Optimization of ultrasound-assisted dispersive solid-phase microextraction based on nanoparticles followed by spectrophotometry for the simultaneous determination of dyes using experimental design

A simple, low cost and ultrasensitive method for the simultaneous preconcentration and determination of trace amount of auramine-O and malachite green in aqueous media following accumulation on novel and lower toxicity nanomaterials by ultrasound-assisted dispersive solid phase micro-extraction (UA-DSPME) procedure combined with spectrophotometric has been described. The Mn doped ZnS nanoparticles loaded on activated carbon were characterized by Field emission scanning electron microscopy (FE-SEM), particle size distribution, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) analyses and subsequently were used as green and efficient material for dyes accumulation. Contribution of experimental variables such as ultrasonic time, ultrasonic temperature, adsorbent mass, vortex time, ionic strength, pH and elution volume were optimized through experimental design, and while the preconcentrated analytes were efficiently eluted by acetone. Preliminary Plackett–Burman design was applied for selection of most significant factors and giving useful information about their main and interaction part of significant variables like ultrasonic time, adsorbent mass, elution volume and pH were obtained by central composite design combined with response surface analysis and optimum experimental conditions was set at pH of 8.0, 1.2 mg of adsorbent, 150 μL eluent and 3.7 min sonication. Under optimized conditions, the average recoveries (five replicates) for two dyes (spiked at 500.0 ng mL⁻¹) changes in the range of 92.80–97.70% with acceptable RSD% less than 4.0% over a linear range of 3.0–5000.0 ng mL⁻¹ for the AO and MG in water samples with regression coefficients (R²) of 0.9975 and 0.9977, respectively. Acceptable limits of detection of 0.91 and 0.61 ng mL⁻¹ for AO and MG, respectively and high accuracy and repeatability are unique advantages of present method to improve the figures of merit for their accurate determination at trace level in complicated materials.     

Ultrasound assisted extraction of Maxilon Red GRL dye from water samples using cobalt ferrite nanoparticles loaded on activated carbon as sorbent: Optimization and modeling

In this research, a selective, simple and rapid ultrasound assisted dispersive solid-phase micro-microextraction (UA-DSPME) was developed using cobalt ferrite nanoparticles loaded on activated carbon (CoFe₂O₄-NPs-AC) as an efficient sorbent for the preconcentration and determination of Maxilon Red GRL (MR-GRL) dye. The properties of sorbent are characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Vibrating sample magnetometers (VSM), Fourier transform infrared spectroscopy (FTIR), Particle size distribution (PSD) and Scanning Electron Microscope (SEM) techniques. The factors affecting on the determination of MR-GRL dye were investigated and optimized by central composite design (CCD) and artificial neural networks based on genetic algorithm (ANN-GA). CCD and ANN-GA were used for optimization. Using ANN-GA, optimum conditions were set at 6.70, 1.2 mg, 5.5 min and 174 μL for pH, sorbent amount, sonication time and volume of eluent, respectively. Under the optimized conditions obtained from ANN-GA, the method exhibited a linear dynamic range of 30–3000 ng mL⁻¹ with a detection limit of 5.70 ng mL⁻¹. The preconcentration factor and enrichment factor were 57.47 and 93.54, respectively with relative standard deviations (RSDs) less than 4.0% (N = 6). The interference effect of some ions and dyes was also investigated and the results show a good selectivity for this method. Finally, the method was successfully applied to the preconcentration and determination of Maxilon Red GRL in water and wastewater samples.     

Effects of various factors of ultrasonic treatment on the extraction recovery of drugs from fish tissues

In the present research, a combined extraction method of ultrasound-assisted extraction (UAE) in conjunction with solid phase extraction (SPE) was applied to isolation and enrichment of selected drugs (metoprolol, ticlopidine, propranolol, carbamazepine, naproxen, acenocumarol, diclofenac, ibuprofen) from fish tissues. The extracted analytes were separated and determined by ultra-high performance liquid chromatography with UV detection (UHPLC–UV) technique. The selectivity of the developed UHPLC–UV method was confirmed by comparison with ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) analysis.The important parameters, such as composition of type and pH of extraction solvent, solid/liquid rate volume of extraction solvent and number of extraction cycles were studied. The ultrasonic parameters, such as time, power and temperature of the process were optimized by using a half-fraction factorial central composite design (CCD). The mixture of 10 mL of methanol and 7 mL of water (pH 2.2) (three times) was chosen for the extraction of selected drug from fish tissues. The results showed that the highest recoveries of analytes were obtained with an extraction temperature of 40 °C, ultrasonic power of 300 W, extraction time of 30 min.Under the optimal conditions, the linearity of method was 0.12–5.00 μg/g. The determination coefficients (R²) were from 0.979 to 0.998. The limits of detection (LODs) and limits of quantification (LOQs) for the extracted compounds were 0.04–0.17 μg/g and 0.12–0.50 μg/g, respectively. The recoveries were between 85.5% and 115.8%.     

