The application of magnetized graphene (G) layers synthesized on the carbon nanofibers (CNFs) (m-G/CNF) was investigated as novel adsorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in water samples followed by gas chromatography-flame ionization detector (GC-FID). Six important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 5min for extraction time, 20mg for sorbent amount, dichloromethane as desorption solvent, 1mL for desorption solvent volume, 5min for desorption time and 15% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. The calibration curves were linear over the concentration ranges from 0.012 to 100ngmL(-1) with correlation coefficients (r) between 0.9950 and 0.9967 for all the analytes. The limits of detection (LODs, S/N=3) of the proposed method for the studied PAHs were 0.004-0.03ngmL(-1). The relative standard deviations (RSDs) for five replicates at two concentration levels (0.1 and 50ngmL(-1)) of PAHs were ranged from 3.4 to 5.7%. Appropriate relative recovery values, in the range of 95.5-99.9%, were also obtained for the real water sample analysis.
Co(II)-Ti(IV)-substituted magnetoplumbite-type (M-type) barium ferrite nanoparticles were synthesized via the sol-gel technique employing ethylene glycol as the gel precursor. Structural and magnetic properties were characterised via X-ray diffraction (XRD), high resolution transmission electron microscopy and superconducting quantum interference device magnetometry. The particle sizes of the M-type BaCoXTiXFe12-2XO19 (0.2 ≤ ≤ 1.0) were found to be 900 Å – 1500 Å. The XRD results confirmed that the Co(II)-Ti(IV) substituted ferrites in the range of 0.2 ≤ ≤ 1.0 substitution had the M-type ferrite as the dominant phase. The hysteresis loss per-cycle decreased with increasing Co(II)-Ti(IV) substitution in M-type ferrites which showed reduced values in coercivity and remnant magnetisation with moderate effect on the saturation magnetisation.
Lanthanum substituted Ni-Zn ferrite nanoparticles (Ni0.5Zn0.5LaxFe1-xO4; 0.00 ≤x≤ 1.00) synthesized by sol-gel method were presented. X-ray diffraction patterns reveal the typical single phase spinel cubic ferrite structure, with the traces of secondary phase for lanthanum substituted nanocrystals. In addition, the structural analysis also demonstrates that the average crystallite size varied in the range of 21-25 nm. FTIR spectra present the two prominent absorption bands in the range of 400 to 600 cm-1 which are the fingerprint region of all ferrites. Surface morphology of both substituted and unsubstituted Ni-Zn ferrite nanoparticle samples was studied using FESEM technique and it indicates a significant increase in the size of spherical shaped particles with La3+ substitution. Magnetic properties of all samples were analyzed using vibrating sample magnetometer (VSM). The results revealed that saturation magnetization (Ms) and coercivity (Hc) of La3+ substituted samples has decreased as compared to the Ni-Zn ferrite samples. Hence, the observed results affirm that the lanthanum ion substitution has greatly influenced the structural, morphology and magnetic properties of Ni-Zn ferrite nanoparticles.
The magnetic adsorbents i.e. oil palm frond-magnetic particles (OPF-MP) and oil palm frond activated carbon-magnetic particles (OPFAC-MP) have been prepared by impregnation of iron oxide via co-precipitation method. The magnetic adsorbents and their parent materials were characterized using Fourier transform infrared (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), Brunauer Emmett Teller (BET), Barrett, Joyner & Halenda (BJH) and t-plot method, x-ray diffraction (XRD) and also using vibrating sample magnetometry (VSM) to study their properties and surface chemistry. The activated carbon magnetic adsorbent confers high surface area of 700 m2/g with amorphous structure and magnetic properties of 2.76 emu/g. The OPF-MP and OPFAC-MP were then applied in adsorption study for ions removal of Pb(II), Zn(II) and Cu(II). OPFAC-MP has shown high removal efficiency of 100 % with adsorption capacity up to 15 mg/g of Pb(II), Zn(II) and Cu(II) ions compared to OPF-MP. In addition, the magnetic adsorbents were also compared with their parent materials to observe the effect of magnetic particles. Accordingly, the impregnation of magnetic particles enhances the metal ions adsorption comparing to their parent materials.
