Evaluation of Water-in-Crude-Oil Emulsion Stability Using Critical Electric Field: Effect of Emulsion Preparation Procedure and Crude Oil Properties

The critical electrical field has been used as a tool to probe water in crude emulsion stability to electrical fields in many previous studies. Given the increasing importance of this metric, this study investigates factors that are important to the reproducibility of the measurement and the effect of emulsion preparation variables on the critical electric field. It was observed that the emulsion preparation procedure has a strong effect on the measured critical electric field due to droplet size effects. Furthermore, the effect of crude oil properties on the critical electric field was investigated using emulsions from different oils but with the same average droplet diameter, where it was found that the measurement was dominated by crude oil viscosity.     

Investigations of the Effects of Xanthan and Sodium Caseinate on the Formation and Stability of an Oil-in-Water Emulsion Stabilized by a Nonionic Surfactant Using a Response Surface Method

Effects of xanthan and sodium caseinate concentrations on the rheological properties and stability of an oil-in water emulsion stabilized by a nonionic surfactant (Tween 20) were investigated. In order to evaluate the influence of component concentrations on the emulsion properties, a response surface method was applied. It was shown by polynomial simulation and modelization of responses of storage modulus and creaming index that in absence of Tween 20, the oily droplets were flocculated by bridging of sodium caseinate macromolecules, when those are insufficient to cover the entire interface. Additionally, it was noted that xanthan reinforces the polymeric network in the aqueous phase when the caseinate is not moved toward the phase. On the other hand, in presence of nonadsorbed caseinate, the polysaccharide develops segregative interactions by thermodynamic incompatibility. These nonadsorbed macromolecules can also flocculate the fatty globules by depletion.     

Experimental Design Approach to Investigate the Effects of Operating Factors on the Surface Tension,Viscosity, and Stability of Heavy Crude Oil-in-Water Emulsions

In this article, the effects of various operating factors on the surface tension, viscosity, and stability of two heavy oil types in water emulsions for pipeline transportation are studied using the Taguchi experimental design approach. The surface tension of heavy crude oil-in-water emulsion is decreased by increasing the emulsifier concentration while the stability of emulsions is increased. The viscosity and stability are increased by an increase in oil content. An increase in the salinity and mixing speed leads to an increase in the stability of emulsion.     

Formulation and Optimization by Experimental Design of Low-Fat Mayonnaise Based on Soy Lecithin and Whey

The main objective of this study is to develop a new formula for a diet mayonnaise-like sauce without cholesterol. Emulsifying power is provided by the use of soy lecithin and the total fat content was limited to 16%. Droplet size measurement of employed mayonnaise samples at different times show that the largest diameter of fat does not exceed 18.5 µm with a yield stress of 56.1 Pa. Results of stability to centrifugation reveal that the absence of the supernatant oily layer ensures the stability of the emulsion. Using the experimental design method, the number of trials can be limited to a number of 16 experiments, and best formulation of the mayonnaise (without cholesterol) was obtained.     

Extraction of Priority Pollutant 4-Nitrophenol from Water by Emulsion Liquid Membrane: Emulsion Stability,Effect of Operational Conditions and Membrane Reuse

This work aims to the extraction of the priority pollutant 4-nitrophenol (4-NP) from water by emulsion liquid membrane (ELM). Liquid membrane consists of a diluent (hexane) and a surfactant (Span 80). Sodium carbonate solution was used as internal aqueous phase. Effects of important experimental conditions governing the stability of the W/O emulsion were investigated. Influence of operating parameters that affects the permeation of 4-NP such as surfactant concentration, emulsification time, sulfuric acid concentration in external phase, acid type in external phase, internal phase concentration, type of internal phase, stirring speed, volume ratio of internal phase to membrane phase, treatment ratio, 4-NP initial concentration, and diluent type was examined. This study also evaluated the effect of Na₂CO₃ concentration in the internal aqueous phase on the stripping of 4-NP. Additionally, the reuse of the recovered membrane was studied. Under most favorable conditions, practically all the 4-NP and aniline (AN) molecules present in the feed phase were extracted. The recovery of the membrane phase was total and the extraction of 4-NP was not decreased. The ELM treatment process represents a very interesting advanced separation process for the removal of 4-NP and AN from aqueous solutions.     