Ultrasound assisted combined molecularly imprinted polymer for selective extraction of nicotinamide in human urine and milk samples: Spectrophotometric determination and optimization study

Ultrasound-assisted dispersive solid phase microextraction followed by UV–vis spectrophotometer (UA-DSPME-UV–vis) was designed for extraction and preconcentration of nicotinamide (vitamin B₃) by HKUST-1 metal organic framework (MOF) based molecularly imprinted polymer (MIP). This new material was characterized by FTIR and FE-SEM techniques. The preliminary Plackett–Burman design was used for screening and subsequently the central composite design justifies significant terms and possible construction of mathematical equation which give the individual and cooperative contribution of variables like HKUST-1-MOF-NA-MIP mass, sonication time, temperature, eluent volume, pH and vortex time. Accordingly the optimum condition was set as: 2.0 mg HKUST-1-MOF-NA-MIP, 200 μL eluent and 5.0 min sonication time in center points other variables were determined as the best conditions to reach the maximum recovery of the analyte. The UA-DSPME-UV–vis method performances like excellent linearity (LR), limits of detection (LOD), limits of quantification of 10–5000 μg L⁻¹ with R² of 0.99, LOD (1.96 ng mL⁻¹), LOQ (6.53 μg L⁻¹), respectively show successful and accurate applicability of the present method for monitoring analytes with within- and between-day precision of 0.96–3.38%. The average absolute recoveries of the nicotinamide extracted from the urine, milk and water samples were 95.85–101.27%.     

Cu@SnS/SnO2 nanoparticles as novel sorbent for dispersive micro solid phase extraction of atorvastatin in human plasma and urine samples by high-performance liquid chromatography with UV detection: Application of central composite design (CCD)

Separation and detection of residual drug in biological fluids has directly related to human health in term of their beneficial or side effects. In biological fluid samples (complex matrix which containing drug at very low level) conduction of preliminary efficient technique as good choice for pre-concentration and clean-up of real sample before their instrumental analysis is highly recommended. In this result technique, based on nano-structure material which poses higher available surface area and larger member of reactive sites led to significant improvement in characteristic performance of analytical method. This paper focused on the synthesis and application of novel nano-sorbent for pre-concentration and extraction of atorvastatin (AT) from different biological fluids. Influence of various variables including sorbent dosage, eluent volume and sonication time on present method response was studied and optimized by central composite design under response surface methodology and accordingly an acceptable calibration curves over wide linear ranges (0.3–2000 μg L⁻¹) with high coefficient of determination higher than 0.999 strongly confirm high applicability of present method for quantification of analyte while limit of detection and quantification in plasma sample were 0.0608 and 0.2033 μg L⁻¹, respectively.     

Ultrasonic assisted dispersive solid-phase microextraction of Eriochrome Cyanine R from water sample on ultrasonically synthesized lead (II) dioxide nanoparticles loaded on activated carbon: Experimental design methodology

The present research focus on designing an appropriate dispersive solid-phase microextraction (UA-DSPME) for preconcentration and determination of Eriochrome Cyanine R (ECR) in aqueous solutions with aid of sonication using lead (II) dioxide nanoparticles loaded on activated carbon (PbO-NPs-AC). This material was fully identified with XRD and SEM. Influence of pH, amounts of sorbent, type and volume of eluent, and sonication time on response properties were investigated and optimized by central composite design (CCD) combined with surface response methodology using STATISTICA. Among different solvents, dimethyl sulfoxide (DMSO) was selected as an efficient eluent, which its combination by present nanoparticles and application of ultrasound waves led to enhancement in mass transfer. The predicted maximum extraction (100%) under the optimum conditions of the process variables viz. pH 4.5, eluent 200 μL, adsorbent dosage 2.5 mg and 5 min sonication was close to the experimental value (99.50%). at optimum conditions some experimental features like wide 5–2000 ng mL⁻¹ ECR, low detection limit (0.43 ng mL⁻¹, S/N = 3:1) and good repeatability and reproducibility (relative standard deviation, <5.5%, n = 12) indicate versatility in successful applicability of present method for real sample analysis. Investigation of accuracy by spiking known concentration of ECR over 200–600 ng mL⁻¹ gave mean recoveries from 94.850% to 101.42% under optimal conditions. The procedure was also applied for the pre-concentration and subsequent determination of ECR in tap and waste waters.     

