Search results for: liquid chromatography-mass spectrometry

Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

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The process of assembling metal nanoparticles at the interface of two liquids has received a great interest over the past few years due to a wide range of important applications and their unusual properties compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: firstly, to describe the achievement of a closed loop recycling for producing cadmium sulphide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulphides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be applied to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferro-fluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Noble metal like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: assembling nanoparticles, liquid/liquid interface, thin film, core/shell, solar cells, recording media

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Authors: Mohammad R. Jalali

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Movement of liquid with a free surface in a container is known as slosh. For instance, slosh occurs when water in a closed tank is set in motion by a free surface displacement, or when liquid natural gas in a container is vibrated by an external driving force, such as an earthquake or movement induced by transport. Slosh is also derived from resonant switching of a natural basin. During sloshing, different types of motion are produced by energy exchange between the liquid and its container. In present study, a numerical model is developed to simulate the nonlinear even harmonic oscillations of free surface sloshing of an initial disturbance to the free surface of a liquid in a closed square basin. The response of the liquid free surface is affected by amplitude and motion frequencies of its container; therefore, sloshing involves complex fluid-structure interactions. In the present study, nonlinear interaction of free surface sloshing of an initial Gaussian hump with its uneven container is predicted numerically. For this purpose, Green-Naghdi (GN) equations are applied as governing equation of fluid field to produce nonlinear second-order and higher-order wave interactions. These equations reduce the dimensions from three to two, yielding equations that can be solved efficiently. The GN approach assumes a particular flow kinematic structure in the vertical direction for shallow and deep-water problems. The fluid velocity profile is finite sum of coefficients depending on space and time multiplied by a weighting function. It should be noted that in GN theory, the flow is rotational. In this study, GN numerical simulations of initial Gaussian hump are compared with Fourier series semi-analytical solutions of the linearized shallow water equations. The comparison reveals that satisfactory agreement exists between the numerical simulation and the analytical solution of the overall free surface sloshing patterns. The resonant free surface motions driven by an initial Gaussian disturbance are obtained by Fast Fourier Transform (FFT) of the free surface elevation time history components. Numerically predicted velocity vectors and magnitude contours for the free surface patterns indicate that interaction of Gaussian hump with its container has localized effect. The result of this sloshing is applicable to the design of stable liquefied oil containers in tankers and offshore platforms.

Keywords: fluid-structure interactions, free surface sloshing, Gaussian hump, Green-Naghdi equations, numerical predictions

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Authors: S. G. Vasantharaju, Viswanath Guptha, Raghavendra Shetty

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Introduction: Aminophylline is a methylxanthine derivative belonging to the class bronchodilator. From the literature survey, reported methods reveals the solid phase extraction and liquid liquid extraction which is highly variable, time consuming, costly and laborious analysis. Present work aims to develop a simple, highly sensitive, precise and accurate high-performance liquid chromatography method for the quantification of Aminophylline in rat plasma samples which can be utilized for preclinical studies. Method: Reverse Phase high-performance liquid chromatography method. Results: Selectivity: Aminophylline and the internal standard were well separated from the co-eluted components and there was no interference from the endogenous material at the retention time of analyte and the internal standard. The LLOQ measurable with acceptable accuracy and precision for the analyte was 0.5 µg/mL. Linearity: The developed and validated method is linear over the range of 0.5-40.0 µg/mL. The coefficient of determination was found to be greater than 0.9967, indicating the linearity of this method. Accuracy and precision: The accuracy and precision values for intra and inter day studies at low, medium and high quality control samples concentrations of aminophylline in the plasma were within the acceptable limits Extraction recovery: The method produced consistent extraction recovery at all 3 QC levels. The mean extraction recovery of aminophylline was 93.57 ± 1.28% while that of internal standard was 90.70 ± 1.30%. Stability: The results show that aminophylline is stable in rat plasma under the studied stability conditions and that it is also stable for about 30 days when stored at -80˚C. Pharmacokinetic studies: The method was successfully applied to the quantitative estimation of aminophylline rat plasma following its oral administration to rats. Discussion: Preclinical studies require a rapid and sensitive method for estimating the drug concentration in the rat plasma. The method described in our article includes a simple protein precipitation extraction technique with ultraviolet detection for quantification. The present method is simple and robust for fast high-throughput sample analysis with less analysis cost for analyzing aminophylline in biological samples. In this proposed method, no interfering peaks were observed at the elution times of aminophylline and the internal standard. The method also had sufficient selectivity, specificity, precision and accuracy over the concentration range of 0.5 - 40.0 µg/mL. An isocratic separation technique was used underlining the simplicity of the presented method.

