Facile preparation of amidoxime-functionalized Fe3O4@SiO2-g-PAMAM-AO magnetic composites for enhanced adsorption of Pb(ii) and Ni(ii) from aqueous solution

In this paper, using amidoxime as a functional monomer, different generations of polyamidoxime dendrimer magnetic microspheres (Fe₃O₄@SiO₂-g-PAMAM-AO) were fabricated to adsorb Pb²⁺ and Ni²⁺ in aqueous solution. The magnetic adsorbents were characterized by FTIR, XRD, SEM, XPS, TEM, EDS, TGA and BET. The effects of different factors (such as solution pH, adsorption time, adsorption temperature, adsorbent dosage etc.) on adsorption were evaluated. Fe₃O₄@SiO₂-g-PAMAM-AO has a maximum Pb(ii) adsorption of 157.25 mg g⁻¹ (100 mg L⁻¹) at pH 5.5. Furthermore, Fe₃O₄@SiO₂-g-PAMAM-AO showed an excellent adsorption performance for the removal of Ni(ii) with a maximum adsorption capacity of 191.78 mg g⁻¹ (100 mg L⁻¹) at pH 8.0. The sorption isotherm data fitted the Freundlich isotherm model well. Adsorption kinetics analysis showed that it was best described by the pseudo-second-order rate model. Desorption experiment results showed that the adsorbent can be reused in the adsorption–desorption cycles.

In this paper, using amidoxime as a functional monomer, different generations of polyamidoxime dendrimer magnetic microspheres (Fe₃O₄@SiO₂-g-PAMAM-AO) were fabricated to adsorb Pb²⁺ and Ni²⁺ in aqueous solution.     

Removal of arsenic(v) from aqueous solutions using sulfur-doped Fe3O4 nanoparticles

In this study, magnetic sulfur-doped Fe₃O₄ nanoparticles (Fe₃O₄:S NPs) were applied as adsorbents for the removal of As(v). Fe₃O₄:S NPs were fabricated by a two-step route, which included low-temperature mixing and high-temperature sintering. The as-prepared Fe₃O₄:S NPs could effectively remove As(v) under a wide pH range of 2–10 and presented a high As(v) adsorption capacity of 58.38 mg g⁻¹, which was much better than undoped Fe₃O₄ nanoparticles (20.24 mg g⁻¹). Adsorption experiments exhibited a pseudo-second-order model of adsorption kinetics and a Langmuir isotherm model of adsorption isotherms. Additionally, the coexisting ions such as NO₃⁻, SO₄²⁻, and CO₃²⁻ had no significant effect on As(v) adsorption and the adsorbent worked well in actual smelting wastewater. XPS and FTIR spectra of Fe₃O₄:S NPs before and after As(v) adsorption showed that Fe–OH groups played a significant role in the adsorption mechanisms. Moreover, the magnetic Fe₃O₄:S NPs adsorbents after adsorption could be rapidly separated from wastewater with an external magnetic field. Therefore, Fe₃O₄:S NPs could be an ideal candidate for the removal of As(v) from water.

Magnetic Fe₃O₄:S NPs presented a much better As(v) adsorption performance than undoped Fe₃O₄ NPs due to sulfur doping.     

Synthesis of Fe3O4@PVBC–TMT nanoparticles for the efficient removal of heavy metals ions

Core–shell magnetic Fe₃O₄@PVBC–TMT (Fe₃O₄@polyvinylbenzyl chloride–trithiocyanuric acid) nanoparticles containing trithiocyanuric acid groups were fabricated and employed for the fast removal of heavy metals from an aquatic environment. The morphology, structure and properties of Fe₃O₄@PVBC–TMT nanoparticles were characterized by a series of modern analytical tools. The adsorption behavior of the Fe₃O₄@PVBC–TMT nanoparticles for heavy metals ions in aqueous solutions was investigated by batch experiments. The maximum removal capacities of the Fe₃O₄@PVBC–TMT nanoparticles toward Mn²⁺, Ni²⁺, Cu²⁺, Cd²⁺ and Pb²⁺ ions were 127.4, 146.6, 180.5, 311.5, and 528.8 mg g⁻¹, respectively. Importantly, it is found that Pb²⁺ ions can be completely and quickly removed by the Fe₃O₄@PVBC–TMT nanoparticles. The equilibrium was established within 6 min, and the removal efficiencies were found to be 99.9%, 99.8% and 99.5% for Pb²⁺ ions at the initial concentrations of 100 mg L⁻¹, 200 mg L⁻¹ and 300 mg L⁻¹, respectively. It is hoped that the core–shell magnetic Fe₃O₄@PVBC–TMT nanoparticles may find application in wastewater treatment.