Sonochemical degradation of ethyl paraben in environmental samples: Statistically important parameters determining kinetics,by-products and pathways

The sonochemical degradation of ethyl paraben (EP), a representative of the parabens family, was investigated. Experiments were conducted at constant ultrasound frequency of 20 kHz and liquid bulk temperature of 30 °C in the following range of experimental conditions: EP concentration 250–1250 μg/L, ultrasound (US) density 20–60 W/L, reaction time up to 120 min, initial pH 3–8 and sodium persulfate 0–100 mg/L, either in ultrapure water or secondary treated wastewater.A factorial design methodology was adopted to elucidate the statistically important effects and their interactions and a full empirical model comprising seventeen terms was originally developed. Omitting several terms of lower significance, a reduced model that can reliably simulate the process was finally proposed; this includes EP concentration, reaction time, power density and initial pH, as well as the interactions (EP concentration) × (US density), (EP concentration) × (pH_o) and (EP concentration) × (time).Experiments at an increased EP concentration of 3.5 mg/L were also performed to identify degradation by-products. LC–TOF–MS analysis revealed that EP sonochemical degradation occurs through dealkylation of the ethyl chain to form methyl paraben, while successive hydroxylation of the aromatic ring yields 4-hydroxybenzoic, 2,4-dihydroxybenzoic and 3,4-dihydroxybenzoic acids. By-products are less toxic to bacterium V. fischeri than the parent compound.     

Sonophotocatalytic degradation of trypan blue and vesuvine dyes in the presence of blue light active photocatalyst of Ag3PO4/Bi2S3-HKUST-1-MOF: Central composite optimization and synergistic effect study

An efficient simultaneous sonophotocatalytic degradation of trypan blue (TB) and vesuvine (VS) using Ag₃PO₄/Bi₂S₃-HKUST-1-MOF as a novel visible light active photocatalyst was carried out successfully in a continuous flow-loop reactor equipped to blue LED light. Ag₃PO₄/Bi₂S₃-HKUST-1-MOF with activation ability under blue light illumination was synthesized and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), photoluminescence (PL) and diffuse reflectance spectra (DRS). The effect of operational parameters such as the initial TB and VS concentration (5–45 mg/L), flow rate (30–110 mL/min), irradiation and sonication time (10–30 min), pH (3–11) and photocatalyst dosage (0.15–0.35 g/L) has been investigated and optimized using central composite design (CCD) combined with desirability function (DF). Maximum sonophotodegradation percentage (98.44% and 99.36% for TB and VS, respectively) was found at optimum condition set as: 25 mg/L of each dye, 70 mL/min of solution flow rate, 25 min of irradiation and sonication time, pH 6 and 0.25 g/L of photocatalyst dosage. At optimum conditions, synergistic index value was obtained 2.53 that indicated the hybrid systems including ultrasound irradiation and photocatalysis have higher efficiency compared with sum of the individual processes.     

Novel synthesis of nanocomposite for the extraction of Sildenafil Citrate (Viagra) from water and urine samples: Process screening and optimization

A sensitive analytical method is investigated to concentrate and determine trace level of Sildenafil Citrate (SLC) present in water and urine samples. The method is based on a sample treatment using dispersive solid-phase micro-extraction (DSPME) with laboratory-made Mn@ CuS/ZnS nanocomposite loaded on activated carbon (Mn@ CuS/ZnS-NCs-AC) as a sorbent for the target analyte. The efficiency was enhanced by ultrasound-assisted (UA) with dispersive nanocomposite solid-phase micro-extraction (UA-DNSPME). Four significant variables affecting SLC recovery like; pH, eluent volume, sonication time and adsorbent mass were selected by the Plackett-Burman design (PBD) experiments. These selected factors were optimized by the central composite design (CCD) to maximize extraction of SLC. The results exhibited that the optimum conditions for maximizing extraction of SLC were 6.0 pH, 300 μL eluent (acetonitrile) volume, 10 mg of adsorbent and 6 min sonication time. Under optimized conditions, virtuous linearity of SLC was ranged from 30 to 4000 ng mL⁻¹ with R² of 0.99. The limit of detection (LOD) was 2.50 ng mL⁻¹ and the recoveries at two spiked levels were ranged from 97.37 to 103.21% with the relative standard deviation (RSD) less than 4.50% (n = 15). The enhancement factor (EF) was 81.91. The results show that the combination UAE with DNSPME is a suitable method for the determination of SLC in water and urine samples.     

