Study on immobilization of lipase onto magnetic microspheres with epoxy groups

Magnetic microspheres were synthesized by the suspension polymerization of glycidyl methacrylate (GMA), methacrylic acid (MAA) and divinyl benzene (DVB) in the presence of oleic acid-coated Fe₃O₄ nanoparticles. Triacylglycerol lipase from porcine pancreas was covalently immobilized on the magnetic microspheres via the active epoxy groups with the activity yield up to 63% (±2.3%) and enzyme loading of 39 (±0.5) mg/g supports. The resulting immobilized lipase had higher optimum temperature compared with those of free lipase and exhibited better thermal, broader pH stability and excellent reusability. Furthermore, the catalyzed capability of immobilized lipase was also investigated by catalyzing synthesis of hexyl acetate and the esterification conversion rate reached to 83% (±2.5%) after 12 h in nonaqueous solvent.     

Low-density core-shell composite hollow microspheres with tunable magnetic properties

Low-density (about 0.9 g/cm³) composite core-shell hollow microspheres with tunable magnetic properties were fabricated by Ni-Fe-P deposition on hollow glass microspheres (HGM) with modified electroless plating process. The effects of mole ratio of Fe²⁺/Ni²⁺, concentration of the reducer and pH value of the solution on the magnetic properties of the products were investigated. In conclusion, the increase in the mole ratio of Fe²⁺/Ni²⁺ and pH value of the solution could improve the soft magnetic properties of composite microspheres remarkably, while the increase in the concentration of NaH₂PO₂ had the opposite effect. The as-obtained metallic shells were amorphous and the crystallization got better with increased annealing temperature after plating. In addition, the saturation intensity of the composite microspheres was enhanced monotonically by increasing the annealing temperature. This work provided a facile and effective strategy to fabricate core-shell composite hollow microspheres with tailored magnetic properties.     

Superparamagnetic silica nanoparticles with immobilized metal affinity ligands for protein adsorption

Superparamagnetic silica-coated magnetite (Fe₃O₄) nanoparticles with immobilized metal affinity ligands were prepared for protein adsorption. First, magnetite nanoparticles were synthesized by co-precipitating Fe²⁺ and Fe³⁺ in an ammonia solution. Then silica was coated on the Fe₃O₄ nanoparticles using a sol–gel method to obtain magnetic silica nanoparticles. The condensation product of 3-Glycidoxypropyltrimethoxysilane (GLYMO) and iminodiacetic acid (IDA) was immobilized on them and after charged with Cu²⁺, the magnetic silica nanoparticles with immobilized Cu²⁺ were applied for the adsorption of bovine serum albumin (BSA). Scanning electron micrograph showed that the magnetic silica nanoparticles with an average size of 190 nm were well dispersed without aggregation. X-ray diffraction showed the spinel structure for the magnetite particles coated with silica. Magnetic measurement revealed the magnetic silica nanoparticles were superparamagnetic and the saturation magnetization was about 15.0 emu/g. Protein adsorption results showed that the nanoparticles had high adsorption capacity for BSA (73 mg/g) and low nonspecific adsorption. The regeneration of these nanoparticles was also studied.     

Preparation of magnetic polylactic acid microspheres and investigation of its releasing property for loading curcumin

In order to obtain a targeting drug carrier system, magnetic polylactic acid (PLA) microspheres loading curcumin were synthesized by the classical oil-in-water emulsion solvent-evaporation method. In the Fourier transform infrared spectra of microspheres, the present functional groups of PLA were all kept invariably. The morphology and size distribution of magnetic microspheres were observed with scanning electron microscopy and dynamic light scattering, respectively. The results showed that the microspheres were regularly spherical and the surface was smooth with a diameter of 0.55-0.75 μm. Magnetic Fe₃O₄ was loaded in PLA microspheres and the content of magnetic particles was 12 wt% through thermogravimetric analysis. The magnetic property of prepared microspheres was measured by vibrating sample magnetometer. The results showed that the magnetic microspheres exhibited typical superparamagnetic behavior and the saturated magnetization was 14.38 emu/g. Through analysis of differential scanning calorimetry, the curcumin was in an amorphous state in the magnetic microspheres. The drug loading, encapsulation efficiency and releasing properties of curcumin in vitro were also investigated by ultraviolet-visible spectrum analysis. The results showed that the drug loading and encapsulation efficiency were 8.0% and 24.2%, respectively. And curcumin was obviously slowly released because the cumulative release percentage of magnetic microspheres in the phosphate buffer (pH=7.4) solution was only 49.01% in 72 h, and the basic release of curcumin finished in 120 h.     