Core–shell Fe₃O₄@PVBC–TMT nanoparticles were fabricated and served as a valid magnetic adsorbent for the removal of heavy metals ions.     

Sulfated zirconium oxide-decorated magnetite KCC-1 as a durable and recyclable adsorbent for the efficient removal of asphaltene from crude oil

Sulfated zirconium oxide (ZrO₂/SO₄²⁻) as a highly durable acidic reagent was immobilized on magnetite KCC-1 nanoparticles (Fe₃O₄@SiO₂/KCC-1@ZrO₂/SO₄²⁻ NPs), and the resulting hybrid was used as a highly efficient recyclable adsorbent for the adsorption and removal of asphaltene from crude oil. The presence of ZrO₂/SO₄²⁻ groups not only promotes the adsorption capacity, but also helps recycle the adsorbents without any significant efficiency loss arising from its high chemical resistance. The results showed an obvious synergistic effect between the magnetic core (Fe₃O₄ NPs), fibrous silica (KCC-1) and the sulfated zirconium oxide groups with high correlation for asphaltene adsorption. The effective parameters in asphaltene adsorption, including initial asphaltene concentration, catalyst concentration and temperature, were investigated. Maximum adsorption occurred in the presence of 0.7 g L⁻¹ of the adsorbent, at a concentration of 2000 mg L⁻¹ of asphaltene. The asphaltene adsorption by NPs follows a quasi-second order adsorption kinetics. Asphaltene adsorption kinetics were studied by Langmuir, Freundlich, and Temkin isotherms. The prominent advantage of the adsorbent is its ability to be recovered after each adsorption by acid treatment, so that no significant reduction in adsorbent adsorption activity was observed, which can be directly attributed to the presence of ZrO₂/SO₄²⁻ groups in the hybrid.

A new, efficient and recyclable hybrid based on immobilized sulfated zirconium oxide on magnetite fibrous silica (KCC-1) has been developed and utilized for the efficient adsorption and removal of asphaltene from crude oil.     

Fabrication of a novel magnetic metal–organic framework functionalized with 2-aminothiophenol for preconcentration of trace silver amounts in water and wastewater

Herein, a novel magnetic metal–organic framework functionalized (MMOF) with 2-aminothiophenol (2-ATP) was fabricated and employed for separation/preconcentration of trace silver amounts. At first magnetite nanoparticles (Fe₃O₄ NPs) were synthesized and then coated with SiO₂. Thereafter, the Fe₃O₄@SiO₂ nanoparticles were modified with 2-ATP. Finally, the functionalized MMOF was prepared by the fabrication of MIL-101(Cr) in the presence of Fe₃O₄@SiO₂@2-ATP NPs. MIL-101(Cr)/Fe₃O₄@SiO₂@2-ATP nanocomposite was characterized with FT-IR, SEM, elemental analysis, XRD and VSM and then utilized in the separation/determination of silver ions in various real samples. The effects of diverse experimental variables such as pH, uptake time, adsorbent amount, desorption time, eluent concentration and volume were studied comprehensively employing experimental design methodology. After optimization, LOD and linearity were 0.05 ng mL⁻¹ and 0.2–200 ng mL⁻¹, respectively. Repeatability of the new method was determined based on RSD value for 5, 50, 150 ng mL⁻¹ (n = 5) concentrations which was 9.3%, 6.8% and 4.5%, respectively. Ultimately, the outlined method was utilized in the separation/determination of silver ions in various water and wastewater samples satisfactorily.

A scheme for the synthesis of MIL-101/Fe₃O₄@SiO₂@2-ATP nanocomposite.     

Acetylacetone functionalized magnetic carbon microspheres for the highly-efficient adsorption of heavy metal ions from aqueous solutions

Herein, Acac-C@Fe₃O₄, a magnetic carbon (C@Fe₃O₄) modified with acetylacetone (Acac), was first prepared and used as a solid-phase adsorbent for adsorbing some heavy metal ions from aqueous solution. The adsorbent was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometry (VSM) and BET studies. Some parameters affecting the adsorption and desorption processes were studied in Pb²⁺ solution, including sample pH, contact time, initial concentration, type and connection of the desorption solution. Absorption results showed that removal of Pb²⁺ was 100% under optimal conditions at an initial concentration of 10.0 mg L⁻¹. The adsorption mechanism conformed well to a pseudo-second order kinetic model. The adsorption capacity of the sorbent also showed promising results with Hg²⁺, Cr³⁺, Fe²⁺, Cd²⁺, Mn²⁺, Zn²⁺, Cu²⁺ and Pb²⁺, where maximum adsorption capacities reached 98.0, 151.2, 188.9, 202.2, 286.3, 297.2, 305.1 and 345.3 mg g⁻¹, respectively. The Acac-C@Fe₃O₄ microsphere material was successfully applied to the adsorption of heavy metal ions in aqueous solution.

