Synthesis of nanocomposites of iron oxide/gold (Fe3O4/Au) loaded on activated carbon and their application in water treatment by using sonochemistry: Optimization study

This paper focuses on the finding best operational conditions using response surface methodology (RSM) for Rhodamine123 (R123) and Disulfine blue (DSB) dyes removal by ultrasound assisted adsorption onto Au-Fe₃O₄ nanoparticles loaded on activated carbon (Au-Fe₃O₄ NPs-AC). The influences of variables such as initial R123 (X₁) and DSB concentration (X₂), pH (X₃), adsorbent mass (X₄) and sonication time (X₅) on their removal were investigated by small central composite design (CCD) under response surface methodology. The significant variables and the possible interactions among variables were investigated and estimated accordingly. The best conditions were set as: 4 min, 4.0, 0.025 g, 13.5 and 26.5 mg L⁻¹ for sonication time, pH, adsorbent weight, initial R123 and DSB concentration, respectively. At above conditions, the adsorption equilibrium and kinetic follow the Langmuir isotherm and pseudo-second-order kinetic model, respectively. The maximum monolayer capacity (Q_max) of 71.46 and 76.38 mg g⁻¹ for R123 and DSB show sufficiency of model for well presentation of experimental data.     

Advanced oxidation of Reactive Blue 181 solution: A comparison between Fenton and Sono-Fenton Process

In this work, the decolorization of C.I. Reactive Blue 181 (RB181), an anthraquinone dye, by Ultrasound and Fe²⁺ H₂O₂ processes was investigated. The effects of operating parameters, such as Fe²⁺ dosage, H₂O₂ dosage, pH value, reaction time and temperature were examined. Process optimisation [pH, ferrous ion (Fe²⁺), hydrogen peroxide (H₂O₂), and reaction time], kinetic studies and their comparison were carried out for both of the processes. The Sono-Fenton process was performed by indirect sonication in an ultrasonic water bath, which was operated at a fixed 35-kHz frequency. The optimum conditions were determined as [Fe²⁺] = 30 mg/L, [H₂O₂] = 50 mg/L and pH = 3 for the Fenton process and [Fe²⁺] = 10 mg/L, [H₂O₂] = 40 mg/L and pH = 3 for the Sono-Fenton process. The colour removals were 88% and 93.5% by the Fenton and Sono-Fenton processes, respectively. The highest decolorization was achieved by the Sono-Fenton process because of the production of some oxidising agents as a result of sonication. The paper also discussed kinetic parameters. The decolorization kinetic of RB181 followed pseudo-second-order reaction (Fenton study) and Behnajady kinetics (Sono-Fenton study).     

Optimization of simultaneous ultrasound assisted toxic dyes adsorption conditions from single and multi-components using central composite design: Application of derivative spectrophotometry and evaluation of the kinetics and isotherms

Present study is devoted on the efficient application of Sn (O, S)-NPs -AC for simultaneous sonicated accelerated adsorption of some dyes from single and multi-components systems. Sn (O, S) nanoparticles characterization by FESEM, EDX, EDX mapping and XRD revel its nano size structure with high purity of good crystallinity. Present adsorbent due to its nano spherical shape particles with approximate diameter of 40–60 nm seems to be highly effective in this regard. The effects of five variables viz. pH (3.5–9.5), 0.010–0.028 g of adsorbent and 0.5–6.5 min mixing by sonication is good and practical conditions for well and expected adsorption of MB and CV over concentration range of 3–15 mg L⁻¹. Combination of response surface methodology (RSM) based on central composite design (CCD) and subsequent of analysis of variance (ANOVA) and t-test statistics were used to test the significance of the independent variables and their interactions. Regression analysis reveal that experimental data with high repeatability and efficiency well represented by second-order polynomial model with coefficient of determination value of 0.9988 and 0.9976 for MB and CV, respectively following conditions like pH 8.0, 0.016 g adsorbent, 15 mg L⁻¹ of both dyes 4 min sonication time is proportional with achievement of experimental removal percentage of 99.80% of MB and 99.87% of CV in batch experiment. Evaluation and estimation of adsorption data with Langmuir and Freundlich isotherm well justify the results based on their correlation coefficient and error analysis confirm that Langmuir model is good model with adsorption capacity of 109.17 and 115.34 mg g⁻¹ in single system and 95.69 and 102.99 mg g⁻¹ in binary system for MB and CV, respectively. MB and CV kinetic and rate of adsorption well fitted by pseudo-second order equation both in single and binary systems and experimental results denote more and favorable adsorption of CV than respective value in single system. The pseudo-second-order rate constant k₂ in binary system larger than single system.     