Gelation Studies: Comparison of the Critical Exponents Obtained by Dynamic Light Scattering and Rheology, 2

Summary: The sol–gel transition of two thermoreversible gelling mixtures made of xanthan gum and locust‐bean gum has been studied by using in situ, time‐resolved dynamic light scattering (DLS) and in situ rheology. A critical dynamical behavior was observed near the sol–gel transition, which was characterized by the presence of power‐law spectra over three and four decades in the time‐intensity correlation function g₂(t) − 1 ∼ t^−μ and over four and three decades in the oscillatory shear experiment G′(ω) ∼ G″(ω) ∼ ωⁿ. A comparison of the critical exponents obtained (μ₁ ≈ 0.36, μ₂ ≈ 0.32 and n₁ ≈ 0.62, n₂ ≈ 0.67) was made as a function of the dependence of the two mixing ratios according to the theory by Doi and Onuki. New experiments were also performed to compare the critical exponents on such a thermoreversible system.

Double‐logarithmic plot of the time‐intensity correlation functions g₂(t) − 1 versus the delay time, t, at a 90° scattering angle and at several temperatures of the mixture 1.     

Effects of Salts Containing Mono-, Di-, and Trivalent Ions on Electrical and Rheological Properties of Oil-Water Interface in Presence of Cationic Surfactant: Importance in the Stability of Oil-in-Water Emulsions

Many industrial applications of oil-in-water emulsions involve salts containing ions of different valence. The properties of the oil-water interface (e.g., interfacial tension, zeta potential and interfacial shear viscosity) are strongly influenced by the presence of these salts. This work investigates the role of NaCl, CaCl₂ and AlCl₃ on these properties of the hexane-water interface in presence of a cationic surfactant, viz., hexadecyltrimethylammonium bromide. Addition of salt enhanced the adsorption of surfactant molecules at the hexane-water interface, which increased the interfacial charge density, and consequently, the zeta potential. Interfacial shear viscosity significantly decreased in the presence of salt. The effectiveness of salt at a given concentration was in the sequence: AlCl₃ > CaCl₂ > NaCl. The hexane-in-water emulsions coarsened with time due to the coalescence of hexane droplets. The increase in droplet size with time was analyzed by a model based on the frequency of rupture of the thin aqueous film. The rate constants for coalescence were determined. The rate of coalescence increased in presence of salt.      

Chiral Discrimination of Mexiletine Enantiomers by Capillary Electrophoresis Using Cyclodextrins as Chiral Selectors and Experimental Design Method Optimization

Mexiletine (MXL) is a class IB antiarrhythmic agent, acting as a non-selective voltage-gated sodium channel blocker, used in therapy as a racemic mixture R,S-MXL hydrochloride. The aim of the current study was the development of a new, fast, and efficient method for the chiral separation of MXL enantiomers using capillary electrophoresis (CE) and cyclodextrins (CDs) as chiral selectors (CSs). After an initial CS screening, using several neutral and charged CDs, at four pH levels, heptakis-2,3,6-tri-O-methyl-β-CD (TM-β-CD), a neutral derivatized CD, was chosen as the optimum CS for the enantioseparation. For method optimization, an initial screening fractional factorial design was applied to identify the most significant parameters, followed by a face-centered central composite design to establish the optimal separation conditions. The best results were obtained by applying the following optimized electrophoretic conditions: 60 mM phosphate buffer, pH 5.0, 50 mM TM-β-CD, temperature 20 °C, applied voltage 30 kV, hydrodynamic injection 50 mbar/s. MXL enantiomers were baseline separated with a resolution of 1.52 during a migration time of under 5 min; S-MXL was the first migrating enantiomer. The method’s analytical performance was verified in terms of precision, linearity, accuracy, and robustness (applying a Plackett–Burman design). The developed method was applied for the determination of MXL enantiomers in pharmaceuticals. A computer modeling of the MXL-CD complexes was applied to characterize host–guest chiral recognition.     