Ultrasonically tailored,chemically engineered and “QbD” enabled fabrication of agomelatine nanoemulsion; optimization,characterization, ex-vivo permeation and stability study

The objective of present study was to develop a nanoemulsion formulation of agomelatine (BCS class II drug) for the solubility enhancement. Capmul MCM, Tween 80 and PEG-400 were selected as oil, surfactant and co-surfactant respectively. The high energy ultrasonication method was used for the preparation of nanoemulsion. Three-factor three-level central composite design was employed to get the best formulation. The independent variables selected for the optimization were % oil, %S_mix and sonication time (second). Based on the constraints applied to independent and dependent variables, the optimized formulation was selected with 2% oil, 10% S_mix and 45 s sonication time. The experimental values for dependent variables such as hydrodynamic diameter (nm), % transmittance and % CDR were found to be 73.72 ± 2.53 nm, 98.2 ± 0.42%, 84.71 ± 4.05% respectively. TEM and AFM−assisted morphological characterization of optimized Ago-NE was done and it was found with a spherical shape. The PDI, Zeta potential and the refractive index of optimized Ago-NE were found to be 0.137 ± 0.016, −7.40 ± 0.12 mV and 1.423 ± 0.045 respectively. The viscosity, pH and drug content of optimized Ago-NE were found as 25.12 ± 0.67 cP, 6.4 ± 0.17 and 97.83 ± 1.03% respectively. The ex-vivo permeation profile of optimized Ago-NE and agomelatine suspension through goat nasal mucosa were compared till 12 h and % cumulative drug permeated was found to be 90% and 40% respectively. The higher drug permeation profile of optimized Ago-NE confirmed that the solubility of agomelatine has been improved.     

Dispersion of hydrophobic magnetic nanoparticles using ultarsonic-assisted in combination with coacervative microextraction for the simultaneous preconcentration and determination of tricyclic antidepressant drugs in biological fluids

A two-step sample preparation technique based on dispersive micro solid-phase extraction combined with coacervative microextraction is presented for preconcentration and determination of tricyclic antidepressant drugs in biological samples. An important feature of the method is the application of hydrophobic magnetic nanoparticles, which in combination with coacervative microextraction method enables development of rapid and efficient extraction procedure in order to achievement of a high extraction efficiency. Simultaneous optimization by experimental design lead to improvement of method with low cost which supply useful information about interaction among variables. Under the optimized conditions, a linear range of 5–1000 ng mL⁻¹ with detection limits from 0.51 to 1.4 ng mL⁻¹ were obtained for target analytes. The method was successfully used for the determination of analytes in biological fluids (plasma and urine) with relative recoveries in the range of 89–105% (RSDs < 3.5%).     

Reduction of core loss in non-oriented (NO) electrical steel by electroless-plated magnetic coating

An important issue in development of electrical steels for core-laminated products is to reduce core loss to improve energy conversion efficiency. This is usually obtained by tailoring the composition, microstructure, and texture of electrical steels themselves. A new technique to reduce core loss in electrical steel has been investigated. This technique involves electroless plating of magnetic thin coating onto the surface of electrical steel. The material system was electroless Ni–Co–P coatings with different thicknesses (1, 5, and 10 μm) deposited onto the surface of commercially available Fe–3% Si electrical steel. Characterization of deposited Ni–Co–P coating was carried out using X-ray diffraction (XRD), scanning electron microscope (SEM), and energy dispersive X-ray (EDX) spectrometer. The deposited Ni–Co–P coatings were amorphous and composed of 56–59% Ni, 32–35% Co, and 8–10% P by mass. The effect of coatings on core loss of the electrical steel was determined using single sheet test. A core loss reduction of 4% maximum was achieved with the Ni–Co–P coating of 1 μm thickness at 400 Hz and 0.3 T.     