Application of modificated magnetic nanomaterial for optimization of ultrasound-enhanced removal of Pb2+ ions from aqueous solution under experimental design: Investigation of kinetic and isotherm

Magnetic γ-Fe₂O₃ nanoparticles modificated by bis(5-bromosalicylidene)-1,3-propandiamine (M-γ-Fe₂O₃-NPs-BBSPN) and characterized by field emission scanning electron microscopy (FE-SEM), Fourier transforms infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). This modified compound as novel adsorbent was applied for the ultrasound-assisted removal of Pb²⁺ ion in combination with flame atomic absorption spectroscopy (FAAS). The influences of the effective parameters including initial Pb²⁺ ion concentration, pH, adsorbent mass and ultrasound time were optimized by central composite design (CCD). Maximum removal percentage of Pb²⁺ ion which obtained at 25 mg L⁻¹ of Pb²⁺, 25 mg of adsorbent and 4 min mixing with sonication at pH 6.0. The precision of the equation obtained by CCD was confirmed by the analysis of variance and calculation of correlation coefficient relating the predicted and the experimental values of removal percentage of Pb²⁺ ion. The kinetic and isotherm of ultrasound-assisted removal of Pb²⁺ ion was well described by second-order kinetic and Langmuir isotherm model with maximum adsorption capacity of 163.57 mg g⁻¹.     

Improved adsorption performance of nanostructured composite by ultrasonic wave: Optimization through response surface methodology,isotherm and kinetic studies

In this work, ultrasound-assisted adsorption of an anionic dye, sunset yellow (SY) and cationic dyes, malachite green (MG), methylene blue (MB) and their ternary dye solutions onto Cu@ Mn-ZnS-NPs-AC from water aqueous was optimized by response surface methodology (RSM) using the central composite design (CCD). The adsorbent was characterized using Field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDX) and EDX mapping images. The effects of various parameters such as pH, sonication time, adsorbent mass and initial concentrations of SY, MG and MB were examined. A total 33 experiments were conducted to establish a quadratic model. Cu@ Mn-ZnS-NPs-AC has the maximum adsorption efficiency (>99.5%) when the pH, sonication time, adsorbent mass and initial concentrations of SY, MG and MB were optimally set as 6.0, 5 min, 0.02 g, 9, 12 and 12 mg L⁻¹, respectively. Sonication time has a statistically significant effect on the selected responses. Langmuir isotherm model was found to be best fitted to adsorption and adsorption capacities were 67.5 mg g⁻¹ for SY, 74.6 mg g⁻¹ for MG and 72.9 mg g⁻¹ for MB. Four kinetic models (pseudo-first order, pseudo-second order, Weber–Morris intraparticle diffusion rate and Elovich) were tested to correlate the experimental data and the sorption was fitted well with the pseudo-second order kinetic model.     

Reprint of: Decomposition of PPCPs by ultrasound-assisted advanced Fenton reaction: A case study with salicylic acid

The study is about the degradation of a widely used pharmaceutical and personal care product-salicylic acid by sonocatalysis, and the experimental design of the reaction system. The first part of the study consists of sonication (572 kHz) in the presence of zero-valent iron (ZVI) with or without H₂O₂ to select and optimize the operational parameters as frequency, time, initial solute concentration, dose of reagents and pH. The second part consists of the use of response surface methodology and multiple regression to develop an experimental design modeland to assess the individual and interactive effects of pH, power (P_o), ZVI dose and H₂O₂. The results showed that the optimal conditions predicted by the model without defining any restrictions are: pH = 2.0, P_o = 120 W, ZVI = 24 mg L⁻¹, which provide total salicyclic acid and 48% TOC decay. However, the prediction implies intensive consumption of energy and reagents, and must therefore be modified by restricting the value of TOC decay to a lower value and that of pH to a higher one. Cross-validation tests showed that the prediction accuracy of the model was considerably high with 5.0–9.4% deviation from the experimental data.     