Packed Column SFC of Gas Oils. Part II: Experimental Design Optimization of the Group-Type Analysis using CO2-SF6 as the Mobile Phase

An optimization procedure is presented for group-type analysis of diesel fuel by supercritical fluid chromatography using packed silica column and a mixed mobile phase. A set of five responses, four values of resolution of a performance mixture and analysis time, was modeled using a Doehlert matrix for experimental design. Optimized experimental conditions for the five responses were obtained from a response surfaces optimization, taking into account various constraints on SF₆ content in mobile phase and analysis time. The predicted and experimental resolutions were in good agreement for the different optimized conditions and one of them was selected to for application to a given diesel fuel for comparison with the results obtained by SFC using pure CO₂ and by HPLC. The conditions found in this study provide an alternative method for the determination of mono-, di-, and polyaromatic compounds in middle distillates.     

Molar Mass,Radius of Gyration and Second Virial Coefficient from new Static Light Scattering Equations for Dilute Solutions: Application to 21 (Macro)molecules

New equations for static light scattering of dilute binary solutions allow molar mass determination of macromolecules from measurements of scattered intensity ratios between solution and solvent (I_r). In contrast to the standard Carr–Zimm equations, they do not rely on the experimental absolute value of the Rayleigh ratio of a reference liquid. The picture shows a typical plot for the surfactant BRIJ72 in CH₂Cl₂ (M_Supplier=0.359 kg mol^?1).

     

Supercritical Fluid Extraction (SFE) Optimization by Full-Factorial Design for the Determination of Irganox 1076, Irgafos 168, and Chimassorb 81 in Virgin and Recycled Polyolefins

The performance and feasibility of supercritical fluid extraction (SFE) applied to the extraction of some antioxidants (Irganox 1076, Irgafos 168) and one UV-stabilizer (Chimassorb 81) from both virgin and recycled low density polyethylene (LDPE), and virgin high density polyethylene (HDPE) are studied. Due to the high number of variables a full-factorial design has been applied to minimize the number of experiments required to reach the optimum extraction conditions. Further analysis has been carried out off-line by reversed-phase HPLC. Modification of the physical properties of the polymeric matrix and increased number of recycling cycles as well as the influence of physical properties on the efficiency of SFE are also discussed.     

Prediction of Stability for Polychlorinated Biphenyls in Transformer Insulation Oil Through Three-dimensional Quantitative Structure-activity Relationship Pharmacophore Model and Full Factor Experimental Design

Based on the obtained data of half-lives(t_1/2) for 31 polychlorinated biphenyl congeners(PCBs), 3D quantitative structure-activity relationship(QSAR) pharmacophore was used to establish a 3D QSAR model to predict the t_1/2 values of the remaining 178 PCBs, using the structural parameters as independent variables and lgt_1/2 values as the dependent variable. Among this process, the whole data set(31 compounds) was divided into a training set(24 compounds) for model generation and a test set(7 compounds) for model validation. Then, the full factor experimental design was used to research the potential second-order interactional effect between different substituent positions, obtaining the final regulation scheme for PCB. At last, a 3D QSAR pharmacophore model was established to validate the reasonable regulation targeting typical PCB with respect to half-lives and thermostability. As a result, the cross-validation correlation coefficient(q²) obtained by the 3D QSAR model was 0.845(>0.5) and the coefficient of determination(r²) obtained was 0.936(>0.9), indicating that the models were robust and predictive. CoMSIA analyses upon steric, electrostatic and hydrophobic fields were 0.7%, 85.9%, and 13.4%, respectively. The electrostatic field was determined to be a primary factor governing the t_1/2. From CoMSIA contour maps, t_1/2 increased when substi- tuents possessed electropositive groups at the 2'-, 3-, 3'-, 5- and 5'- positions and electronegative groups at the 3-, 3'-, 5-, 6- and 6'- positions, which could increase the PCB stability in transformer insulation oil. Modification of two typical PCB congeners(PCB-77 and PCB-81) showed that the lgt_1/2for three selected modified compounds increased by 13%(average ratio) compared with that of each congener and the thermostability of them were higher, validating the reasonability of the regulatory scheme obtained from the 3D QSAR model. These results are expected to be beneficial in predicting t_1/2 values of PCB homologues and derivatives and in providing a theoretical foundation for further elucidation of the stability of PCBs.     