Herein, Acac-C@Fe₃O₄, a magnetic carbon (C@Fe₃O₄) modified with acetylacetone (Acac), was first prepared and used as a solid-phase adsorbent for adsorbing some heavy metal ions from aqueous solution.     

Selective aptamer conjugation to silver-coated magnetite nanoparticles for magnetic solid-phase extraction of trace amounts of Pb2+ ions

Herein, a novel aptamer-functionalized magnetic adsorbent was developed and combined with magnetic solid-phase extraction (MSPE) for the specific enrichment of Pb²⁺ ions prior to flame atomic absorption spectrometric detection. First, silver-coated magnetite core–shell nanoparticles (Fe₃O₄@Ag MNPs) were synthesized by the chemical reduction of silver ions on the surface of magnetite nanoparticles. After that, the selective DNA aptamer against Pb²⁺ was conjugated on the surface of the synthesized nanoparticles to form aptamer-modified magnetic nanoparticles (Fe₃O₄@Ag-APT). The characterization of the prepared adsorbent was performed through SEM imaging, XRD, FT-IR, EDX, and DRS instruments. The influence of the various experimental parameters on the adsorption and desorption steps in MSPE was investigated via Taguchi experimental design to optimize different parameters. Under the optimized conditions, the Pb²⁺ calibration graph was linear in the range of 33–1000 μg L⁻¹. The relative standard deviation (RSD%) of the method for six replicates containing 100 μg L⁻¹ of Pb²⁺ ions was 0.34%. Furthermore, the limit of detection (LOD) and the limit of quantification (LOQ) were 10 μg L⁻¹ and 33.3 μg L⁻¹, respectively. Finally, the applicability of the proposed method was successfully confirmed by preconcentration and determination of trace amounts of Pb²⁺ ions in tap and seawater samples. We showed a proof of concept for Fe₃O₄@Ag-APT as an efficient bio-adsorbent, offering a promising strategy for the specific binding/removal of toxic heavy metal ions.

Herein, a novel aptamer-functionalized magnetic adsorbent was developed and combined with magnetic solid-phase extraction (MSPE) for the specific enrichment of Pb²⁺ ions prior to flame atomic absorption spectrometric detection.     

Adsorption mechanism of polyethyleneimine modified magnetic core–shell Fe3O4@SiO2 nanoparticles for anionic dye removal

In this paper, polyethyleneimine modified magnetic core–shell Fe₃O₄@SiO₂ nanoparticles (Fe₃O₄@SiO₂/PEI) were innovatively synthesized and investigated using various techniques such as TEM, TGA, FT-IR, XRD, VSM and XPS. The adsorption performance based on the removal of the anionic dyes Methyl orange and Congo red from aqueous solution was studied systematically. The results showed that the adsorption rate of anionic dyes MO and CR increased rapidly then decreased gradually as the pH increased, the adsorption capacity of Fe₃O₄@SiO₂/PEI for MO was better than that for CR, and the maximum adsorption capacity for MO and CR was 231.0 mg g⁻¹ at pH 4 and 134.6 mg g⁻¹ at pH 6, respectively. The equilibrium adsorption capacities for MO and CR increased rapidly in the initial 40 min, and reached equilibrium in approximately 180 min, while the adsorption capacity for MB was relative low even negligible, demonstrating the strong adsorptive affinity of Fe₃O₄@SiO₂/PEI toward anionic compounds. Both of the adsorption processes followed the pseudo-second-order kinetics model and the Freundlich isotherm model. The mechanism of adsorption was mainly related to electrostatic attraction and the number of active sites occupied by anionic dyes. This study provides valuable guidance and is an effective method for the removal of anionic dyes from aquatic environments.

In this paper, polyethyleneimine modified magnetic core–shell Fe₃O₄@SiO₂ nanoparticles (Fe₃O₄@SiO₂/PEI) were innovatively synthesized and investigated using various techniques such as TEM, TGA, FT-IR, XRD, VSM and XPS.     

