Search Results (12)

The present study attempted to investigate the best conditions to use 2-(4-chlorophenyle)-1,4,5-triphenyle-H-imidazole as a corrosion inhibitor of mild steel in a 7% HCl and 20% H₂SO₄ pickling bath mixture, using chemical, electrochemical, and surface response methodologies in a spherical field. For this, a Doehlert matrix and two principal factors of the Pickling Process were examined. An experimental evaluation was carried out using weight loss, electrochemical impedance spectroscopy, and polarization curve measurements. Impedance diagrams and Bode plots for uninhibited and inhibited systems were analyzed and simulated using the Z-view program, the fitted data obtained closely followed the same pattern as the experimental results. This study demonstrates that the 2-(4-chlorophenyle)-1,4,5-triphenyle-H-imidazole compound is an effective inhibitor for mild steel in pickling bath solutions, and corrosion inhibition efficiency increases with increases in inhibitor concentration to attain 93.2% imidazole at 10⁻³ M. This is due to the absorbability of Cl⁻ and SO₄²⁻ present in the pickling bath solution and the synergistic effect between both elements. The response used in the exploitation of the design was the determination of inhibitor efficiency. This was assessed through weight loss measurements and electrochemical studies on samples in the absence and presence of 2-(4-chlorophenyle)-1,4,5-triphenyle-H-imidazole. It has been shown that the compound under investigation is an effective cathodic-type inhibitor of mild steel corrosion in pickling bath mixtures. Therefore, the inhibition efficiency was improved with the concentration of the inhibitor, which depended on the molecular structure. The optimal corrosion inhibition efficiency as a function of variation in 2-(4-chlorophenyle)-1,4,5-triphenyle-H-imidazole concentration and pickling bath temperature was simulated and demonstrated using canonical analysis; the obtained efficiency at 324 K for 6 h was 81.3% for the coded variable and 83.4% for the real variable. The experimental results are based on a real-time system and provide much more precise results than the simulated results. Full article

The presence of silver nanoparticles (AgNPs) in water bodies has emerged as a new environmental concern and the efficient separation of these nanoparticles remains a critical challenge. Here, we developed novel magnetic nanoflocculants for the recovery of AgNPs from water. Alternating layers of biopolymers, in particular, chitosan, alginate, and polymeric bio-based soluble substances (BBS) derived from urban waste, were coated on magnetic nanoparticles via the layer-by-layer technique to prepare reusable magnetic nanoflocculants (MNFs). The MNFs obtained were characterized with diverse physicochemical techniques. Surface response methodology, based on the Doehlert matrix, has shown to be a useful tool to determine the effect of pH (in the range 5–9), concentration of AgNPs (7–20 mg L⁻¹), and MNFs (50–1000 mg L⁻¹) on the performance of AgNPs removal. The model predicts a high AgNPs removal percentage at low pH values and high MNF concentration. In particular, for the most efficient MNFs, 90% of AgNPs removal was obtained at pH 5 and 600 mg L⁻¹ MNF concentration. Additionally, the effects of AgNPs size, ionic strength, the presence of humic acids, and two types of surfactants (LAS anionic and TWEEN 20 nonionic) on the AgNPs removal were evaluated. Finally, recovery and reuse experiments showed that MNF made of Chitosan-BBS can be reused in ten cycles, losing only 30% of the initial removal capacity. Therefore, magnetic flocculation could represent a sustainable alternative for AgNPs separation with potential applications in water treatment and remediation of nanoparticle contamination. Full article

This work describes the development of a method for the extraction of methylxanthines from cocoa bean shell (CBS) by employing the novel Energized Dispersive Guided Extraction (EDGE) system. The mixtures were composed of ethanol–methanol–water and the ratio was optimized using a simplex-centroid design. Doehlert design (DD) was used to optimize the variables of temperature and time while using methylxanthine content obtained by HPLC-DAD as an analytical response. The optimized mixture consisted of water–ethanol in a 3:2 ratio. The optimum operating conditions for extraction were achieved at a temperature of 148.5 °C and 382 s. Under optimal conditions, 20.14 mg g⁻¹ DM of theobromine and 3.53 mg g⁻¹ DM of caffeine were found in the CBS extract. Methylxanthines were quantified with good linearity, LOQs, LODs, precision, and accuracy. The EDGE system, a newly automated extraction instrument, has proven to be very efficient for the recovery of theobromine and caffeine, and is considered a green extraction procedure, as demonstrated by the analytical greenness metric for sample preparation. Full article