This work describes the development of a new methodology based on magnetic nanoparticles assisted dispersive liquid-liquid microextraction (DLLME-MNPs) for preconcentration and extraction of chloramphenicol (CAP) antibiotic residues in water. The approach is based on the use of decanoic acid as the extraction solvent followed by the application of MNPs to magnetically retrieve the extraction solvent containing the extracted CAP. The coated MNPs were then desorbed with methanol, and the clean extract was analysed using ultraviolet-visible spectrophotometry. Several important parameters, such as the amount of decanoic acid, extraction time, stirring rate, amount of MNPs, type of desorption solvent, salt addition and sample pH, were evaluated and optimized. Optimum parameters were as follows: amount of decanoic acid: 200 mg; extraction time: 10 min; stirring rate: 800 rpm; amount of MNPs: 60 mg; desorption solvent: methanol; salt: 10%; and sample pH, 8. Under the optimum conditions, the method demonstrated acceptable linearity (R2 = 0.9933) over a concentration range of 50-1000 µg l-1. Limit of detection and limit of quantification were 16.5 and 50.0 µg l-1, respectively. Good analyte recovery (91-92.7%) and acceptable precision with good relative standard deviations (0.45-6.29%, n = 3) were obtained. The method was successfully applied to tap water and lake water samples. The proposed method is rapid, simple, reliable and environmentally friendly for the detection of CAP.
In this present study, magnetic nanoparticles (MNPs) nanocomposites modified with polyaniline (PANI) coated newly synthesised dicationic ionic liquid (DICAT) forming MNP-PANI-DICAT were successfully synthesised as new generation material for magnetic solid phase extraction (MSPE). MNP-PANI-DICAT was characterised by FT-IR NMR, CHN, BET, SEM, TEM, and VSM techniques and the results were compared with MNP-PANI and native MNP. This new material was applied as a magnetic adsorbent for the pre-concentration and separation of polycyclic aromatic hydrocarbons (PAHs) due to the π-π interaction between polyaniline shell and dicationic ionic liquid (DICAT) with PAHs compounds. Under the optimal conditions, the proposed method was evaluated and applied for the analysis of PAHs in environmental samples using gas chromatography-mass spectrometry (GC-MS). The validation method showed good linearity (0.005-500µgL-1) with the coefficient of determination (R2) > 0.999. The limits of detection (LOD) and quantification (LOQ) of the developed method (MNP-PANI-DICAT-MSPE) were in the range of 0.0008-0.2086µgL-1and 0.0024-0.6320µgL-1, respectively. The enrichment factor (EF) of PAHs on MNP-PANI-DICAT-MSPE were in the range of 7.546-29.632. The extraction recoveries of natural water, sludge, and soil samples were ranged from 80.2% to 111.9% with relative standard deviation (RSD) less than 5.6%. The newly synthesised MNP-PANI-DICAT possess good sensitivity, reusability, and fast extraction of PAHs under the MSPE procedure in various environmental samples.
The nanobiocatalyst (NBC) is an emerging innovation that synergistically integrates advanced nanotechnology with biotechnology and promises exciting advantages for improving enzyme activity, stability, capability and engineering performances in bioprocessing applications. NBCs are fabricated by immobilizing enzymes with functional nanomaterials as enzyme carriers or containers. In this paper, we review the recent developments of novel nanocarriers/nanocontainers with advanced hierarchical porous structures for retaining enzymes, such as nanofibres (NFs), mesoporous nanocarriers and nanocages. Strategies for immobilizing enzymes onto nanocarriers made from polymers, silicas, carbons and metals by physical adsorption, covalent binding, cross-linking or specific ligand spacers are discussed. The resulting NBCs are critically evaluated in terms of their bioprocessing performances. Excellent performances are demonstrated through enhanced NBC catalytic activity and stability due to conformational changes upon immobilization and localized nanoenvironments, and NBC reutilization by assembling magnetic nanoparticles into NBCs to defray the high operational costs associated with enzyme production and nanocarrier synthesis. We also highlight several challenges associated with the NBC-driven bioprocess applications, including the maturation of large-scale nanocarrier synthesis, design and development of bioreactors to accommodate NBCs, and long-term operations of NBCs. We suggest these challenges are to be addressed through joint collaboration of chemists, engineers and material scientists. Finally, we have demonstrated the great potential of NBCs in manufacturing bioprocesses in the near future through successful laboratory trials of NBCs in carbohydrate hydrolysis, biofuel production and biotransformation.