Application of bifunctional Saccharomyces cerevisiae to remove lead(II) and cadmium(II) in aqueous solution

A magnetic adsorbent, EDTAD-functionalized Saccharomyces cerevisiae, has been synthesized to behave as an adsorbent for heavy metal ions by adjusting the pH value of the aqueous solution to make carboxyl and amino groups protonic or non-protonic. The bifunctional Saccharomyces cerevisiae (EMS) were used to remove lead(II) and cadmium(II) in solution in a batch system. The results showed that the adsorption capacity of the EMS for the heavy metal ions increased with increasing solution pH, and the maximum adsorption capacity (88.16 mg/g for Pb²⁺, 40.72 mg/g for Cd²⁺) at 10 °C was found to occur at pH 5.5 and 6.0, respectively. The adsorption process followed the Langmuir isotherm model. The regeneration experiments revealed that the EMS could be successfully reused.     

Adsorption of 2,4,6-trinitrotoluene on carboxylated porous polystyrene microspheres

Large-pore-size (150 nm) polystyrene (PSt) microspheres were carboxylated with phthalic anhydride (PA) through Friedel-Crafts acetylation to study the adsorption of 2,4,6-trinitrotoluene (TNT) on this material from aqueous solution. The scanning electron microscope (SEM) images and mercury porosimetry measurements (MPM) of the microspheres showed that the pore structure was unchanged during the reaction. High adsorption capacity (11.2 mg g⁻¹ of suction-dried adsorbent) and adsorption rate (33.9 mg g⁻¹ h⁻¹) for TNT were observed during the study. As shown by the adsorption isotherm, the adsorption of TNT on PA-PSt can be described by the Freundlich adsorption equation, indicating heterogeneous adsorption process. On-column adsorption of TNT on PA-PSt and elution indicated that TNT can be completely removed from aqueous solution and condensed into acetone.     

Preparation and characterization of biodegradable magnetic carriers by single emulsion-solvent evaporation

This paper describes a single emulsion-solvent evaporation protocol to prepare PEGylated biodegradable/biocompatible magnetic carriers by utilizing hydrophobic magnetite and a mixture of poly(D,L lactide-co-glycolide) (PLGA) and poly(lactic acid-block-polyethylene glycol) (PLA-PEG) (26:1 by mass) polymers. We characterized the magnetic microspheres in terms of morphology, composite microstructure, size and size distribution, and magnetic properties. Results show that the preparation produces magnetic microspheres with a good spherical morphology, small size (mean diameter of 1.2–1.5 μm) by means of large size distributions, and magnetizations up to 20–30 emu/g of microspheres.     

Production of magnetic microspheres by ultrasonic atomisation

Magnetic microspheres, with mean particle sizes from 23 to 32 μm were produced by the ultrasonic atomisation of a suspension of magnetite particles, of approximately 200 nm diameter, in a solution of poly–l–lactic acid (PLLA). The mean particle diameter and the width of the particle diameter distribution both increased with increasing magnetite concentration. The particles appear to be suitable for magnetic hyperthermic treatment of liver cancers, with the hysteresis loop areas increasing linearly with nominal magnetite concentration up to 30 wt% magnetite.     

Magnetic properties of anisotropic Sm–Fe–N bulk magnets produced by spark plasma sintering method

Sm–Fe–N powders were consolidated into bulk materials by the spark plasma sintering (SPS) method. Although partial decomposition of the Sm₂Fe₁₇N₃ phase was noted in the magnets, the decomposition was reduced by the addition of a small amount of Zn powder to the Sm–Fe–N powder. The anisotropic Sm–Fe–N magnet obtained from a mixture of Sm–Fe–N and Zn powders exhibited a high remanence of 0.90 T with a coercivity of 0.54 MA m⁻¹.     