Catalytic dechlorination of 2,4-dichlorophenol by Ni/Fe nanoparticles prepared in the presence of ultrasonic irradiation

In this study, nickle/iron (Ni/Fe) nanoparticles were synthesized by liquid phase reductive method in the presence of 20 kHz ultrasonic irradiation to improve nanoparticles’ disparity and avoid agglomeration. The characterized results showed that this method has obviously modified most of the particles in term of sizes and specific surface areas. Meanwhile, the improved nanoscale Ni/Fe particles were employed for the reductive dechlorination of 2,4-dichlorophenol (2,4-DCP) as a function of some influential factors (Ni content, Ni/Fe nanoparticles dosage, reaction temperature and initial pH values) and degradation path. Experimental results showed that 2,4-DCP was first adsorbed by Ni/Fe nanoparticles, then quickly reduced to o-chlorophenol (o-CP), p-chlorophenol (p-CP), and finally to phenol (P). The application of ultrasonic irradiation for Ni/Fe nanoparticles synthesis was found to significantly enhance the removal efficiency of 2,4-DCP. Consequently, the phenol production rates increased from 68% (in the absence of ultrasonic irradiation) to 87% (in the presence of ultrasonic irradiation) within 180 min. Nearly 96% of 2,4-DCP was removed after 300 min reaction with these optimized conditions: Ni content over Fe⁰ 3 wt%, initial 2,4-DCP concentration 20 mg L⁻¹, Ni/Fe dosage 3 g L⁻¹, initial pH value 3.0, and reaction temperature 25 °C. The degradation of 2,4-DCP followed pseudo-first-order kinetics reaction and the apparent pseudo-first-order kinetics constant was 0.0737 min⁻¹. This study suggested that the presence of ultrasonic irradiation in the synthesis of nanoscale Ni/Fe particles could be a promising technique to enhance nanoparticle’s disparity and avoid agglomeration.     

Ultrasound-assisted extraction and purification of schisandrin B from Schisandra chinensis (Turcz.) Baill seeds: Optimization by response surface methodology

The objective of this study is to develop a process consisting of ultrasonic-assisted extraction, silica-gel column chromatography and crystallization to optimize pilot scale recovery of schisandrin B (SAB) from Schisandra chinensis seeds. The effects of five independent variables including liquid–solid ratio, ethanol concentration, ultrasonic power, extraction time, and temperature on the SAB yield were evaluated with fractional factorial design (FFD). The FFD results showed that the ethanol concentration was the only significant factor for the yield of SAB. Then, with the liquid–solid ratio 5 (mL/g) and ultrasonic power 600 W, the other three parameters were further optimized by means of response surface methodology (RSM). The RSM results revealed that the optimal conditions consisted of 95% ethanol, 60 °C and 70 min. The average experimental SAB yield under the optimum conditions was found to be 5.80 mg/g, which was consistent with the predicted value of 5.83 mg/g. Subsequently, a silica gel chromatographic process was used to prepare the SAB-enriched extract with petroleum ether/acetone (95:5, v/v) as eluents. After final crystallization, 1.46 g of SAB with the purity of 99.4% and the overall recovery of 57.1% was obtained from 400 g seeds powder. This method provides an efficient and low-cost way for SAB purification for pharmaceutical industrial applications.     

Ultrasound-promoted dispersive micro solid-phase extraction of trace anti-hypertensive drugs from biological matrices using a sonochemically synthesized conductive polymer nanocomposite