Magnetically separable photocatalyst beads containing nano-sized iron oxide in alginate polymer were prepared. This magnetic photocatalyst beads are used in slurry-type reactors. The magnetism of the catalyst arises from the nanostructured particles gamma-Fe(2)O(3), by which the catalyst can be easily recovered by the application of an external magnetic field. These synthesized beads are sunlight-driven photocatalyst. In the system without magnetic photocatalyst beads, no chromium reduction was observed under sunlight irradiation due to the stability of the chromium (VI). Upon the addition of magnetic photocatalyst beads, the photo-reduction of Cr(VI) was completed in just after only 50min under sunlight irradiation due to the photocatalytic activity of the beads. However when placed away from sunlight, the reduction rate of the chromium is just about 10%. These observations were explained in terms of absorption occurrence of chromium (VI) onto the catalyst surface which took place in this reaction. In addition, photo-reduction rate of chromium (VI) was more significant at lower pH. The results suggest that the use of magnetic separable photocatalyst beads is a feasible strategy for eliminating Cr(VI).
This study was designed to determine the optimum vertical height of the retraction force on the power arm that is required for efficient anterior tooth retraction during space closure with sliding mechanics.
A new graphene-based tetraethoxysilane-methyltrimethoxysilane sol-gel hybrid magnetic nanocomposite (Fe3O4@G-TEOS-MTMOS) was synthesised, characterized and successfully applied in magnetic solid-phase extraction (MSPE) for simultaneous analysis of polar and non-polar organophosphorus pesticides from several water samples. The Fe3O4@G-TEOS-MTMOS nanocomposite was characterized using Fourier transform-infrared spectroscopy, energy-dispersive X-ray spectroscopy, field emission scanning electron microscopy and X-ray diffraction. Separation, determination and quantification were achieved using gas chromatography coupled with micro electron capture detector. Adsorption capacity of the sorbent was calculated using Langmuir equation. MSPE was linear in the range 100-1000 pg mL(-1) for phosphamidon and dimethoate, and 10-100 pg mL(-1) for chlorpyrifos and diazinon, with limit of detection (S/N = 3) of 19.8, 23.7, 1.4 and 2.9 pg mL(-1) for phosphamidon, dimethoate, diazinon and chlorpyrifos, respectively. The LODs obtained is well below the maximum residual level (100 pg mL(-1)) as set by European Union for pesticides in drinking water. Acceptable precision (%RSD) was achieved for intra-day (1.3-8.7%, n = 3) and inter-day (7.6-17.8%, n = 15) analyses. Fe3O4@G-TEOS-MTMOS showed high adsorption capacity (54.4-76.3 mg g(-1)) for the selected OPPs. No pesticide residues were detected in the water samples analysed. Excellent extraction recoveries (83-105%) were obtained for the spiked OPPs from tap, river, lake and sea water samples. The newly synthesised Fe3O4@G-TEOS-MTMOS showed high potential as adsorbent for OPPs analysis.
The objectives of this study were to compare the effects of a newly designed magnetic suspension system with that of two existing suspension methods on pistoning inside the prosthetic socket and to compare satisfaction and perceived problems among transtibial amputees.