Adsorption of hexavalent chromium onto montmorillonite modified with hydroxyaluminum and cetyltrimethylammonium bromide

Aluminum hydroxypolycation and cetyltrimethylammonium bromide (CTMAB) were chosen to synthesize inorganic-organic pillared montmorillonite. Three different methods were employed for the intercalation. The characteristics of natural and modified montmorillonite were determined with X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), X-ray photoelectron spectrum (XPS), and zeta potential. It was found that aluminum hydroxypolycation and CTMAB had either entered the interlayer or sorbed on the external surface of the clay. Different intercalation orders can result in different structures. Batch adsorption of hexavalent chromium (Cr⁶⁺) onto modified montmorillonite was also investigated. The experimental data revealed that if aluminum hydroxypolycation was intercalated before CTMAB, the adsorption capacity was better than that of intercalated simultaneously or CTMAB pre-intercalated. The pH of the solution and environmental temperature had significant influences on the adsorption of Cr⁶⁺. The optimal pH for the removal was about 4, and the temperature of 298 K was best suitable. All adsorption processes were rapid during the first 5 min and reached equilibrium in 20 min. The adsorption kinetics can be described quite well by pseudo-second-order model. The adsorption rates of ACM, CAM and ACCOM were 3.814, 0.915, and 3.143 mg/g/min, respectively. The adsorption capacities of Cr⁶⁺ at 298 K on ACM, CAM, and ACCOM inferred from the Langmuir model were 11.970, 6.541, and 9.090 mg/g, respectively. The adsorption of Cr⁶⁺ on modified montmorillonite was mainly induced by the surface charge and the complexation reaction between CTMA⁺ and hexavalent chromium species at the edge of the clay particle.     

Comparison of O adsorption on Ni3Al (0 0 1), (0 1 1), and (1 1 1) surfaces through first-principles calculations

First-principles calculations were performed to study the properties of O adsorption on Ni₃Al (0 0 1), (0 1 1), and (1 1 1) surfaces using the Cambridge serial total package (CASTEP) code. Stable adsorption sites are identified. The atomic and electronic structures and adsorption energies are predicted. The adsorption sites for O on the Ni₃Al (0 0 1) surface are at the 2Ni–2Al fourfold hollow site, whereas O prefers to adsorb at the Ni–Al bridge site on (0 1 1) surface and 2Ni–Al threefold hollow site on (1 1 1) surface. It is found that O shows the strongest affinity for Al and the state of O is the most stabilized when O adsorbs on (0 0 1) surface, while the affinity of O for Al on (0 1 1) surface is weaker than (0 0 1) surface, and (1 1 1) surface is the weakest. The stronger O and Al affinity indicates more stable Al₂O₃ when oxidized. The experiment has shown that the oxidation resistance of single crystal superalloy in different orientations improves in the order of (1 1 1), (0 1 1), and (0 0 1) surface, suggesting that the oxidation in different crystallographic orientations may be related to the affinity of O for Al in the surface.     

Adsorption of BTSE and γ-GPS organosilanes on different microstructural regions of 7075-T6 aluminum alloy

The adsorption of bis-1,2-(triethoxysilyl)ethane (BTSE) and γ-glycidoxypropyltrimethoxysilane (γ-GPS) on mirror-polished 7075-T6 aluminum alloy was studied with an emphasis on the different microstructural regions of the alloy surface, specifically the alloy matrix and the two main types of second-phase particles, as well as how the adsorption was affected by a heating pre-treatment and by changes in the pH of the γ-GPS solution. Surface characterizations were undertaken with scanning Auger microscopy (SAM), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and time-of-flight secondary-ion mass spectrometry (TOF-SIMS). BTSE at its natural pH (4.3) adsorbed at all micro-regions of the air-oxidized surface, while γ-GPS at its natural pH (5.7) was largely ineffective. Adsorption of γ-GPS on all micro-regions was possible after adjusting the solution pH to a lower value (3.2), or by using the solution of natural pH after pre-treating the sample by heating at 200 °C for 15 min. TOF-SIMS measurements indicated that direct metal-O-Si covalent bonding occurred at each silane interface formed to the different micro-regions of the alloy surface, with Al-O-Si bonding being predominant in each case.     