Cellulose tosylate (MCC-Tos) is a key derivative for surface modification and a crucial precursor for cellulose compatibilization in click reactions, enabling its functionalization for advanced applications. Replacing tosyl groups with alkyne groups broadens cellulose’s potential in biocompatible reactions, such as thiol-yne click chemistry and protein/enzyme immobilization. To achieve this, we optimized the heterogeneous synthesis of MCC-Tos using a Doehlert matrix statistical design, evaluating the influence and interaction of the reaction conditions. The optimized conditions—144 h reaction time, 10:1 molar ratio, and 30 °C—yielded a degree of substitution for tosyl groups (DS_tos) of 1.80, determined via elemental analysis and FTIR-ATR spectroscopy. The reaction kinetics followed a first-order model. A subsequent reaction with propargylamine produced aminopropargyl cellulose (MCC-P_NH), reducing DS_tos by 65%, which was confirmed via FTIR, and improving thermal stability by a margin of 30 °C (TGA/DTG). ¹³C CP/MAS NMR confirmed the alkyne group attachment, further validated via coupling an azide-functionalized coumarin through copper(I)-catalyzed alkyne-azide cycloaddition (CuAAC). Fluorescence microscopy and UV spectroscopy were used to estimate a substitution degree of 0.21. This study establishes a feasible route for synthesizing alkyne-functionalized cellulose, paving the way for eco-friendly materials, including protein/enzyme bioconjugates, composites, and advanced materials via thiol-yne and CuAAC reactions. Full article

The many possible treatments and continuously changing consumer trends present a challenge when selecting antimicrobial interventions during pork processing. Thirty-five potential antimicrobials were screened at commercial working concentrations by individually adding them to miniaturized (69 cm³) disks of pork loin ends, followed by inoculation with Salmonella Typhimurium ATCC 19585. Two organic acids and nine essential oils significantly inhibited Salmonella counts on pork (p < 0.05). However, six compounds that represent different levels of significance (p < 0.05–p < 0.0001) were selected as independent variables to build a Response Surface Methodology model based on a Doehlert matrix (Doehlert Matrix—RSM): lactic acid 1.25%, formic acid 0.25%, cumin 0.25%, clove 0.25%, peppermint 0.5%, and spearmint 0.5%. The goal of the Doehlert Matrix—RSM was to study single and paired effects of these antimicrobials on the change in Salmonella over 24 h. The Doehlert Matrix—RSM model predicted that lactic acid, formic acid, cumin, peppermint, and spearmint significantly reduced Salmonella when added alone, while no significant interactions between these antimicrobials were found. A laboratory-scale validation was carried out on pork loin end slices, which confirmed the results predicted by the model. While this screening did not identify novel synergistic combinations, our approach to screening a variety of chemical compounds by implementing a miniaturized pork loin disk model allowed us to identify the most promising antimicrobial candidates to then formally design experiments to study potential interactions with other antimicrobials. Full article

This study developed a predictive model for Escherichia coli survival in Amlou, a Moroccan almond–honey–argan oil spread, focusing on argan oil, sugar, and peptone concentrations. Based on the Doehlert matrix design, relationships were established between these ingredients and the death rate (DR) and survival period (SP). Sugar affected the DR, while argan oil and peptone influenced the SP. The DR model demonstrated an RMSE of 0.0095 and SEP of 22.22%, confirming its accuracy. This work offers valuable insights for food producers about E. coli’s behavior in Amlou-like foods. Full article

There is a growing interest for complex in vitro environments that closely mimic the extracellular matrix and allow cells to grow in microenvironments that are closer to the one in vivo. Protein-based matrices and especially hydrogels can answer this need, thanks to their similarity with the cell microenvironment and their ease of customization. In this study, an experimental design was conducted to study the influence of synthesis parameters on the physical properties of gelatin methacryloyl (GelMA). Temperature, ratio of methacrylic anhydride over gelatin, rate of addition, and stirring speed of the reaction were studied using a Doehlert matrix. Their impact on the following parameters was analyzed: degree of substitution, mass swelling ratio, storage modulus (log(G’)), and compression modulus. This study highlights that the most impactful parameter was the ratio of methacrylic anhydride over gelatin. Although, temperature affected the degree of substitution, and methacrylic anhydride addition flow rate impacted the gel’s physical properties, namely, its storage modulus and compression modulus. Moreover, this experimental design proposed a theoretical model that described the variation of GelMA’s physical characteristics as a function of synthesis conditions. Full article

In this study, calcium and magnesium were removed from Tunisian dam, lake, and tap water using Donnan Dialysis (DD) according to the Doehlert design. Three cation-exchange membranes (CMV, CMX, and CMS) were used in a preliminary investigation to establish the upper and lower bounds of each parameter and to more precisely pinpoint the optimal value. The concentration of compensating sodium ions [Na⁺] in the receiver compartment, the concentration of calcium [Ca²⁺] and magnesium [Mg²⁺] in the feed compartment, and the membrane nature were the experimental parameters. The findings indicate that the CMV membrane offers the highest elimination rate of calcium and magnesium. The Full Factorial Design makes it possible to determine how the experimental factors affect the removal of calcium and magnesium by DD. All parameters used had a favorable impact on the response; however, the calcium and magnesium concentration were the most significant ones. The Doehlert design’s Response Surface Methodology (RSM) was used to determine the optimum conditions ([Mg²⁺] = 90 mg·L⁻¹, [Ca²⁺] = 88 mg·L⁻¹, [Na⁺] = 0.68 mol·L⁻¹) allowing a 90.6% hardness removal rate with the CMV membrane. Finally, we used Donnan Dialysis to remove calcium and magnesium from the three different types of natural water: Dam, Lake, and Tap water. The results indicate that, when compared to lake water and tap water, the removal of calcium and magnesium from dam water is the best. This can be linked to the water matrix’s complexity. Therefore, using Donnan Dialysis to decrease natural waters hardness was revealed to be suitable. Full article