Catalytic-oxidative/adsorptive denitrogenation of model hydrocarbon fuels under ultrasonic field using magnetic reduced graphene oxide-based phosphomolybdic acid (PMo-Fe3O4/rGO)

In this work, the effect of ultrasound irradiation on the catalytic oxidative/adsorptive denitrogenation (COADN) of model hydrocarbon fuels (composed of pyrrole or indole as an organonitrogen compounds dissolved in n-nonane) has been investigated using magnetic reduced graphene oxide supported with phosphomolybdic acid (PMo-Fe₃O₄/rGO) as a heterogeneous catalyst/adsorbent and hydrogen peroxide as an oxidant. The synthesized PMo-Fe₃O₄/rGO nanocomposite was characterized by XRD, FE-SEM, VSM and BET surface area analysis methods. Moreover, different experimental variables including catalyst dose, initial pyrrole/indole concentration, H₂O₂ to pyrrole/indole molar ratio, ultrasound power and sonication time have been studied on the COADN process. The regeneration/recyclability of PMo-Fe₃O₄/rGO catalyst was also examined. Experimental results revealed that, the ultrasound treatment significantly improved the adsorption process of organonitrogen compounds from model fuels (q_e increased by 50.3% for pyrrole and 18% for indole). Furthermore, high ultrasound-aided catalytic oxidative denitrogenation efficiency (85.6% for pyrrole and 90% for indole) has been attained under optimal conditions (ultrasonic power = 200 W, sonication time = 240 min, catalyst dose = 2 g/L, and H₂O₂:pyrrole/indole molar ratio = 5). The recyclability of catalyst displayed that the prepared catalyst can be reused five times without any significant reduction in its performance.     

Ultrasonically assisted hydrothermal synthesis of activated carbon–HKUST-1-MOF hybrid for efficient simultaneous ultrasound-assisted removal of ternary organic dyes and antibacterial investigation: Taguchi optimization

Activated carbon (AC) composite with HKUST-1 metal organic framework (AC–HKUST-1 MOF) was prepared by ultrasonically assisted hydrothermal method and characterized by FTIR, SEM and XRD analysis and laterally was applied for the simultaneous ultrasound-assisted removal of crystal violet (CV), disulfine blue (DSB) and quinoline yellow (QY) dyes in their ternary solution. In addition, this material, was screened in vitro for their antibacterial actively against Methicillin-resistant Staphylococcus aureus (MRSA) and Pseudomonas aeruginosa (PAO1) bacteria. In dyes removal process, the effects of important variables such as initial concentration of dyes, adsorbent mass, pH and sonication time on adsorption process optimized by Taguchi approach. Optimum values of 4, 0.02 g, 4 min, 10 mg L⁻¹ were obtained for pH, AC–HKUST-1 MOF mass, sonication time and the concentration of each dye, respectively. At the optimized condition, the removal percentages of CV, DSB and QY were found to be 99.76%, 91.10%, and 90.75%, respectively, with desirability of 0.989. Kinetics of adsorption processes follow pseudo-second-order model. The Langmuir model as best method with high applicability for representation of experimental data, while maximum mono layer adsorption capacity for CV, DSB and QY on AC–HKUST-1 estimated to be 133.33, 129.87 and 65.37 mg g⁻¹ which significantly were higher than HKUST-1 as sole material with Q_m to equate 59.45, 57.14 and 38.80 mg g⁻¹, respectively.     

A simultaneous,direct microwave/ultrasound-assisted digestion procedure for the determination of total Kjeldahl nitrogen

Simultaneous direct irradiation with microwaves and ultrasound was used to determine total Kjeldahl nitrogen. The method involves chemical digestion in two steps, mineralization with sulfuric acid and oxidation with H₂O₂. The most influential variables for the microwave/ultrasound (MW/US)-assisted digestion were optimized using tryptophan as the model substance. The optimum conditions were: H₂SO₄ volume, 10 mL; H₂O₂ volume, 5 mL; weight of sample, 0.05 g; MW power, 500 W; US power, 50 W; digestion time, 7 min (i.e., 5 min mineralization and 2 min oxidation). A modification of the classical Kjeldahl (Hach) method and an US-assisted digestion method were used for comparison. The latter was also optimized; the optimum conditions were: H₂SO₄ volume, 10 mL; H₂O₂ volume, 5 mL; sonication time with H₂SO₄, 15 min; sonication time with H₂O₂,10 min; US power, 50 W; weight of sample, 0.05 g. Five pure amino acids and two certified reference materials (NIST standard reference materials 1547 (peach leaves), and soil, NCS DC 73322) were analyzed to assess the accuracy of our new MW/US-assisted digestion method, that was successfully applied to five real samples. The significant reduction in digestion time (being 30 min and 25 min for classical Kjeldahl and US-assisted digestion methods, respectively) and consumption of reagents show that simultaneous and direct MW/US irradiation is a powerful and promising tool for low-pressure digestion of solid and liquid samples.     