Preparation of magnetic poly(methylmethacrylate–divinylbenzene–glycidylmethacrylate) microspheres by spraying suspension polymerization and their use for protein adsorption

Moderately uniform magnetic poly(methylmethacrylate–divinylbenzene–glycidylmethacrylate) microspheres (poly(MMA–DVB–GMA) microspheres) were prepared by spraying suspension copolymerization of methyl methacrylate, divinylbenzene and glycidyl methacrylate in the presence of Fe₃O₄ magnetic fluid. A protein adsorption assay indicated that these magnetic microspheres could significantly improve the capacity of protein adsorption.     

The colloidal stability and core-shell structure of magnetite nanoparticles coated with alginate

The adsorption of alginate (Alg) onto the surface of in water dispersed Fe₃O₄ nanoparticles and zeta potential of alginate-coated Fe₃O₄ nanoparticles have been investigated to optimize the colloidal stability of Alg-coated Fe₃O₄ nanoparticles. The adsorption amount of Alg increased with the decrease of adsorption pH. The zeta potential of Fe₃O₄ nanoparticles shifted to a lower value after adsorption of Alg. The lower adsorption pH was the lower zeta potential of Fe₃O₄ nanoparticles became. The Alg-coated Fe₃O₄ nanoparticles were found to be stabilized by steric and electrostatic repulsions. Those prepared at pH 6 were not stable around pH 5, and those prepared at pH 4 became unstable at pH below 3.5. Alg of M_w 45 kDa was a little bit more adsorbed onto nanoparticles surface than that of M_w 24 kDa. An average Fe₃O₄ core size of 9.3 ± 1.7 nm was found by transmission electronic microscopy. An average hydrodynamic diameter of 30-150 nm was measured by photon correlation spectroscopy. However, an average core size of 10 nm and an average hydrodynamic diameter of 38 nm were estimated from the magnetization curve of the concentrated magnetic fluids (MFs). The maximum available saturation magnetization of MFs was about 3.5 kA/m.     

Preparation and characterization of magnetic P(St-co-MAA-co-AM) microspheres

In this study, magnetic polymer-coated microspheres were prepared by the microemulsion polymerization of styrene (St), methacrylic acid (MAA), acryamide (AM) in the presence of emulsifiers with the size of 1–5 μm. The magnetic material (i.e. Fe₃O₄) coated with oleic acid used in the preparation of the microspheres was synthesized in a classical co-precipitation procedure. The morphological and magnetic properties of the microspheres were investigated by different techniques (i.e. TEM, TGA, optical microscopy, vibrating sample magnetometer). The results indicated that the magnetic microspheres were superparamagnetic, well shaped spheres, mono-dispersed with abundant functional groups on the surfaces of the magnetic microspheres and good thermal stability. The microspheres could be linked well with the avidin and FITC antibody.     

Magnetic properties of spray-formed Fe–6.5%Si and Fe–6.5%Si–1.0%Al after rolling and heat treatment

The maximum silicon content in commercial Fe–Si steels is limited to about 3.5 wt%Si, since the ductility declines sharply as this maximum is exceeded, hindering the production of thin sheets by cold/hot rolling. However, the best magnetic properties are attained at about 6.5 wt%Si, a silicon content that renders magnetostriction practically null and minimizes magnetic losses. Using spray-forming, our research group has successfully produced this type of high silicon alloy in thin sheet form by carefully controlling the many variables of the process and subsequent rolling operations. In the present study, we investigated the magnetic properties and the microstructure of spray-formed Fe–6.5 wt%Si and Fe–6.5 wt%Si–1.0 wt%Al alloys after warm rolling and heat treatment. The main cause for the brittleness of Fe–6.5 wt%Si alloy has been attributed to the B2 phase long-range ordering, which leads to premature fractures. The presence of aluminum could avoid B2 formation and improve the alloy's ductility. The binary Fe–6.5 wt% Si alloy showed the best magnetic properties, which were ascribed to a recrystallized, coarse grain size (∼500 μm; and 340 μm for the Al-containing alloy). TEM analysis showed that a well-developed B2 domain structure (about 50–300 nm in size) was formed in the binary alloy when low cooling rates are prevailing after heat treatment. This structure contributed to improve additionally the magnetic properties, but its effect was not so strong as that of the grain size. The addition of Al to the binary alloy suppressed B2 formation, as indicated by Mossbauer spectroscopy, and apparently hindered excessive grain growth, which may explain the slightly poorer magnetic properties when compared with the binary alloy.     