基于深度学习的“实验方案设计”主题式复习教学——以“阿司匹林的制备和提纯”为例

针对实验方案设计题的得分率分析和教学现状,基于课程标准、教材、真题和文献研究,构建“阿司匹林的制备和提纯”深度学习主题模型。通过设计制备和提纯阿司匹林的实验方案,构建实验方案设计的思维模型,并以制备七水合硫酸锌为例内化思维模型,在解决真实、复杂的问题过程中实现核心知识结构化,生成指向深度学习的主题式复习教学流程。     

Optimization of Extraction or Purification Process of Multiple Components from Natural Products: Entropy Weight Method Combined with Plackett–Burman Design and Central Composite Design

In this paper, the optimization of the extraction/purification process of multiple components was performed by the entropy weight method (EWM) combined with Plackett–Burman design (PBD) and central composite design (CCD). We took the macroporous resin purification of Astragalus saponins as an example to discuss the practicability of this method. Firstly, the weight of each component was given by EWM and the sum of the product between the componential content and its weight was defined as the comprehensive score, which was taken as the evaluation index. Then, the single factor method was adopted for determining the value range of each factor. PBD was applied for screening the significant factors. Important variables were further optimized by CCD to determine the optimal process parameters. After the combination of EWM, PBD and CCD, the resulting optimal purification conditions were as follows: pH value of 6.0, the extraction solvent concentration of 0.15 g/mL, and the ethanol volume fraction of 75%. Under the optimal conditions, the practical comprehensive score of recoveries of saponins was close to the predicted value (n = 3). Therefore, the present study provided a convenient and efficient method for extraction and purification optimization technology of multiple components from natural products.     

银-铜-铁-镍体系测定条件的旋转设计优化和目标转换因子分析法的同时测定

利用二次通用旋转组合设计的方法 ,建立了吸光度与显色剂、增敏剂用量以及p H值之间的数学模型 ,进而得到使吸光度最大的显色剂用量、增敏剂用量及 p H值。在此优化的基础上 ,用目标转换因子分析分光光度法对银、铜、铁、镍的合成样品的合谱进行了解析处理 ,得到较为满意的结果。     

Microwave-Assisted Extraction of Curcuma longa L. Oil: Optimization,Chemical Structure and Composition,Antioxidant Activity and Comparison with Conventional Soxhlet Extraction

Curcuma root (Curcuma longa L.) is a very important plant in gastronomy and medicine for its unique antiseptic, anti-inflammatory, antimicrobial and antioxidant properties. Conventional methods for the extraction of curcuma oil require long extraction times and high temperatures that can degrade the active substances. Therefore, the objectives of the present study were: (i) first, to optimize the extraction yield of curcuma oil by applying a Box-Behnken experimental design using surface response methodology to the microwave-assisted extraction (MAE) technique (the independent variables studied were reaction time (10–30 min), microwave power (150–200 W) and curcuma powder/ethanol ratio (1:5–1:20; w/v); and, (ii) second, to assess the total phenolic content (TPC) and their antioxidant activity of the oil (at the optimum conditions point) and compare with the conventional Soxhlet technique. The optimum conditions for the MAE were found to be 29.99 min, 160 W and 1:20 w/v to obtain an optimum yield of 10.32%. Interestingly, the oil extracted by microwave-assisted extraction showed higher TPC and better antioxidant properties than the oil extracted with conventional Soxhlet technique. Thus, it was demonstrated that the method applied for extraction influences the final properties of the extracted Curcuma longa L. oil.     