Keywords: Aminophyllin, preclinical pharmacokinetics, rat plasma, RPHPLC

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Authors: Wasim Sajjad, Manzoor Ahmad, Sundas Qadir, Muhammad Rafiq, Fariha Hasan, Richard Tehan, Kerry L. McPhail, Aamer Ali Shah

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Aim: This study aims to investigate the possible radiation protective role of a compatible solute in the tolerance of radio-halophilic bacterium against stresses, like desiccation and exposure to ionizing radiation. Methods and Results: Nine different radio-resistant bacteria were isolated from desert soil, where strain WMA-LM19 was chosen for detailed studies on the basis of its high tolerance for ultraviolet radiation among all these isolates. 16S rRNA gene sequencing indicated that the bacterium was closely related to Stenotrophomonas sp. (KT008383). A bacterial milking strategy was applied for extraction of intracellular compatible solutes in 70% (v/v) ethanol, which were purified by high-performance liquid chromatography (HPLC). The compound was characterized as ectoine by 1H and 13C nuclear magnetic resonance (NMR), and mass spectrometry (MS). Ectoine demonstrated more efficient preventive activity (54.80%) to erythrocyte membranes and also inhibited oxidative damage to proteins and lipids in comparison to the standard ascorbic acid. Furthermore, a high level of ectoine-mediated protection of bovine serum albumin against ionizing radiation (1500-2000 Jm-2) was observed, as indicated by sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) analysis. Conclusion: The results indicated that ectoine can be used as a potential mitigator and radio-protective agent to overcome radiation- and salinity-mediated oxidative damage in extreme environments. Significance and Impact of the Study: This study shows that ectoine from radio-halophiles can be used as a potential source in topical creams as sunscreen. The investigation of ectoine as UV protectant also changes the prospective that radiation resistance is specific only to molecular adaptation.

Keywords: ectoine, anti-oxidant, stenotrophomonas sp., ultraviolet radiation

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Authors: Soomal Hamza, Uzma Imran

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Organochlorine pesticides bio-accumulate into the fat of fish, birds, and animals through which it enters the human food cycle. Due to their persistence and stability in the environment, many health impacts are associated with them, most of which are carcinogenic in nature. In this study, the level of organochlorine pesticides has been detected in Keenjhar Lake and remediated using Rhizoremediation technique. 14 OC pesticides namely, Aldrin, Deldrin, Heptachlor, Heptachlor epoxide, Endrin, Endosulfun I and II, DDT, DDE, DDD, Alpha, Beta, Gamma BHC and two plants namely, Water Hyacinth and Slvinia Molesta were used in the system using pot experiment which processed for 11 days. A consortium was inoculated in both plants to increase its efficiency. Water samples were processed using liquide-liquid extraction. Sediments and roots samples were processed using Soxhlet method followed by clean-up and Gas Chromatography. Delta-BHC was the predominantly found in all samples with mean concentration (ppb) and standard deviation of 0.02 ± 0.14, 0.52 ± 0.68, 0.61 ± 0.06, in Water, Sediments and Roots samples respectively. The highest levels were of Endosulfan II in the samples of water, sediments and roots. Water Hyacinth proved to be better bioaccumulaor as compared to Silvinia Molesta. The pattern of compounds reduction rate by the end of experiment was Delta-BHC>DDD > Alpha-BHC > DDT> Heptachlor> H.Epoxide> Deldrin> Aldrin> Endrin> DDE> Endosulfun I > Endosulfun II. Not much significant difference was observed between the pots with the consortium and pots without the consortium addition. Phytoremediation is a promising technique, but more studies are required to assess the bioremediation potential of different aquatic plants and plant-endophyte relationship.