Thickness dependence of the magnetic properties and magnetoimpedance effect in CoFeAlO thin films

The change of the magnetic properties and magnetoimpedance effect of Co–Fe–Al–O thin films with film thicknesses 50–1200 nm has been investigated. The coercivity and the anisotropy field changed strongly with increase of film thickness, while the saturation induction almost remained unchanged. The maximum value of GMI effect obtained about 33% for a film thickness of 1200 nm.     

Preparation and characterization of hexadecyl functionalized magnetic silica nanoparticles and its application in Rhodamine 6G removal

In this paper, a new adsorbent, hexadecyl functionalized magnetic silica nanoparticles (C₁₆/SiO₂-Fe₃O₄ NPs), was prepared by a facile method. The final product was characterized by X-ray diffractometer, transmission electron microscope, Fourier transform infrared spectrometer and vibration sample magnetometer. The preparation and adsorption conditions of the adsorbent were optimized. The adsorbent prepared maintaining volume ratio of tetraethylorthosilicate to hexadecyltrimethoxysilane at 1:0.5 and their total volume at 1100 μL exhibited high adsorption capacity. The optimum pH value for the adsorption experiments was 11.00. The adsorption behavior of Rhodamine 6G onto C₁₆/SiO₂-Fe₃O₄ NPs obeyed pseudo-second-order kinetic model and Langmuir isotherm. Thermodynamic data indicated that the adsorption process was spontaneous and exothermic. The adsorption capacity of the adsorbent could reach to 35.6 mg g⁻¹, owing to the hydrophobic attraction and the enhanced electrostatic attraction. The saturation magnetization of the magnetic adsorbent was 35 emu g⁻¹, which ensured the magnetic separation after adsorption.     

Optimization of nickel adsorption from aqueous solution by using activated carbon prepared from waste apricot by chemical activation

Waste apricot supplied by Malatya apricot plant (Turkey) was activated by using chemical activation method and K₂CO₃ was chosen for this purpose. Activation temperature was varied over the temperature range of 400-900 °C and N₂ atmosphere was used with 10 °C/min heat rate. The maximum surface area (1214 m²/g) and micropore volume (0.355 cm³/g) were obtained at 900 °C, but activated carbon was predominantly microporous at 700 °C. The resulting activated carbons were used for removal of Ni(II) ions from aqueous solution and adsorption properties have been investigated under various conditions such as pH, activation temperature, adsorbent dosage and nickel concentration. Adsorption parameters were determined by using Langmuir model. Optimal condition was determined as; pH 5, 0.7 g/10 ml adsorbent dosage, 10 mg/l Ni(II) concentration and 60 min contact time. The results indicate that the effective uptake of Ni(II) ions was obtained by activating the carbon at 900 °C.     

Batch study of arsenate (V) adsorption using Akadama mud: Effect of water mineralization

Akadama mud, consisting mainly of different forms of iron and aluminum oxide minerals, was used for arsenate (V) adsorption from aqueous solutions. The adsorption process fitted the first-order kinetic equation and the Langmuir monolayer model well. The adsorption capacity, estimated by the Langmuir isotherm model, was 5.30 mg/g at 20 ± 0.5 °C. The effects of the solution properties (initial concentration of As (V), pH, temperature, and mineralization degree) on As (V) removal were investigated. Various mineralization degrees in underground water were simulated by adjusting the ionic strength of the solution or adding coexisting ions to the contaminated solution. It was found that mineralization of the water significantly influenced the arsenic adsorption. The existence of multivalent metallic cations significantly enhanced the As (V) adsorption ability, whereas competing anions such as fluoride and phosphate greatly decreased the As (V) adsorption. This result suggests that Akadama mud is more suitable for arsenic adsorption in low-level phosphate and fluoride solutions. The loaded Akadama mud could be desorbed at polar pH conditions, especially in acidic conditions, and more than 65% As (V) sorption has been achieved at pH 1.