MoS42− intercalated NiFeTi LDH as an efficient and selective adsorbent for elimination of heavy metals

The enormous increase of heavy metal pollution has led to a rise in demand for synthesizing efficient and stable adsorbents for its treatment. Therefore, we have designed a novel adsorbent by introducing (MoS₄)²⁻ moieties within the layers of NiFeTi LDH-NO₃, via an ion exchange mechanism, as a stable and efficient adsorbent to deal with the increasing water pollution due to heavy metals. Characterization techniques such as XRD, FTIR, TGA, SEM, TEM, and Raman spectroscopy were used to confirm the formation of (MoS₄)²⁻ intercalated NiFeTi LDH and structural changes after the adsorption process. The efficiency of the material was tested with six heavy metal ions, among which it was found to be effective for toxic Pb²⁺ and Ag⁺ ions. When selectivity was studied with all six of the metal ions copresent in one solution, the material showed greater selectivity for Pb²⁺ and Ag⁺ ions with the selectivity order of Ni²⁺ < Cu²⁺ < Zn²⁺ < Fe³⁺ < Pb²⁺ < Ag⁺, with great adsorption capacities of 653 mg g⁻¹ for Pb²⁺ and 856 mg g⁻¹ for Ag⁺ metal ions. Further, the kinetics adsorption study for both the metal ions had a great correlation with the pseudo-second-order model and supported the chemisorption process via the formation of M–S bonding. The adsorption process obeyed the Langmuir model. Therefore, the MoS₄-LDH material could be a promising adsorbent for the removal of heavy metals.

Elimination of the heavy metals by using the MoS₄-LDH adsorbent.     

Zn2+ removal from the aqueous environment using a polydopamine/hydroxyapatite/Fe3O4 magnetic composite under ultrasonic waves

In this study, an easily magnetically recoverable polydopamine (PDA)-modified hydroxyapatite (HAp)/Fe₃O₄ magnetic composite (HAp/Fe₃O₄/PDA) was suitably synthesized to exploit its adsorption capacity to remove Zn²⁺ from aqueous solution, and its structural properties were thoroughly examined using different analytical techniques. The effect of multiple parameters like pH, ultrasonic power, ultrasonic time, adsorbent dose, and initial Zn²⁺ concentration on the adsorption efficiency was assessed using RSM-CCD. According to the acquired results, by increasing the adsorbent quantity, ultrasonic power, ultrasonic time, and pH, the Zn²⁺ adsorption efficiency increased and the interaction between the variables of ultrasonic power/Zn²⁺ concentration, pH/Zn²⁺ concentration, pH/absorbent dose, and ultrasonic time/adsorbent dose has a vital role in the Zn²⁺ adsorption. The uptake process of Zn²⁺ onto PDA/HAp/Fe₃O₄ followed Freundlich and pseudo-second order kinetic models. The maximum capacity of Zn²⁺ adsorption (q_m) obtained by PDA/HAp/Fe₃O₄, HAp/Fe₃O₄, and HAp was determined as 46.37 mg g⁻¹, 40.07 mg g⁻¹, and 37.57 mg g⁻¹, respectively. Due to its good performance and recoverability (ten times), the HAp/Fe₃O₄/PDA magnetic composite can be proposed as a good candidate to eliminate Zn²⁺ ions from a water solution.

A magnetically recoverable polydopamine (PDA)-modified hydroxyapatite (HAp)/Fe₃O₄ magnetic composite (HAp/Fe₃O₄/PDA) was synthesized to exploit its adsorption capacity to remove Zn²⁺ from aqueous solution and the structural properties were examined.     

Novel easily separable core–shell Fe3O4/PVP/ZIF-8 nanostructure adsorbent: optimization of phosphorus removal from Fosfomycin pharmaceutical wastewater

A new easily separable core–shell Fe₃O₄/PVP/ZIF-8 nanostructure adsorbent was synthesized and then examined for removal of Fosfomycin antibiotic from synthetic pharmaceutical wastewater. The removal process of Fosfomycin was expressed through testing the total phosphorus (TP). A response surface model (RSM) for Fosfomycin adsorption (as mg-P L⁻¹) was used by carrying out the experiments using a central composite design. The adsorption model showed that Fosfomycin adsorption is directly proportional to core–shell Fe₃O₄/PVP/ZIF-8 nanostructure adsorbent dosage and time, and indirectly to initial Fosfomycin concentration. The removal increased by decreasing the pH to 2. The Fosfomycin removal was done at room temperature under an orbital agitation speed of 250 rpm. The adsorption capacity of core–shell Fe₃O₄/PVP/ZIF-8 nanostructure adsorbent reached around 1200 mg-P g⁻¹, which is significantly higher than other MOF adsorbents reported in the literature. The maximum Langmuir adsorption capacity of the adsorbent for Fosfomycin was 126.58 mg g⁻¹ and Fosfomycin adsorption behavior followed the Freundlich isotherm (R² = 0.9505) in the present study. The kinetics was best fitted by the pseudo-second-order model (R² = 0.9764). The RSM model was used for the adsorption process in different target modes.