Keywords: aquatic plant, bio remediation, gas chromatography, liquid liquid extraction

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Authors: Pradeep G. Siddheshwar, K. M. Lakshmi

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The present study deals with weakly non-linear stability analysis of Rayleigh-Benard-Brinkman convection in nanoliquid-saturated porous enclosures. The modified-Buongiorno-Brinkman model (MBBM) is used for the conservation of linear momentum in a nanoliquid-saturated-porous medium under the assumption of Boussinesq approximation. Thermal equilibrium is imposed between the base liquid and the nanoparticles. The thermophysical properties of nanoliquid are modeled using phenomenological laws and mixture theory. The fifth-order Lorenz model is derived for the problem and is then reduced to the first-order Ginzburg-Landau equation (GLE) using the multi-scale method. The analytical solution of the GLE for the amplitude is then used to quantify the heat transport in closed form, in terms of the Nusselt number. It is found that addition of dilute concentration of nanoparticles significantly enhances the heat transport and the dominant reason for the same is the high thermal conductivity of the nanoliquid in comparison to that of the base liquid. This aspect of nanoliquids helps in speedy removal of heat. The porous medium serves the purpose of retainment of energy in the system due to its low thermal conductivity. The present model helps in making a unified study for obtaining the results for base liquid, nanoliquid, base liquid-saturated porous medium and nanoliquid-saturated porous medium. Three different types of enclosures are considered for the study by taking different values of aspect ratio, and it is observed that heat transport in tall porous enclosure is maximum while that of shallow is the least. Detailed discussion is also made on estimating heat transport for different volume fractions of nanoparticles. Results of single-phase model are shown to be a limiting case of the present study. The study is made for three boundary combinations, viz., free-free, rigid-rigid and rigid-free.

Keywords: Boungiorno model, Ginzburg-Landau equation, Lorenz equations, porous medium

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Authors: Yumei Wang, Xiaoyu Xu, Li Lu

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Solid-state battery adopts solid-state electrolyte such as oxide- and composite-based solid electrolytes. With the adaption of nonflammable or less flammable solid electrolytes, the safety of solid-state batteries can be largely increased. NASICON (Na₃Zr₂Si₂PO₁₂, NZSP) is one of the sodium ion conductors that possess relatively high ionic conductivity, wide electrochemical stable range and good chemical stability. Therefore, it has received increased attention. We report the development of high-density NZSP through liquid phase sintering and its organic-inorganic composite electrolyte. Through reactive liquid phase sintering, the grain boundary conductivity can be largely enhanced while using an organic-inorganic composite electrolyte, interfacial wetting and impedance can be largely reduced hence being possible to fabricate scalable solid-state batteries.

Keywords: solid-state electrolyte, composite electrolyte, electrochemical performance, conductivity

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Authors: A. Cervantes-Diaz, B. Sevilla-Moran, Manuel Alcami, Al Mokhtar Lamsabhi, J. L. Alonso-Prados, P. Sandin-España