In this work, a rapid and efficient procedure named ultrasound meliorated dispersive micro solid-phase extraction followed by high performance liquid chromatography-ultra violet detection (US-D-μSPE-HPLC-UV) was developed for the pre-concentration of the main trace anti-hypertensive drugs in complex matrices. The basis of this procedure was a polypyrrole-sodium dodecylbenzenesulfonate/zinc oxide (PPy-DBSNa/ZnO) nanocomposite. It was readily synthesized by the impressive way of in situ sonochemical oxidative polymerization in the presence of some additives such as FeCl₃ and DBSNa, ultimately leading to the effective coating of PPy on the ZnO nanoparticle cores. Characterization of the proposed nanosorbent was performed by different techniques such as FESEM, XRD,EDX, and TGA, confirming the high quality and proper physico-chemical properties of the proposed sorbent. In order to better investigate the input variables, the central composite design (CCD) combined with the desirability function (DF) was utilized. The enriched optimum conditions consisted of the initial pH value of 11.8, 15 mg of the PPy-DBSNa/ZnO nanocomposite, a sonication time of 4.6 min, and 100 μL of methanol, resulting in maximum responses at a relatively low extraction time with a logical DF. Under the optimum conditions, good linearity (5–5000, 2.5–3500, and 2.5–3000 ng mL⁻¹ for metoprolol, propranolol, and carvedilol, respectively, with the correlation of determinations (R²s) higher than 0.99), low limits of detection (LODs) (0.8–1.5 ng mL⁻¹), proper repeatabilities (relative standard deviation values (RSDs) below 6.3%, n = 3), reasonable enrichment factors (EFs) (60–72), and good extraction recoveries (ERs) (higher than %75) were obtainable. These appropriate validations corroborated a good effectiveness of ultrasonic waves in the achievement of a supreme solid phase as well as a facile and efficient microextraction of the low therapeutic concentrations in human plasma and urine samples.     

Surface modification of Ni and Co metal nanowires through MeV high energy ion irradiation

Nickel (Ni) and cobalt (Co) metal nanowires were fabricated by using an electrochemical deposition method based on an anodic alumina oxide (Al₂O₃) nanoporous template. The electrolyte consisted of NiSO₄ · 6H₂O and H₃BO₃ in distilled water for the fabrication of Ni nanowires, and of CoSO₄ · 7H₂O with H₃BO₃ in distilled water for the fabrication of the Co ones. From SEM and TEM images, the diameter and length of both the Ni and Co nanowires were measured to be ∼ 200 nm and 5–10 μm, respectively. We observed the oxidation layers in nanometer scale on the surface of the Ni and Co nanowires through HR–TEM images. The 3 MeV Cl²⁺ ions were irradiated onto the Ni and Co nanowires with a dose of 1 × 10¹⁵ ions/cm². The surface morphologies of the pristine and the 3 MeV Cl²⁺ ion-irradiated Ni and Co nanowires were compared by means of SEM, AFM, and HR–TEM experiments. The atomic concentrations of the pristine and the 3 MeV Cl²⁺ ion-irradiated Ni and Co nanowires were investigated through XPS experiments. From the results of the HR–TEM and XPS experiments, we observed that the oxidation layers on the surface of the Ni and Co nanowires were reduced through 3 MeV Cl²⁺ ion irradiation.     

Structural origin of perpendicular magnetic anisotropy in Ni–W thin films

The magnetic properties and microstructure of electrodeposited Ni–W thin films (0–11.7 at% W in composition) were studied. The film structures were divided into three regions: an FCC nanocrystalline phase (0–2 at% W), a transition region from FCC nanocrystalline to amorphous phase (2–7 at% W), and an amorphous phase (>7 at% W). In the transition region, (4–5 at% W) films with perpendicular magnetic anisotropy (PMA) were found. The saturation magnetization, magnetic anisotropy field, perpendicular magnetic anisotropy and perpendicular coercivity for a typical Ni–W film (4.5 at% W) were 420 kA/m, 451 kA/m, 230 kJ/m and 113 kA/m, respectively. The microstructure of Ni–W films with PMA is composed of isolated columnar crystalline grains (27–36 nm) with the FCC phase surrounded by the Ni–W amorphous phase. The appearance of the interface between the magnetic core of Ni crystalline grains and the Ni–W non-magnetic boundary layer seems to be the driving mechanism for the appearance of PMA. The origin of PMA in Ni–W films is mainly attributed to the magnetoelastic anisotropy associated with in-plane internal stress and positive magnetostriction. The secondary source of PMA is believed to be the magnetocrystalline anisotropy of 〈1 1 1〉 columnar grains and its shape magnetic anisotropy. It is concluded that Ni–W electrodeposited films (4–5 at% W) may be applicable for perpendicular magnetic recording media.     