In this work, zinc chromite (ZnCr2O4) nanostructures have been synthesized through co-precipitation method. The effect of various parameters such as alkaline agent, pH value, and capping agent type was investigated on purity, particle size and morphology of samples. It was found that particle size and morphology of the products could be greatly influenced via these parameters. The synthesized products were characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), fourier transform infrared (FT-IR) spectra, X-ray energy dispersive spectroscopy (EDS), photoluminescence (PL) spectroscopy, diffuse reflectance spectroscopy (DRS) and vibrating sample magnetometry (VSM). The superhydrophilicity of the calcined oxides was investigated by wetting experiments and a sessile drop technique which carried out at room temperature in air to determine the surface and interfacial interactions. Furthermore, the photocatalytic activity of ZnCr2O4 nanoparticles was confirmed by degradation of anionic dyes such as Eosin-Y and phenol red under UV light irradiation. The obtained ZnCr2O4 nanoparticles exhibit a paramagnetic behavior although bulk ZnCr2O4 is antiferromagnetic, this change in magnetic property can be ascribed to finite size effects.
The authors describe a method for solvent-free mechano-chemical synthesis of a bioinspired sorbent. A 2D ultra-thin carbon sheet similar to graphene oxide was prepared using a natural waste (onion sheet). The formation of 2D carbon sheets was confirmed by Raman spectroscopy, X-ray photoelectron spectroscopy and ATR-IR. The surface morphology was characterized by field emission scanning electron microscopy and high-resolution tunneling electron microscopy. The carbon sheets were decorated with crystalline MnFe2O4 nanoparticles by solid-state reaction at room temperature. The presence of magnetic particles in the final product was confirmed by vibrating sample magnetometry and electron microscopy. The synergistic effect of carbon sheets and MnFe2O4 led to an enhanced sorption of arsenic species compared to bare carbon sheets or to MnFe2O4 nanoparticles. A column was prepared for the simultaneous preconcentration and determination of trace levels of As(III) and As(V) from water samples. The preconcentration factors are between 900 and 833 for As(III) and As(V) species, respectively. The linearity of the calibration plot ranges from 0.4-10 ng mL-1. The detection limits (at 3σ) for both As(III) and As(V) are 30 pg mL-1. The Student's t values for the analysis of spiked samples are lower than the critical Student's t values at a 95% confidence level. The recoveries from spiked water samples range between 99 and 102.8%. Graphical abstract Schematic representation of the preparation of carbon sheets similar to graphene oxide from onion sheaths after pyrolysis at 800 °C. The prepared carbon sheet-MnFe2O4 composite shows excellent arsenic sorption and preconcentration down to the pg mL-1 concentration.
Undoped and Mn2+ doped CoAl2O4 (MnxCo1-xAl2O4; x = 0.0 to 1.0) spinel nanoparticles were successfully synthesized by a microwave heating method using glycine as the fuel. X-ray powder diffraction (XRD) was confirmed the cubic spinel structure. The average crystallite size of the samples was found to be in the range of 16.46 nm to 20.25 nm calculated by Scherrer's formula. The nano-sized particle-like morphology of the samples was confirmed by high resolution scanning electron microscopy (HR-SEM) and transmission electron microscopy (HR-TEM) analysis. Energy dispersive X-ray (EDX) results showed the pure form of spinel aluminate structure. The band gap energy (Eg) of pure CoAl2O4 was estimated to be 3.68 eV from UV-Visible diffuse reflectance spectroscopy (DRS), and the Eg values increased with increase of Mn2+ ions, due to the smaller grain size. The magnetic hysteresis (M-H) loop showed the superparamagnetic nature, and the magnetization and coercivity values increased with increasing Mn2+ ions, which was confirmed by vibrating sample magnetometer (VSM). All compositions of the nano-catalysts were tested as catalyst successfully for the conversion of benzyl alcohol into benzaldehyde and observed good catalytic activity.