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Profoxydim is a post-emergence herbicide belonging to the cyclohexanedione oxime family, used to control weeds in rice crops. The use of soil organic amendments has increased significantly in the last decades, and their effects on the behavior of many herbicides are still unknown. Additionally, it is known that photolysis is an important degradation process to be considered when evaluating the persistence of this family of herbicides in the environment. In this work, the photodegradation of profoxydim in an amended paddy soil-water system with alperujo compost was studied. Photodegradation experiments were carried out under laboratory conditions using simulated solar light (Suntest equipment) in order to evaluate the reaction kinetics of the active substance. The photochemical behavior of profoxydim was investigated in soil with and without alperujo amendment. Furthermore, due to the rice crop characteristics, profoxydim photodegradation in water in contact with these types of soils was also studied. Determination of profoxydim degradation kinetics was performed by High-Performance Liquid Chromatography with Diode-Array Detection (HPLC-DAD). Furthermore, we followed the evolution of resulting transformation by-products, and their tentative identification was achieved by mass spectrometry. All the experiments allowed us to fit the data of profoxydim photodegradation to a first-order kinetic. Photodegradation of profoxydim was very rapid in all cases. The half-lives in aqueous matrices were in the range of 86±0.3 to 103±0.5 min. The addition of alperujo amendment to the soil produced an increase in the half-life from 62±0.2 min (soil) to 75±0.3 min (amended soil). In addition, a comparison to other organic amendments was also performed. Results showed that the presence of the organic amendment retarded the photodegradation in paddy soil and water. Regarding degradation products, the main process involved was the cleavage of the oxime moiety giving rise to the formation of the corresponding imine compound.

Keywords: by-products, herbicide, organic amendment, photodegradation, profoxydim

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Authors: Makhlouf Mourad, Medkour Mihoub, Bouchher Omar, Messabih Sidi Mohamed, Benrachedi Khaled

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This work is the modeling and simulation of fluid flow (liquid) through porous media. This type of flow occurs in many situations of interest in applied sciences and engineering, fluid (oil) consists of several individual substances in pure, single-phase flow is incompressible and isothermal. The porous medium is isotropic, homogeneous optionally, with the rectangular format and the flow is two-dimensional. Modeling of hydrodynamic phenomena incorporates Darcy's law and the equation of mass conservation. Correlations are used to model the density and viscosity of the fluid. A finite volume code is used in the discretization of differential equations. The nonlinearity is treated by Newton's method with relaxation coefficient. The results of the simulation of the pressure and the mobility of liquid flowing through porous media are presented, analyzed, and illustrated.

Keywords: Darcy equation, middle porous, continuity equation, Peng Robinson equation, mobility

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Authors: Ahmed Alkarimi, Kevin Welham

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Organic mixed mode monolithic columns were fabricated from; glycidyl methacrylate-co-ethylene dimethacrylate-co-stearyl methacrylate, using glycidyl methacrylate and stearyl methacrylate as co monomers representing 30% and 70% respectively of the liquid volume with ethylene dimethacrylate crosslinker and 2,2-dimethoxy-2-phenylacetophenone as the free radical initiator. The monomers were mixed with a binary porogenic solvent, comprising propan-1-ol, and methanol (0.825 mL each). The monolith was formed by photo polymerization (365 nm) inside a borosilicate glass tube (1.5 mm ID and 3 mm OD x 50 mm length). The monolith was observed to have formed correctly by optical examination and generated reasonable backpressure, approximately 650 psi at a flow rate of 0.2 mL min⁻¹ 50:50 acetonitrile: water. The morphological properties of the monolithic columns were investigated using scanning electron microscopy images, and Brunauer-Emmett-Teller analysis, the results showed that the monolith was formed properly with 19.98 ± 0.01 mm² surface area, 0.0205 ± 0.01 cm³ g⁻¹ pore volume and 6.93 ± 0.01 nm average pore size. The polymer monolith formed was further investigated using proton nuclear magnetic resonance, and Fourier transform infrared spectroscopy. The monolithic columns were investigated using high-performance liquid chromatography to test their ability to separate different samples with a range of properties. The columns displayed both hydrophobic/hydrophilic and hydrophobic/ion exchange interactions with the compounds tested indicating that true mixed mode separations. The mixed mode monolithic columns exhibited significant separation of proteins.

