acid (PASP) exhibit a relatively high saturation magnetization (57.1 emu/g) and a much strong magnetic resonance (MR) T₂ relaxation effect with the transverse relaxivity coefficient (r₂) as high as 302.6 s⁻¹ mM⁻¹. Interestingly, the as-prepared Fe₃O₄@PASP NPs are highly stable in aqueous solution and demonstrate the property of magnetic nanofluids. The high T₂ effect, good water-stability, superparamagnetization, biocompatibility and bioconjugatability render the as-synthesized Fe₃O₄@PASP NPs great desirable for bioapplications such as magnetic resonance imaging (MRI), bioseparation, targeted drug delivery, and so on.