This is our initial response towards preparation of nano-inductors garnet for high operating frequencies strontium iron garnet (Sr3Fe5O12) denoted as SrIG and yttrium iron garnet (Y3Fe5O12) denoted as YIG. The garnet nano crystals were prepared by novel sol-gel technique. The phase and crystal structure of the prepared samples were identified by using X-ray diffraction analysis. SEM images were done to reveal the surface morphology of the samples. Raman spectra was taken for yttrium iron garnet (Y3Fe5O12). The magnetic properties of the samples namely initial permeability (micro), relative loss factor (RLF) and quality factor (Q-Factor) were done by using LCR meter. From the XRD profile, both of the Y3Fe5O12 and Sr3Fe5O12 samples showed single phase garnet and crystallization had completely occurred at 900 degrees C for the SrIG and 950 degrees C for the YIG samples. The YIG sample showed extremely low RLF value (0.0082) and high density 4.623 g/cm3. Interesting however is the high Q factor (20-60) shown by the Sr3Fe5O12 sample from 20-100 MHz. This high performance magnetic property is attributed to the homogenous and cubical-like microstructure. The YIG particles were used as magnetic feeder for EM transmitter. It was observed that YIG magnetic feeder with the EM transmitter gave 39% higher magnetic field than without YIG magnetic feeder.
The present work reports the successful synthesis of biosynthesized iron oxide nanoparticles (Fe3O4-NPs) with the use of non-toxic leaf extract of Neem (Azadirachta indica) as a reducing and stabilizing agent. The successful synthesis was confirmed by infrared spectra analysis with strong peak observed between 400-600 cm-1 that corresponds to magnetite nanoparticles characteristics. X-ray diffraction (XRD) analysis revealed that iron oxide nanoparticles were of high purity with crystalline cubic structure phases in nature. Besides, the average size of magnetite nanoparticles was observed to be 9-12 nm with mostly irregular shapes using a transmission electron microscope (TEM) and was supported by field emission scanning electron microscope (FESEM). Energy dispersive X-ray analysis shown that the elements iron (Fe) and oxygen (O) were present with atomic percentages of 33.29% and 66.71%, respectively. From the vibrating sample magnetometer (VSM) analysis it was proven that the nanoparticles exhibited superparamagnetic properties with a magnetization value of 73 emu/g and the results showed superparamagnetic behavior at room temperature, suggesting potential applications for a magnetic targeting drug delivery system.
This work presents the synthesis of the novel silica-cyanopropyl functionalized magnetic graphene oxide (MGO/SiO2-CN) hybrid nanomaterial derived by sol-gel method as a cheap efficient magnetic sorbent for the removal of extremely hazardous lead ions from aqueous media. The integration of the magnetic property, the carbon substrate, and the nitrile (-C ≡ N) containing organic grafted silica matrix promoted the adsorption capability against lead ions along with its simple synthesis recovery and low cost. The prepared nanocomposite was comprehensively characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. Adsorption of lead was found to be pH dependent because of the charged nature of both analyte and adsorbent surface. Adsorption experiments were conducted under the optimum conditions, and the obtained experimental data from atomic absorption spectroscopy were analyzed using the popular isothermal models namely Langmuir, Freundlich, and Dubinin-Radushkevich isotherms as well as kinetically studied and evaluated for adsorption standard free energy (E). The experimental results have demonstrated the enhanced adsorption capability of the proposed sorbent nanocomposite for lead ion removal with the maximum adsorption capacity of 111.11 mg/g at pH 5.0. The proposed mechanism of lead adsorption was mainly attributed to the complexation of lead positive ions with the grafted -C ≡ N bond. The synergistic effect of the combination of three components (i.e., the magnetic graphene oxide matrix, the triple bond containing organic moiety, and the inorganic porous silica framework) excelled the adsorption capability and proved to be a good candidate as adsorbent for the removal of lead ions.