Keywords: LC separation, proteins separation, monolithic column, mixed mode

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Authors: Adriana Muñoz-Talavera, Ana Rosa Rincón-Sánchez, Abraham Escobedo-Moratilla, María Cristina Islas-Carbajal, Miguel Ángel Gómez-Lim

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The highest rates of diabetes incidence and prevalence worldwide will increase the number of diabetic patients requiring insulin or insulin analogues. Then, current production systems would not be sufficient to meet the future market demands. Therefore, developing efficient expression systems for insulin and insulin analogues are needed. In addition, insulin analogues with better pharmacokinetics and pharmacodynamics properties and without mitogenic potential will be required. SCI-57 (single chain insulin-57) is an insulin analogue having 10 times greater affinity to the insulin receptor, higher resistance to thermal degradation than insulin, native mitogenicity and biological effect. Plants as expression platforms have been used to produce recombinant proteins because of their advantages such as cost-effectiveness, posttranslational modifications, absence of human pathogens and high quality. Immunoglobulin production with a yield of 50% has been achieved by transient expression in Nicotiana benthamiana (Nb). The aim of this study is to produce SCI-57 by transient expression in Nb. Methodology: DNA sequence encoding SCI-57 was cloned in pICH31070. This construction was introduced into Agrobacterium tumefaciens by electroporation. The resulting strain was used to infiltrate leaves of Nb. In order to isolate SCI-57, leaves from transformed plants were incubated 3 hours with the extraction buffer therefore filtrated to remove solid material. The resultant protein solution was subjected to anion exchange chromatography on an FPLC system and ultrafiltration to purify SCI-57. Detection of SCI-57 was made by electrophoresis pattern (SDS-PAGE). Protein band was digested with trypsin and the peptides were analyzed by Liquid chromatography tandem-mass spectrometry (LC-MS/MS). A purified protein sample (20µM) was analyzed by ESI-Q-TOF-MS to obtain the ionization pattern and the exact molecular weight determination. Chromatography pattern and impurities detection were performed using RP-HPLC using recombinant insulin as standard. The identity of the SCI-57 was confirmed by anti-insulin ELISA. The total soluble protein concentration was quantified by Bradford assay. Results: The expression cassette was verified by restriction mapping (5393 bp fragment). The SDS-PAGE of crude leaf extract (CLE) of transformed plants, revealed a protein of about 6.4 kDa, non-present in CLE of untransformed plants. The LC-MS/MS results displayed one peptide with a high score that matches SCI-57 amino acid sequence in the sample, confirming the identity of SCI-57. From the purified SCI-57 sample (PSCI-57) the most intense charge state was 1069 m/z (+6) on the displayed ionization pattern corresponding to the molecular weight of SCI-57 (6412.6554 Da). The RP-HPLC of the PSCI-57 shows the presence of a peak with similar retention time (rt) and UV spectroscopic profile to the insulin standard (SCI-57 rt=12.96 and insulin rt=12.70 min). The collected SCI-57 peak had ELISA signal. The total protein amount in CLE from transformed plants was higher compared to untransformed plants. Conclusions: Our results suggest the feasibility to produce insulin analogue SCI-57 by transient expression in Nicotiana benthamiana. Further work is being undertaken to evaluate the biological activity by glucose uptake by insulin-sensitive and insulin-resistant murine and human cultured adipocytes.

Keywords: insulin analogue, mass spectrometry, Nicotiana benthamiana, transient expression

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Authors: M. Al Zallouha, Y. Landkocz, J. Brunet, R. Cousin, J. M. Halket, E. Genty, P. J. Martin, A. Verdin, D. Courcot, S. Siffert, P. Shirali, S. Billet