Supercritical CO2 Extraction of High-Added Value Compounds from Chlorella vulgaris: Experimental Design,Modelling and Optimization

Microalgae are well-known for their high-added value compounds and their recovery is currently of great interest. The aim of this work is the recovery of such components from Chlorella vulgaris through supercritical fluid extraction (SFE) with CO₂. The effect of the extraction temperature (40–60 °C), pressure (110–250 bar), and solvent flow rate (20–40 g/min) was tested on yield, the extract’s antioxidant activity, and the phenolic, chlorophyll and carotenoid content. Thus, data analysis indicated that the yield was mainly affected by temperature, carotenoids by pressure, while the extract’s phenolics and antioxidant activity were affected by the synergy of temperature and pressure. Moreover, SFE’s kinetic study was performed and experimental data were correlated using Sovová’s mass transfer-based model. SFE optimization (60 °C, 250 bar, 40 g/min) led to 3.37% w/w yield, 44.35 mg_extr/mg_DPPH antioxidant activity (IC50), 18.29 mg_GA/g_extr total phenolic content, 35.55, 21.14 and 10.00 mg/g_extr total chlorophyll, carotenoid and selected carotenoid content (astaxanthin, lutein and β-carotene), respectively. A comparison of SFE with conventional aq. ethanol (90% v/v) extraction proved SFE’s superiority regarding extraction duration, carotenoids, antioxidant activity and organoleptic characteristics of color and odor despite the lower yield. Finally, cosolvent addition (ethanol 10% w/w) at optimum SFE conditions improved the extract’s antioxidant activity (19.46%) as well as yield (101.81%).     

Fabrication and Characterization of β-Cyclodextrin/Mosla Chinensis Essential Oil Inclusion Complexes: Experimental Design and Molecular Modeling

Essential oils (EOs) are primarily isolated from medicinal plants and possess various biological properties. However, their low water solubility and volatility substantially limit their application potential. Therefore, the aim of the current study was to improve the solubility and stability of the Mosla Chinensis (M. Chinensis) EO by forming an inclusion complex (IC) with β-cyclodextrin (β-CD). Furthermore, the IC formation process was investigated using experimental techniques and molecular modeling. The major components of M. Chinensis ‘Jiangxiangru’ EOs were carvacrol, thymol, o-cymene, and terpinene, and its IC with β-CD were prepared using the ultrasonication method. Multivariable optimization was studied using a Plackett-Burman design (step 1, identifying key parameters) followed by a central composite design for optimization of the parameters (step 2, optimizing the key parameters). SEM, FT-IR, TGA, and dissolution experiments were performed to analyze the physicochemical properties of the ICs. In addition, the interaction between EO and β-CD was further investigated using phase solubility, molecular docking, and molecular simulation studies. The results showed that the optimal encapsulation efficiency and loading capacity of EO in the ICs were 86.17% and 8.92%, respectively. Results of physicochemical properties were different after being encapsulated, indicating that the ICs had been successfully fabricated. Additionally, molecular docking and dynamics simulation showed that β-CD could encapsulate the EO component (carvacrol) via noncovalent interactions. In conclusion, a comprehensive methodology was developed for determining key parameters under multivariate conditions by utilizing two-step optimization experiments to obtain ICs of EO with β-CD. Furthermore, molecular modeling was used to study the mechanisms involved in molecular inclusion complexation.