The synthesis of an easily separable novel core–shell Fe₃O₄/PVP/ZIF-8 nanostructure adsorbent and its usage for Fosfomycin pharmaceutical wastewater treatment.     

Fe3O4@SiO2@Au nanoparticles for MRI-guided chemo/NIR photothermal therapy of cancer cells

Novel functionalized (biofunctionalization followed by cisplatin immobilization) Fe₃O₄@SiO₂@Au nanoparticles (NPs) were designed. The encapsulation of Fe₃O₄ cores inside continuous SiO₂ shells preserves their initial structure and strong magnetic properties, while the shell surface can be decorated by small Au NPs, and then cisplatin (cPt) can be successfully immobilized on their surface. The fabricated NPs exhibit very strong T₂ contrasting properties for magnetic resonance imaging (MRI). The functionalized Fe₃O₄@SiO₂@Au NPs are tested for a potential application in photothermal cancer therapy, which is simulated by irradiation of two colon cancer cell lines (SW480 and SW620) with a laser (λ = 808 nm, W = 100 mW cm⁻²). It is found that the functionalized NPs possess low toxicity towards cancer cells (∼10–15%), which however could be drastically increased by laser irradiation, leading to a mortality of the cells of ∼43–50%. This increase of the cytotoxic properties of the Fe₃O₄@SiO₂@Au NPs, due to the synergic effect between the presence of cPt plus Au NPs and laser irradiation, makes these NPs perspective agents for potential (MRI)-guided stimulated chemo-photothermal treatment of cancer.

Novel functionalized nanoparticles, with toxicity controlled by laser irradiation, are perspective agents for potential (MRI)-guided stimulated chemo-photothermal treatment of cancer.     

Microwave assisted green synthesis of Fe2O3/biochar for ultrasonic removal of nonsteroidal anti-inflammatory pharmaceuticals

Iron oxide/biochar (Fe₂O₃/biochar) was prepared by green synthesis via a microwave to evaluate ultrasound-assisted adsorption capacity of Nonsteroidal Anti-inflammatory Drugs (NSAIDs) (salicylic acid, naproxen, and ketoprofen) from the water. Several techniques of characterization, including, Fourier transform infrared spectrometry, scanning electron microscopy, EDS analysis, N₂ adsorption–desorption, X-ray diffraction, and Raman spectrometry were applied. The adsorption of NSAIDs onto Fe₂O₃/biochar was performed using an ultrasonic bath. The effects of batch adsorption under various experimental parameters such as contact time (0–120 min), initial concentration (10–500 mg L⁻¹) and pH (2–12) were tested. The obtained Fe₂O₃/biochar specific surface area, mesopore volume/micropore volume, and pores size were equal to 786 m² g⁻¹, 0.409 cm³ g⁻¹, and 1.534 cm³ g⁻¹, respectively. The pseudo-second-order model could describe better all NSAID adsorptions onto Fe₂O₃/biochar. The Langmuir model agreed well with the NSAID adsorptions and the maximum adsorption capacities reached 683 mg g⁻¹, 533 mg g⁻¹ and 444 mg g⁻¹ for salicylic acid, naproxen, and ketoprofen, respectively. Fe₂O₃/biochar can be used as an excellent adsorbent for the treatment of NSAIDs in water.

Here, we have developed a simple and green microwave synthesis of iron oxide/biochar for the removal of new emergent pharmaceutical pollutants.     