Screening and optimization of highly effective ultrasound-assisted simultaneous adsorption of cationic dyes onto Mn-doped Fe3O4-nanoparticle-loaded activated carbon

The ultrasound-assisted simultaneous adsorption of brilliant green (BG) and malachite green (MG) onto Mn-doped Fe₃O₄ nanoparticle-loaded activated carbon (Mn-Fe₃O₄-NP-AC) as a novel adsorbent was investigated and analyzed using first derivative spectrophotometry. The adsorbent was characterized using FT-IR, FE-SEM, EDX and XRD. Plackett–Burman design was applied to reduce the total number of experiments and to optimize the ultrasound-assisted simultaneous adsorption procedure, where pH, adsorbent mass and sonication time (among six tested variables) were identified as the most significant factors. The effects of significant variables were further evaluated by a central composite design under response surface methodology. The significance of independent variables and their interactions was investigated by means of the analysis of variance (ANOVA) within 95% confidence level together with Pareto chart. Using this statistical tool, the optimized ultrasound-assisted simultaneous removal of basic dyes was obtained at 7.0, 0.02 g, 3 min for pH, adsorbent mass, and ultrasonication time, respectively. The maximum values of BG and MG uptake under these experimental conditions were found to be 99.50 and 99.00%, respectively. The adsorption process was found to be followed by the Langmuir isotherm and pseudo-second order model using equilibrium and kinetic studies, respectively. According to Langmuir isotherm model, the maximum adsorption capacities of the adsorbent were obtained to be 101.215 and 87.566 mg g⁻¹ for MG and BG, respectively. The value of apparent energy of adsorption obtained from non-linear Dubinin–Radushkevich model (4.348 and 4.337 kJ mol⁻¹ for MG and BG, respectively) suggested the physical adsorption of the dyes. The studies on the well regenerability of the adsorbent in addition to its high adsorption capacity make it promising for such adsorption applications.     

Obtaining Ca(H2PO4)2·H2O,monocalcium phosphate monohydrate,via monetite from brushite by using sonication

Brushite was synthesized by precipitation of calcium chloride (CaCl₂) and sodium phosphate monobasic (Na₂HPO₄) dried in vacuum and monetite was obtained from this brushite by sonication with a frequency of 90 kHz at 500 W for 90 min. Monetite itself was also transformed in Ca(H₂PO₄)₂·H₂O, monocalcium phosphate monohydrate (MCPM), by sonication with a frequency of 90 kHz at 500 W for 60 min followed by lyophilization. The MCPM was sonicated and lyophilized by three times more until reach over 240 min, but any other phase transformation was observed. All these phase transformations were analyzed by X-ray diffraction (XRD) and infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated a grain size of about 200 nm in all the samples. The morphology observed was a corn-flake-like grain for brushite, a pseudo-needle-like grains for monetite, and lamellar-like grains for MCPM.     

Dual frequency cavitation event sensor with iodide dosimeter

The inertial cavitation activity depends on the sonication parameters. The purpose of this work is development of dual frequency inertial cavitation meter for therapeutic applications of ultrasound waves. In this study, the chemical effects of sonication parameters in dual frequency sonication (40 kHz and 1 MHz) were investigated in the progressive wave mode using iodide dosimetry. For this purpose, efficacy of different exposure parameters such as intensity, sonication duration, sonication mode, duty factor and net ultrasound energy on the inertial cavitation activity have been studied. To quantify cavitational effects, the KI dosimeter solution was sonicated and its absorbance at a wavelength of 350 nm was measured. The absorbance values in continuous sonication mode was significantly higher than the absorbance corresponding to the pulsed mode having duty factors of 20–80% (p < 0.05). Among different combination modes (1 MHz_100% + 40 kHz_100%, 1 MHz_100% + 40 kHz_80%, 1 MHz_80% + 40 kHz_100%, 1 MHz_80% + 40 kHz_80%), the continuous mode for dual frequency sonication is more effective than other combinations (p < 0.05). The absorbance for this combined dual frequency mode was about 1.8 times higher than that obtained from the algebraic summation of single frequency sonications. It is believed that the optimization of dual frequency sonication parameters at low-level intensity (<3 W/cm²) by optically assisted cavitation event sensor can be useful for ultrasonic treatments.     