New-generation adsorbent, Fe3O4@SiO2/GO, was developed by modification of graphene oxide (GO) with silica-coated (SiO2) magnetic nanoparticles (Fe3O4). The synthesized adsorbent was characterized using Fourier transform infrared spectroscopy, X-ray diffractometry, energy-dispersive X-ray spectroscopy, and field emission scanning electron microscopy. The developed adsorbent was used for the removal and simultaneous preconcentration of As(III) and As(V) from environmental waters prior to ICP-MS analysis. Fe3O4@SiO2/GO provided high adsorption capacities, i.e., 7.51 and 11.46 mg g(-1) for As(III) and As(V), respectively, at pH 4.0. Adsorption isotherm, kinetic, and thermodynamic were investigated for As(III) and As(V) adsorption. Preconcentration of As(III) and As(V) were studied using magnetic solid-phase extraction (MSPE) method at pH 9.0 as the adsorbent showed selective adsorption for As(III) only in pH range 7-10. MSPE using Fe3O4@SiO2/GO was developed with good linearities (0.05-2.0 ng mL(-1)) and high coefficient of determination (R (2) = 0.9992 and 0.9985) for As(III) and As(V), respectively. The limits of detection (LODs) (3× SD/m, n = 3) obtained were 7.9 pg mL(-1) for As(III) and 28.0 pg mL(-1) for As(V). The LOD obtained is 357-1265× lower than the WHO maximum permissible limit of 10.0 ng mL(-1). The developed MSPE method showed good relative recoveries (72.55-109.71 %) and good RSDs (0.1-4.3 %, n = 3) for spring water, lake, river, and tap water samples. The new-generation adsorbent can be used for the removal and simultaneous preconcentration of As(III) and As(V) from water samples successfully. The adsorbent removal for As(III) is better than As(V).
The pollution of water resources due to the disposal of industrial wastes that have organic material like phenol is causing worldwide concern because of their toxicity towards aquatic life, human beings and the environment. Phenol causes nervous system damage, renal kidney disease, mental retardation, cancer and anaemia. In this study, magnetic palm kernel biochar is used for removal of phenol from wastewater. The effect of parameters such as pH, agitation speed, contact time and magnetic biochar dosage are validated using design of experiments. The statistical analysis reveals that the optimum conditions for the highest removal (93.39%) of phenol are obtained at pH of 8, magnetic biochar dosage of 0.6 g, agitation speed at 180 rpm and time of 60 min with the initial concentration of 10 mg/L. The maximum adsorption capacities of phenol were found to be 10.84 mg/g and Langmuir and Freundlich isotherm models match the experimental data very well and adsorption kinetic obeys a pseudo-second order. Hence, magnetic palm kernel can be a potential candidate for phenol removal from wastewater.
Successful application of a magnetophoretic separation technique for harvesting biological cells often relies on the need to tag the cells with magnetic nanoparticles. This study investigates the underlying principle behind the attachment of iron oxide nanoparticles (IONPs) onto microalgal cells, Chlorella sp. and Nannochloropsis sp., in both freshwater and seawater, by taking into account the contributions of various colloidal forces involved. The complex interplay between van der Waals (vdW), electrostatic (ES) and Lewis acid-base interactions (AB) in dictating IONP attachment was studied under the framework of extended Derjaguin-Landau-Verwey-Overbeek (XDLVO) analysis. Our results showed that ES interaction plays an important role in determining the net interaction between the Chlorella sp. cells and IONPs in freshwater, while the AB and vdW interactions play a more dominant role in dictating the net particle-to-cell interaction in high ionic strength media (≥100 mM NaCl), such as seawater. XDLVO predicted effective attachment between cells and surface functionalized IONPs (SF-IONPs) with an estimated secondary minimum of -3.12 kT in freshwater. This prediction is in accordance with the experimental observation in which 98.89% of cells can be magnetophoretically separated from freshwater with SF-IONPs. We have observed successful magnetophoretic separation of microalgal cells from freshwater and/or seawater for all the cases as long as XDLVO analysis predicts particle attachment. For both the conditions, no pH adjustment is required for particle-to-cell attachment.