Preparation,characterization serpentine-loaded hydroxyapatite and its simultaneous removal performance for fluoride,iron and manganese

Aiming at the problem of excessive fluorine, iron, and manganese pollution in groundwater in mining areas, a serpentine-loaded hydroxyapatite (Srp/HAP) composite adsorbent was prepared by wet chemical coprecipitation. The preparation conditions of the Srp/HAP composite adsorbent were explored, Srp/HAP was microscopically characterized, and the adsorption performance and adsorption mechanism of the Srp/HAP composite adsorbent for F⁻, Fe²⁺ and Mn²⁺ were analyzed. The results showed that the optimal preparation conditions for the composite particles were as follows: solid–liquid ratio of Srp to calcium nitrate solution 20%, aging time 20 h, calcination temperature 180 °C, and calcination time 90 min. Compact Srp/HAP composite adsorbent particles were successfully prepared, and both the lamellar crimp structure of the Srp surface and the problem of HAP surface agglomeration were resolved. After loading, the specific surface area and pore volume of the particles significantly increased, and the surface pore structure improved, which is conducive to the simultaneous adsorption and removal of fluorine, iron and manganese. The optimal reaction conditions for Srp/HAP treatment of composite water samples with F⁻, Fe²⁺ and Mn²⁺ mass concentrations of 5 mg L⁻¹, 20 mg L⁻¹ and 5 mg L⁻¹, respectively, are as follows: dosage of Srp/HAP 3 g L⁻¹, pH 7, temperature 35 °C, and reaction time 150 min. Under these conditions, the removal rates of F⁻, Fe²⁺ and Mn²⁺ were 98.6%, 99.9% and 99.8%, respectively. The quasi-second-order kinetic model and Langmuir isothermal adsorption model described the adsorption process of F⁻, Fe²⁺ and Mn²⁺ by the composite particles well. The adsorption process includes both surface physical adsorption and chemical adsorption. Chemical adsorption is mainly characterized by ion exchange and surface complexation. The Srp/HAP composite particles can be used as an excellent adsorbent for the treatment of groundwater containing fluorine, iron and manganese ions in mining areas.

A new adsorbent Srp/HAP for simultaneous removal of fluoride, iron and manganese was prepared, characterized and analyzed.     

Computer-aided design of magnetic molecularly imprinted polymer nanoparticles for solid-phase extraction and determination of levetiracetam in human plasma

Analytical methods should be accurate and specific to measure plasma drug concentration. Nevertheless, current sample preparation techniques suffer from limitations, including matrix interference and intensive sample preparation. In this study, a novel technique was proposed for the synthesis of a molecularly imprinted polymer (MIP) on magnetic Fe₃O₄ nanoparticles (NPs) with uniform core–shell structure. The Fe₃O₄@MIPs NPs were then applied to separate and enrich an antiepileptic drug, levetiracetam, from human plasma. A computational approach was developed to screen the functional monomers and polymerization solvents to provide a suitable design for the synthesized MIP. Different analysis techniques and re-binding experiments were performed to characterize the Fe₃O₄@MIP NPs, as well as to identify optimal conditions for the extraction process. Adsorption isotherms were best fitted to the Langmuir model and adsorption kinetics were modeled with pseudo-second-order kinetics. The Fe₃O₄@MIP NPs showed reasonable adsorption capacity and improved imprinting efficiency. A validated colorimetric assay was introduced as a comparable method to a validated HPLC assay for the quantitation of levetiracetam in plasma in the range of 10–80 μg mL⁻¹ after extraction. The results from the HPLC and colorimetric assays showed good precision (between 1.08% and 9.87%) and recoveries (between 94% and 106%) using the Fe₃O₄@MIP NPs. The limit of detection and limit of quantification were estimated to be 2.58 μg mL⁻¹ and 7.81 μg mL⁻¹, respectively for HPLC assay and 2.32 μg mL⁻¹ and 7.02 μg mL⁻¹, respectively for colorimetric assay. It is believed that synthesized Fe₃O₄@MIP NPs as a sample clean-up technique combined with the proposed assays can be used for determination of levetiracetam in plasma.

A novel molecularly imprinted polymer on Fe₃O₄ nanoparticles was applied to extract antiepileptic drug; levetiracetam from plasma for TDM purposes.     