Synthesis and application of molecularly imprinted nanoparticles combined ultrasonic assisted for highly selective solid phase extraction trace amount of celecoxib from human plasma samples using design expert (DXB) software

In this work molecular imprinted nanoparticles (MINPs) was synthesized and applied for ultrasonic assisted solid phase extraction of celecoxib (CEL) from human plasma sample following its combination by HPLC–UV. The MINPs were prepared in a non-covalent approach using methacrylic acid as monomer, CEL as template, ethylene glycol dimethacrylate as cross-linker, and 2,2-azobisisobutyronitrile (AIBN) as the initiator of polymerization. pH, volume of rinsing and eluent solvent and amount of sorbent influence on response were investigated using factorial experimental design, while optimum point was achieved and set as 250 mg sorbent, pH 7.0, 1.5 mL washing solvent and 2 mL eluent by analysis of results according to design expert (DX) software. At above specified conditions, CEL in human plasma with complicated matrices with acceptable high recoveries (96%) and RSD% lower than 10% was quantified and estimated.The proposed MISPE-HPLC–UV method has linear responses among peak area and concentrations of CEL in the range of 0.2–2000 μg L⁻¹, with regression coefficient of 0.98. The limit of detection (LOD) and quantification (LOQ) based on three and ten times of the noise of HPLC peaks correspond to blank solution were 0.08 and 0.18 μg L⁻¹, respectively.     

Sonocatalytic degradation of methylene blue by a novel graphene quantum dots anchored CdSe nanocatalyst

Cadmium selenide/graphene quantum dots (CdSe/GQDs) nanocatalyst with small band gap energy and a large specific surface area was produced via a facile three-step sonochemical-hydrothermal process. The features of the as-prepared CdSe, GQDs and CdSe/GQDs samples were characterized by photoluminescence spectroscopy (PL), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction (XRD), Fourier transformed infrared (FT-IR), diffuse-reflectance spectrophotometer (DRS), and Brunauer–Emmett–Teller (BET) analysis. The sonocatalytic activity of the synthesized CdSe/GQDs was effectively accelerated compared with that of pure CdSe nanoparticles in degradation of methylene blue (MB). The influence of the CdSe/GQDs dosage (0.25–1.25 g/L), initial MB concentration (20–30 mg/L), initial solution pH (3–12), and ultrasonic output power (200–600 W/L) were examined on the sonocatalytic treatment of MB aqueous solutions. The degradation efficiency (DE%) of 99% attained at 1 g/L of CdSe/GQDs, 20 mg/L of MB, pH of 9, and an output power of 200 W/L at 90 min of ultrasonic irradiation. Furthermore, DE% increased with addition of K₂S₂O₈ and H₂O₂ as the enhancers via producing more free radicals. However, addition of sulfate, carbonate, and chloride as radical sweeper decreased DE%. Furthermore, well-reusability of the CdSe/GQDs sonocatalyst was demonstrated for 5 successive runs and some of the sonocatalytic generated intermediates were indicated by GC–MS analysis.     

Synthesis and characterization of ZnS:Ni-NPs loaded on AC derived from apple tree wood and their applicability for the ultrasound assisted comparative adsorption of cationic dyes based on the experimental design

The applicability of ZnS:Ni nanoparticles loaded on activated carbon derived from apple tree wood (ZnS:Ni-NPs-ACATW) for the adsorption of Methylene Blue (MB) and Janus Green B (JGB) dyes in single system from water solution has been described. The synthesized adsorbent characterized and identified by UV–Vis, FE-SEM, EDX, TEM, FTIR and XRD. The influences of operation parameters including initial MB or JGB concentration (9.0–33.0 mg L⁻¹), pH (4.0–10.0), extent of adsorbent (0.08–0.12 g) and sonication time (4.0–8.0 min) investigated and subsequently best operational condition optimized by central composite design (CCD) combined with response surface methodology (RSM) and desirability function (DF) using STATISTICA 10.0 software. At optimum conditions, maximum MB and JSB adsorption onto ZnS:Ni-NPs-ACATW, i.e. 99.57% ± 1.34 and 98.70% ± 2.01, respectively was achieved pH of 7.0, 0.11 g adsorbent, 14 and 28 mg L⁻¹ of MB and JSB concentration respectively and 8 min sonication time. Experimental data were modelled by Langmuir, Freundlich, Temkin and Dubinin-Radushkevich (D-R) isotherms. Langmuir isotherm and monolayer adsorption capacity of MB and JSB was found to be 21.79 and 28.01 mg g⁻¹ respectively. The regression results strongly support more contribution of pseudo-second-order model for more accurate and repeatable representation of kinetic data. These results reveal that ZnS:Ni-NPs-ACATW could be useful as agents to efficiently remove dyes (JGB and MB) from contaminated water and can be very well recommended for wastewater remediation and control of environmental pollution.