Ultrasonic assisted-Fenton-like degradation of nitrobenzene at neutral pH using nanosized oxides of Fe and Cu

Ultrasonic-assisted heterogeneous Fenton reaction was used for degradation of nitrobenzene (NB) at neutral pH conditions. Nano-sized oxides of α-Fe₂O₃ and CuO were prepared, characterized and tested in degradation of NB (10 mg L⁻¹) under sonication of 20 kHz at 25 °C. Complete degradation of NB was effected at pH 7 in presence of 10 mM H₂O₂ after 10 min of sonication in presence of α-Fe₂O₃ (1.0 g L⁻¹), (k = 0.58 min⁻¹) and after 25 min in case of CuO (k = 0.126 min⁻¹). α-Fe₂O₃ showed also effective degradation under the conditions of 0.1 g L⁻¹ oxide and 5.0 mM of H₂O₂, even though with a lower rate constant (0.346 min⁻¹). Sonication plays a major role in enhancing the production of hydroxyl radicals in presence of solid oxides. Hydroxyl radicals-degradation pathway is suggested and adopted to explain the differences noted in rate constants recorded on using different oxides.     

Application of ZnO nanorods loaded on activated carbon for ultrasonic assisted dyes removal: Experimental design and derivative spectrophotometry method

A method based on application of ZnO nanorods loaded on activated carbon (ZnO-NRs-AC) for adsorption of Bromocresol Green (BCG) and Eosin Y (EY) accelerated by ultrasound was described. The present material was synthesized under ultrasound assisted wet-chemical method and subsequently was characterized by FE-SEM, TEM, BET and XRD analysis. The extent of contribution of conventional variables like pH (2.0–10.0), BCG concentration (4–20 mg L⁻¹), EY concentration (3–23 mg L⁻¹), adsorbent dosage (0.01–0.03 g), sonication time (1–5 min) and centrifuge time (2–6 min) as main and interaction part were investigated by central composite design under response surface methodology. Analysis of variance (ANOVA) was adapted to experimental data and guide the best operational conditions mass by set at 6.0, 9 mg L⁻¹, 10 mg L⁻¹, 0.02 g, 4 and 4 min for pH, BCG concentration, EY concentration, adsorbent dosage, sonication and centrifuge time, respectively. At these specified conditions dye adsorption efficiency was higher than 99.5%. The suitability and well prediction of optimum point was tested by conducting five experiments and respective results revel that RSD% was lower than 3% and high quality of fitting was confirmed by t-test. The experimental data were best fitted in Langmuir isotherm equation and the removal followed pseudo second order kinetics. The experimentally obtained maximum adsorption capacities were estimated as 57.80 and 61.73 mg g⁻¹ of ZnO-NRs-AC for BCG and EY respectively from binary dye solutions. The mechanism of removal was explained by boundary layer diffusion via intraparticle diffusion.     

Synthesis of magnetic γ-Fe2O3-based nanomaterial for ultrasonic assisted dyes adsorption: Modeling and optimization

γ-Fe₂O₃ nanoparticles were synthesized and loaded on activated carbon. The prepared nanomaterial was characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transforms infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The γ-Fe₂O₃ nanoparticle-loaded activated carbon (γ-Fe₂O₃-NPs-AC) was used as novel adsorbent for the ultrasonic-assisted removal of methylene blue (MB) and malachite green (MG). Response surface methodology and artificial neural network were applied to model and optimize the adsorption of the MB and MG in their individual and binary solutions followed by the investigation on adsorption isotherm and kinetics. The individual effects of parameters such as pH, mass of adsorbent, ultrasonication time as well as MB and MG concentrations in addition to the effects of their possible interactions on the adsorption process were investigated. The numerical optimization revealed that the optimum adsorption (>99.5% for each dye) is obtained at 0.02 g, 15 mg L⁻¹, 4 min and 7.0 corresponding to the adsorbent mass, each dye concentration, sonication time and pH, respectively. The Freundlich, Langmuir, Temkin and Dubinin–Radushkevich isotherms were studied. The Langmuir was found to be most applicable isotherm which predicted maximum monolayer adsorption capacities of 195.55 and 207.04 mg g⁻¹ for the adsorption of MB and MG, respectively. The pseudo-second order model was found to be applicable for the adsorption kinetics. Blank experiments (without any adsorbent) were run to investigate the possible degradation of the dyes studied in presence of ultrasonication. No dyes degradation was observed.     

