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.     

Simultaneous ultrasound-assisted removal of sunset yellow and erythrosine by ZnS:Ni nanoparticles loaded on activated carbon: Optimization by central composite design

The present study focused on the simultaneous ultrasound-assisted removal of sunset yellow and erythrosine dyes from aqueous solutions using ZnS:Ni nanoparticles loaded on activated carbon (ZnS:Ni-NP-AC) as an adsorbent. ZnS:Ni nanoparticles were synthesized and characterized using different techniques such as FESEM, XRD and TEM. The effects of various parameters such as sonication time, pH, initial dye concentrations and adsorbent dose on the percentage of dye removal were investigated. Parameters were optimized by central composite design (CCD) combined with response surface methodology (RSM) and desirability function (DF). A good agreement between experimental and predicted values was observed. The ultrasound-assisted adsorbent (0.04 g) was capable of high percentage removal (98.7% and 99.6%) of sunset yellow and erythrosine in short time (3.8 min).     

Mild synthesis of a Zn(II) metal organic polymer and its hybrid with activated carbon: Application as antibacterial agent and in water treatment by using sonochemistry: Optimization,kinetic and isotherm study

In this work, a room temperature and short method (30 min) for synthesis of nanosized rod-like metal organic polymer (MOP) has been described. Reaction of 1,4-phenylenedioxy diacetic acid with zinc salt leads to the formation of [Zn(C₁₀H₈O₆)(H₂O)₄]_n and subsequently was loaded on activated carbon following sonication and structurally characterized by FTIR, SEM, EDX and XRD analysis. The combination of this new composite with sonication was applied for rapid and efficient adsorption of Bromocresol Purple (BCP). Effects of initial BCP concentration, mass of adsorbent and sonication time on response were investigated and optimized by central composite design (CCD). Analysis of variation (ANOVA) was adapted to experimental data to find best optimum conditions which was set at 15.22 mg L⁻¹, 2.41 min, 0.02 g and 0.009 mg for initial BCP concentration, sonication time and adsorbent mass, respectively. Conduction of similar experiments at specified condition permit achievement of 98.69% removal percentage. 1,4-phenylenedioxy diacetic acid and Zn(NO3)₂.4H₂O which have applied for preparation of MOP are interesting antibacterial properties and accordingly MOP was screened in vitro for their antibacterial actively against Proteus vulgaris bacteria and experimental results reveal this MOP was able to inhibit growth of the tested bacteria. The experimental data were best fitted by pseudo-second order and Langmuir for kinetic model and the adsorption equilibrium isotherm, 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.     

Palm oil hydrolysis catalyzed by lipases under ultrasound irradiation--the use of experimental design as a tool for variables evaluation

Diacylglycerol oil has been increasingly recognized by its good nutritional properties and therefore, different technologies have been developed for obtaining it. The present work focuses on the diacylglycerol production by hydrolysis reaction of the palm oil using the PS IM and TL IM commercial lipases as biocatalysts under ultrasound irradiation. An experimental design (central composite rotatable design - CCRD) adopting surface response was applied as a tool to evaluate the optimal reaction conditions beyond a restrict number of experiments. Reactions were performed in an ultrasound equipment and different variables were investigated, such as temperature (30-55 °C), enzyme content (1-2 wt.% of oil mass), mechanical stirring (300-700 rpm) and reaction time. Both, PS IM and TL IM enzymes showed the best results after 1 h and 30 min of reaction under 30 °C and, applying 300 rpm as stirring. On these conditions, the diacylglycerol yield was around 34% and 39%, respectively; considering that 1% PS IM was applied for the first one and, 2% TL IM for the second one. Therefore, it was obtained good yield of a diacylglycerol-rich oil in shorter reaction times under sonication and soft conditions. The mathematic model proposed suggested a satisfactorily representation of the process and good correlation among the experimental results and the theoretical values predicted by the model equation were achieved.     

Sono-assisted preparation of bio-nanocomposite for removal of Pb2+ ions: Study of morphology,thermal and wettability properties

Multi-walled carbon nanotubes (MWCNT) loaded poly(ethylene terephthalate) (PET) composites, with different CNT contents, were fabricated through an ultrasound assisted method as a fast and green way. Then, the obtained composites were fully characterized via FT-IR, UV–Vis, XRD, TGA, FE-SEM and TEM, etc. For this purpose, PET bottle was recycled and applied as matrix of nanocomposites (NC)s. Then, we dispersed the covalent functionalization of MWCNTs with a protein dispersant and obtained a powder of protein-functionalized CNTs. Bio-functionalized MWCNTs showed higher Pb²⁺ removal efficiency compared to MWCNT-COOH as ascertained via batch equilibrium adsorption experiments. Also, the results indicated the novel NCs presents a high affinity for Pb²⁺ heavy metal owing to the presence of several good sites. The contact angle results indicated that the addition of MWCNT-BSA increased significantly the contact angle compared to the pure PET. It was concluded that inflame retarding feature of NC was higher than pure polymer.     

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.     

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.     

晶体Zn(antipyrine)2(NO3)2:VO2+的EPR谱及光吸收谱的理论研究

由于硝酸钒锌二安替比林晶体[Zn(antipyrine)2(NO3)2:VO2 ]中配体O2-的自旋-轨道耦合参量ζ0p≈150 cm-1与中心过渡族3d1离子V4 的ζ0d≈248 cm-1相差不太大,故配体的自旋-轨道耦合参量ζ0p对电子顺磁共振(EPR)谱和光吸收谱的贡献必须考虑.采用双自旋-轨道耦合参量模型和相关的晶体场能级公式,计算了Zn(antipyrine)2(NO3)2:VO2 晶体的EPR谱和光吸收谱,所得理论结果与实验发现很好符合;确定了该晶体的局域对称结构沿C4轴的四角畸变约为0.45 nm;计算发现,较大的κ值说明VO2 中未配对的s电子对超精细结构常数有较大的贡献.并对上述这些结果的合理性进行了讨论.