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Toluene is one of the most used Volatile Organic Compounds (VOCs) in the industry. Amongst VOCs, Benzene, Toluene, Ethylbenzene and Xylenes (BTEX) emitted into the atmosphere have a major and direct impact on human health. It is, therefore, necessary to minimize emissions directly at source. Catalytic oxidation is an industrial technique which provides remediation efficiency in the treatment of these organic compounds. However, during operation, the catalysts can release some compounds, called byproducts, more toxic than the original VOCs. The catalytic oxidation of a gas stream containing 1000ppm of toluene on Pd/α-Al2O3 can release a few ppm of benzene, according to the operating temperature of the catalyst. The development of new catalysts must, therefore, include chemical and toxicological validation phases. In this project, A549 human lung cells were exposed in air/liquid interface (Vitrocell®) to gas mixtures derived from the oxidation of toluene with a catalyst of Pd/α-Al2O3. Both exposure concentrations (i.e. 10 and 100% of catalytic emission) resulted in increased gene expression of Xenobiotics Metabolising Enzymes (XME) (CYP2E1 CYP2S1, CYP1A1, CYP1B1, EPHX1, and NQO1). Some of these XMEs are known to be induced by polycyclic organic compounds conventionally not searched during the development of catalysts for VOCs degradation. The increase in gene expression suggests the presence of undetected compounds whose toxicity must be assessed before the adoption of new catalyst. This enhances the relevance of toxicological validation of such systems before scaling-up and marketing.

Keywords: BTEX toxicity, air/liquid interface cell exposure, Vitrocell®, catalytic oxidation

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Authors: Deepa S N, Srinivasan a D, Veeramanju K T

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The power transformer is a critical equipment in the transmission and distribution network that must be managed to ensure uninterrupted power service. The liquid insulation is essential for the proper functioning of the transformer, as it serves as both coolant and insulating medium, which influences the transformer’s durability. Further, the insulating state of a power transformer has a significant impact on its reliability. Mineral oil derived from petroleum crude oil has been employed as liquid dielectrics for decades due to its superior functional characteristics, however as a resource for the same are getting depleted over the years. Research is undertaken across the globe to identify a viable substitute for mineral oil. Further, alternate insulating oils are being investigated for better environmental impact, biodegradability and economics. Several combinations of vegetable oil derived natural esters are being inspected by researchers across the globe in these domains. In this work, mineral oil is blended with soyabean oil with various proportions and dielectric properties such as dielectric breakdown voltage, relative permittivity, dissipation factor, viscosity, flash and fire point have been investigated according to international standards. A quantitative comparison is made among various samples and is observed that the blended oil sample of equal proportion of mineral oil and soyabean oil, MO50+SO50 exhibits superior dielectric properties such as breakdown voltage of 65kV, dissipation factor of 0.0044, relative permittivity of 3.1680 that are closer to the range of values recommended for power transformer applications. Also, Breakdown voltage values of all the investigated oil samples obeyed the Weibull and Normal probability distribution.

Keywords: blended oil, dielectric breakdown, liquid insulation, power transformer

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Authors: Ehsan Atefi, Michael Grigware

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Respiratory failure secondary to surfactant deficiency resulting from respiratory distress syndrome is considered one major cause of morbidity in preterm infants. Surfactant replacement treatment (SRT) is considered an effective treatment for this disease. Here, we introduce an AI-mediated approach for estimating the distribution of surfactant in the lung airway of a newborn infant during SRT. Our approach implements machine learning to precisely estimate the splitting ratio of a liquid drop during bifurcation at different injection velocities and patient orientations. This technique can be used to calculate the surfactant residue remaining on the airway wall during the surfactant injection process. Our model works by minimizing the pressure drop difference between the two airway branches at each generation, subject to mass and momentum conservation. Our platform can be used to generate feedback for immediately adjusting the velocity of injection and patient orientation during SRT.

Keywords: respiratory failure, surfactant deficiency, surfactant replacement, machine learning

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Authors: Layla El Gaini, Majdouline Belaqziz, Meriem Outaki, Mariam Minhaj