Development of a new efficient and economical magnetic sorbent silicone surfactant-based activated carbon for the removal of chloro- and nitro-group phenolic compounds from contaminated water samples

In this study, activated carbon (AC) coated with a green silicone surfactant (SS) was further incorporated with magnetite particles (Fe₃O₄) via a co-precipitation method to enhance the separation of the newly designed magnetic AC–SS (Fe₃O₄@AC–SS) in a magnetic field. The properties of this magnetic adsorbent were characterized via Fourier transform-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray diffraction (XRD), and transmission electron microscopy (TEM). The adsorption characteristics of the Fe₃O₄@AC–SS adsorbent were examined using 2,4-nitrophenol and 2,4-dichlorophenol as adsorbates. Experiments were performed to investigate the adsorption kinetics, isotherms, thermodynamics as well as the effects of adsorption dosage and solution pH on the removal of both analytes. The kinetic data were well-fitted by the pseudo-second order model and the Freundlich model best described the adsorption isotherm for both analytes. The maximum adsorption capabilities for 2,4-dinitrophenol and 2,4-dichlorophenol reached 43 and 98 mg g⁻¹, respectively. The analysis was further validated using real industrial effluent, and a removal efficiency of 62.2–98.1% and relative standard deviation value less than 7.2% were attained for both analytes. Thus, the multifunctional adsorbent has potential to function as an adsorbent for the fast, convenient, economical and highly efficient removal of pollutants from wastewater, which is significant for the purification of natural water and industrial effluent.

In this study, activated carbon (AC) coated with a green silicone surfactant (SS) was further incorporated with magnetite particles (Fe₃O₄) to enhance the separation of the newly designed magnetic AC–SS (Fe₃O₄@AC–SS) in a magnetic field.     

A physical approach for the estimation of the SERS enhancement factor through the enrichment and separation of target molecules using magnetic adsorbents

The controllable synthesis of nanosized Fe₃O₄ (10–20 nm) encapsulated in different numbers of graphene layers (1–5 layers) (Fe₃O₄@DGL NPs) was realized through a facile and green hydrothermal reaction at a temperature as low as 200 °C. The competitive reduction–oxidation between reducing ethylene glycol (EG) and oxidizing H₂O under hydrothermal conditions resulted in the emergence of a magnetic Fe₃O₄ core. Then, the pyrolytic reaction of the polyvinyl alcohol (PVA) molecules attached to the surface of the Fe₃O₄ core with different surface densities led to the formation of graphene with a controlled number of layers. These Fe₃O₄@DGL NPs exhibited fast adsorption and sensitive SERS detection for rhodamine B (RhB). A physical and mathematical model was proposed for the estimation of the enhancement factor (EF) by combining the adsorption efficiency and SERS of RhB. This approach and model are applicable for the adsorption, sensitive SERS detection and determination of SERS EF when using functional magnetic nanoparticles as the adsorbent. The Fe₃O₄@1G NPs were also used as a novel nano-adsorbent for the fast removal of Escherichia coli (E. coli) from an aqueous solution. The Fe₃O₄@1G NPs regenerated after 3 cycles also showed high efficiency in the adsorption and separation of RhB and E. coli.

The controllable synthesis of nanosized Fe₃O₄ (10–20 nm) encapsulated in different numbers of graphene layers (1–5 layers) (Fe₃O₄@DGL NPs) was realized through a facile and green hydrothermal reaction at a temperature as low as 200 °C.     

Dual role of coal fly ash in copper ion adsorption followed by thermal stabilization in a spinel solid solution

Coal fly ash is usually used as a cost-effective adsorbent for heavy metal removal, accumulating large amounts of spent coal fly ash that requires further disposal. In this study, fly ash that adsorbs copper with a maximum copper adsorption capacity of 48.8 mg g⁻¹ was further sintered at 900–1050 °C, and it was found that the copper is thermally incorporated in a spinel structure in aluminum- and iron-containing ceramic matrices provided by the fly ash. To further explore the immobilization mechanisms of copper in both aluminum- and iron-containing ceramic matrices like those in fly ash, two systems were prepared from CuO + Fe₂O₃ + kaolinite and CuO + Fe₂O₃ + Al₂O₃. A CuAl_xFe_2−xO₄ spinel solid solution was formed, the peak intensity of which was found to increase upon an increase in the sintering temperature until a maximum amount was reached at 1150 °C. In the CuO + Fe₂O₃ + Al₂O₃ system, the 2θ value of the CuAl_xFe_2−xO₄ peaks was found to increase due to the continuous engagement of aluminum in the spinel structure. However, iron was found to be more likely to react with the copper in CuO + Fe₂O₃ + kaolinite during the formation of CuAl_xFe_2−xO₄. Through effective adsorption of copper on coal fly ash and the subsequent copper stabilization in the spinel, this study found a dual role for fly ash in copper immobilization and further confirmed the potential to recycle waste coal fly ash as a marketable ceramic material.

Coal fly ash is usually used as a cost-effective adsorbent for heavy metal removal, accumulating large amounts of spent coal fly ash that requires further disposal.     