This work investigates the effects of various processing parameters (laser power, scanning speed, hatch distance and beam offset) on the resultant inclined up-facing surface roughness of AlSi10Mg alloys produced by laser powder bed fusion (LPBF). A two-step approach, orthogonal test followed by the Doehlert matrix design (DMD) test is used to efficiently optimize the up-facing surface and contour parameters. The former method aims to determine the significance of variables while the latter one facilitates a rapid optimization. The results show that the interaction and interdependency among the parameters are of great significance to the obtainable surface roughness. Using a rational design of experiments, the optimized up-facing surface roughness of Ra of 5.4 μm is achieved. This is attributed to the elimination of the laser partition track and the reduction in irregularities at the edges of the parts. This work demonstrates an effective approach of experimental processing parameter optimization to improve the surface finish of LPBF parts. Full article

This work aims to present an industrial perspective on Catalytic Wet Peroxide Oxidation (CWPO) technology. Herein, process simulation and experimental design have been coupled to study the optimal process conditions to ensure high-performance oxidation, minimum H₂O₂ consumption and maximum energetic efficiency in an industrial scale CWPO unit. The CWPO of phenol in the presence of carbon black catalysts was studied as a model process in the Aspen Plus^® v11 simulator. The kinetic model implemented, based on 30 kinetic equations with 11 organic compounds and H₂O₂ involvement, was valid to describe the complex reaction network and to reproduce the experimental results. The computer experiments were designed on a six-factor Doehlert Matrix in order to describe the influence of the operating conditions (i.e., the different process temperatures, inlet chemical oxygen demands, doses of H₂O₂ and space time) on each selected output response (conversion, efficiency of H₂O₂ consumption and energetic efficiency) by a quadratic model. The optimization of the WPO performance by a multi-criteria function highlighted the inlet chemical oxygen demand as the most influential operating condition. It needed to have values between 9.5 and 24 g L⁻¹ for autothermal operation to be sustained under mild operating conditions (reaction temperature: 93–130 °C and pressure: 1–4 atm) and with a stoichiometric dose of H₂O₂. Full article

In view of the importance of accurately measuring the relative density of a selective laser melted (SLMed) part for optimizing the selective laser melting (SLM) processing parameters, suitable procedures of the Archimedes method considering the surface-connected cavities were proposed by comparing the results using the Archimedes method with image analysis. The effects of the SLM processing parameters on the relative density of AlSi10Mg were investigated using the proposed procedures of the Archimedes methods and image analysis. Fourteen SLMed samples were produced by different SLM processing parameters according to Doehlert Matrix. The regression models correlating relative density and three SLM processing parameters (laser power, scan speed, and hatching distance) were built and the optimum parameter combination to get a high relative density was obtained. By plotting the response surfaces and contours of the regression models, it was found that the relative densities are both higher at the combination of the higher scan speed, higher power, and lower hatching distance and at the combination of a lower scan speed, a moderate laser power, and a optional hatching distance. It was also found that the parameter of hatching distance is the crucial parameter to get a high relative density and to get high mechanical property. Full article

Nickel (II) preconcentration and speciation analysis using a hollow fiber supported liquid membrane (HFSLM) device was studied. A counterflow of protons coupled to complexation with formate provided the driving force of the process, while Kelex 100 was employed as carrier. The influence of variables related to module configuration (acceptor pH and carrier concentration) and to the sample properties (donor pH) on the preconcentration factor, E, was simultaneously studied and optimized using a 3 factor Doehlert matrix response surface methodology. The effect of metal concentration was studied as well. Preconcentration factors as high as 4240 were observed depending on the values of the different variables. The effects of the presence of inorganic anions (NO₂^-, SO₄^2-, Cl^-, NO₃^-, CO₃^2-, CN^-) and dissolved organic matter (DOM) in the form of humic acids were additionally considered in order to carry out a speciation analysis study. Nickel preconcentration was observed to be independent of both effects, except when cyanide was present in the donor phase. A characterization of the transport regime was performed through the analysis of the dependence of E on the temperature. E increases with the increase in temperature according to the equation E(K) = -8617.3 + 30.5T with an activation energy of 56.7 kJ mol^-1 suggesting a kinetic-controlled regime. Sample depletion ranged from 12 to 1.2% depending on the volume of the donor phase (100 to 1000 mL, respectively). Full article