Sonochemical synthesis of amide-functionalized metal-organic framework/graphene oxide nanocomposite for the adsorption of methylene blue from aqueous solution

Graphene oxide-[Zn₂(oba)₂(bpfb)]·(DMF)₅ metal-organic framework nanocomposite (GO-TMU-23; H₂oba = 4,4′-oxybisbenzoic acid, bpfb = N,N′-bis-(4-pyridylformamide)-1,4-benzenediamine, DMF = N,N-dimethylformamide) is prepared through a simple and large-scale sonochemical preparation method at room temperature. The obtained nanocomposite is characterized by Field Emission Scanning Electron Microscopy (FE-SEM), powder X-ray diffraction (PXRD) and FT-IR spectroscopy. Additionally, the absorption ability of GO-TMU-23 nanocomposite toward cationic dye methylene blue was also performed. Significantly, GO-TMU-23 nanocomposite exhibits remarkably accelerated adsorption kinetics for methylene blue in comparison with the parent materials. The adsorption process shows that 90% of the dye has been removed and the equilibrium status has been reached in 2 min by using the nanocomposites as the adsorbent.     

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.     

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.     

Ultrasonic enhancement of the simultaneous removal of quaternary toxic organic dyes by CuO nanoparticles loaded on activated carbon: Central composite design,kinetic and isotherm study

Copper oxide nanoparticles loaded on activated carbon (CuO-NPs-AC) were prepared and fully analyzed and characterized with FE-SEM, XRD and FT-IR. Subsequently, this novel material was used for simultaneous ultrasound-assisted adsorption of brilliant green (BG), auramine O (AO), methylene blue (MB) and eosin yellow (EY) dyes. Problems regard to dyes spectra overlap in quaternary solution of this dyes were omitted by derivative spectrophotometric method. The best pH in quaternary system was studied by using one at a time method to achieved maximum dyes removal percentage. Subsequently, sonication time, adsorbent dosage and initial dyes concentrations influence on dyes removal was optimized by central composite design (CCD) combined with desirability function approach (DFA). Desirability score of 0.978 show optimum conditions set at sonication time (4.2 min), adsorbent mass (0.029 g), initial dyes concentration (4.5 mg L⁻¹). Under this optimum condition the removal percentage for MB, AO, EY and BG dyes 97.58, 94.66, 96.22 and 94.93, respectively. The adsorption rate well fitted by pseudo second-order while adsorption capacity according to the Langmuir model as best equilibrium isotherm model for BG, MB, AO and EY was 20.48, 21.26, 22.34 and 21.29 mg g⁻¹, respectively.     

Optimization of the ultrasonic assisted removal of methylene blue by gold nanoparticles loaded on activated carbon using experimental design methodology

The present study was focused on the removal of methylene blue (MB) from aqueous solution by ultrasound-assisted adsorption onto the gold nanoparticles loaded on activated carbon (Au-NP-AC). This nanomaterial was characterized using different techniques such as SEM, XRD, and BET. The effects of variables such as pH, initial dye concentration, adsorbent dosage (g), temperature and sonication time (min) on MB removal were studied and using central composite design (CCD) and the optimum experimental conditions were found with desirability function (DF) combined response surface methodology (RSM). Fitting the experimental equilibrium data to various isotherm models such as Langmuir, Freundlich, Tempkin and Dubinin–Radushkevich models show the suitability and applicability of the Langmuir model. Analysis of experimental adsorption data to various kinetic models such as pseudo-first and second order, Elovich and intraparticle diffusion models show the applicability of the second-order equation model. The small amount of proposed adsorbent (0.01 g) is applicable for successful removal of MB (RE > 95%) in short time (1.6 min) with high adsorption capacity (104–185 mg g⁻¹).