Super rapid removal of copper,cadmium and lead ions from water by NTA-silica gel

Copper (Cu²⁺), cadmium (Cd²⁺) and lead ions (Pb²⁺) are toxic to human beings and other organisms. In this study, a silica gel material modified with nitrilotriacetic acid (NTA-silica gel) was sensibly designed and prepared via a simple amidation procedure for the removal of Cu²⁺, Cd²⁺ and Pb²⁺ from water. The NTA-silica gels showed rapid removal performances for the three metal ions (Pb²⁺ (<2 min), Cu²⁺ and Cd²⁺ (<20 min)) with relatively high adsorption capacities (63.5, 53.14 and 76.22 mg g⁻¹ for Cu²⁺, Cd²⁺ and Pb²⁺, respectively). At the same concentration of 20 mg L⁻¹, the removal efficiencies of the three metals by the adsorbent ranged from 96% to 99%. The Freundlich and Langmuir models were utilized to fit the adsorption isotherms. The adsorption kinetics for the three metal ions was pseudo-second-order kinetics. The removal performance of the NTA-silica gels increased in a wide pH range (2–9) and maintained in the presence of competitive metal ions (Na⁺, Mg²⁺, Ca²⁺ and Al³⁺) with different concentrations. In addition, the NTA-silica gels were easily regenerated (washed with 1% HNO₃) and reused for 5 cycles with high adsorption capacity. This study indicates that the NTA-silica gel is a reusable adsorbent for the rapid, convenient, and efficient removal of Cu²⁺, Cd²⁺, and Pb²⁺ from contaminated aquatic environments.

A silica gel material modified with nitrilotriacetic acid (NTA-silica gel) was sensibly designed and prepared via a simple method for the super rapid removal of Cu²⁺, Cd²⁺ and Pb²⁺ from water.     

Design and controllable synthesis of ethylenediamine-grafted ion imprinted magnetic polymers for highly selective adsorption to perchlorate

A series of ethylenediamine-grafted ion imprinted magnetic polymers (Fe₃O₄@IIPs) were synthesized via ultrasonic assisted suspension polymerization with perchlorate (ClO₄⁻) as an ion imprinting template. They were characterized by XRD, EA, VSM, FTIR and XPS and applied as adsorbents for ClO₄⁻ removal from aqueous solutions. The effects of the usage amount of crosslinking agent divinylbenzene (DVB) used for preparation on the structure and the adsorptive performance of Fe₃O₄@IIPs were investigated. The results show that the Fe₃O₄@IIPs have an average size of 200–800 nm, which increases with the increase of the amount of DVB from 0 to 2 g during the preparation process. The saturation magnetization intensities are at 35.6–42.8 emu g⁻¹, which decrease with the increase of the usage amount of DVB. The addition of DVB is beneficial to the formation and stability of the ion imprinted cavity of Fe₃O₄@IIPs. The effects of the solution pH value, initial concentration of ClO₄⁻, and adsorption time on the adsorption properties of ClO₄⁻ in aqueous solutions were investigated. The results show that the adsorption capability is affected significantly by solution pH value and reaches the maximum adsorption capacity at pH 3.0. The best adsorption capacity and selectivity of Fe₃O₄@IIPs to ClO₄⁻ can be obtained when the usage amount of DVB is at 0.5 g for synthesis. The adsorption mechanisms might include both ion exchange and electrostatic interaction. The isothermal adsorption curves mainly obey the Langmuir model with the theoretical maximum adsorption capacities (q_m,c) at 76.92–111.1 mg g⁻¹ and the experimental maximum adsorption capacities (q_m,e) at 75.7–108.9 mg g⁻¹, respectively, which are much higher than those of the non-ion imprinted material (Fe₃O₄@NIP, q_m,NIP: q_m,c at 60.61 mg g⁻¹ and q_m,e at 59.0 mg g⁻¹). The adsorption kinetic studies show that the adsorption processes reach equilibrium within 10 min and the kinetic data are well fitted to the pseudo-second-order model. There is almost no interference by the coexisting anions for the selective adsorption of ClO₄⁻, with a imprinting factor (α) at 1.8, and selectivity factor (β) larger than 5.9 for several kinds of common co-existing anions, respectively. The Fe₃O₄@IIPs are ideal candidates for removal of ClO₄⁻ from aqueous solution.

A series of ethylenediamine-grafted ion imprinted magnetic polymers (Fe₃O₄@IIPs) were synthesized via ultrasonic assisted suspension polymerization with perchlorate (ClO₄⁻) as an ion imprinting template.