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In this study, it introduce and validate a high-performance liquid chromatography method with diode-array detection (HPLC-DAD) specifically designed for the accurate quantification of caffeic acid in phenolic extracts obtained from olive mill wastewater. The separation process of caffeic acid was effectively achieved through the use of an Acclaim Polar Advantage column (5µm, 250x4.6mm). A meticulous multi-step gradient mobile phase was employed, comprising water acidified with phosphoric acid (pH 2.3) and acetonitrile, to ensure optimal separation. The diode-array detection was adeptly conducted within the UV–VIS spectrum, spanning a range of 200–800 nm, which facilitated precise analytical results. The method underwent comprehensive validation, addressing several essential analytical parameters, including specificity, repeatability, linearity, as well as the limits of detection and quantification, alongside measurement uncertainty. The generated linear standard curves displayed high correlation coefficients, underscoring the method's efficacy and consistency. This validated approach is not only robust but also demonstrates exceptional reliability for the focused analysis of caffeic acid within the intricate matrices of wastewater, thus offering significant potential for applications in environmental and analytical chemistry.

Keywords: high-performance liquid chromatography (HPLC-DAD), caffeic acid analysis, olive mill wastewater phenolics, analytical method validation

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Authors: N. S. Achour, M. Hamdaoui, S. Ben Nasrallah, A. Perwuelz

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The main idea of this work is to investigate the effect of knitted fabrics characteristics on moisture management properties. Wetting and transport properties of single jersey, Rib 1&1 and English Rib fabrics made out of cotton and blended Cotton/Polyester yarns were studied. The dynamic water sorption of fabrics was investigated under same isothermal and terrestrial conditions at 20±2°C-65±2% by using the Moisture Management Tester (MMT) which can be used to quantitatively measure liquid moisture transfer in one step in a fabric in multi directions: Absorption rate, moisture absorbing time of the fabric's inner and outer surfaces, one-way transportation capability, the spreading/drying rate, the speed of liquid moisture spreading on fabric's inner and outer surfaces are measured, recorded and discussed. The results show that fabric’s composition and knit’s structure have a significant influence on those phenomena.

Keywords: knitted fabrics characteristics, moisture management properties, multi directions, the moisture management tester

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Authors: Shilpa K. Nandwani, Mousumi Chakraborty, Smita Gupta

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When selecting surfactants for surfactant flooding during enhanced oil recovery, the most important criteria is that the surfactant system should reduce the interfacial tension between water and oil to ultralow values. In the present study, a mixture of ionic liquid surfactant and commercially available binding agent sodium tosylate has been used as a surfactant mixture. Presence of wormlike micelles indicates the possibility of achieving ultralow interfacial tension. Surface tension measurements of the mixed surfactant system have been studied. The emulsion size distribution of the mixed surfactant system at varying salinities has been studied. It has been found that at high salinities the viscoelastic surfactant system loses their efficacy and degenerate. Hence the given system may find application in low salinity reservoirs, providing good mobility to the flood during tertiary oil recovery process.

Keywords: ionic liquis, interfacial tension, Na-tosylate, viscoelastic surfactants

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Authors: Hamza Javar Magnier, Leslie V. Woodcock

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We report extensive molecular dynamics (MD) computational investigations into the thermodynamic description of supercritical properties for a model fluid that is the simplest realistic representation of atoms or molecules. The pair potential is a hard-sphere repulsion of diameter σ with a very short attraction of length λσ. When λ = 1.005 the range is so short that the model atoms are referred to as “adhesive spheres”. Molecular dimers, trimers …etc. up to large clusters, or droplets, of many adhesive-sphere atoms are unambiguously defined. This then defines percolation transitions at the molecular level that bound the existence of gas and liquid phases at supercritical temperatures, and which define the existence of a supercritical mesophase. Both liquid and gas phases are seen to terminate at the loci of percolation transitions, and below a second characteristic temperature (Tc2) are separated by the supercritical mesophase. An analysis of the distribution of clusters in gas, meso- and liquid phases confirms the colloidal nature of this mesophase. The general phase behaviour is compared with both experimental properties of the water-steam supercritical region and also with formally exact cluster theory of Mayer and Mayer. Both are found to be consistent with the present findings that in this system the supercritical mesophase narrows in density with increasing T > Tc and terminates at a higher Tc2 at a confluence of the primary percolation loci. The expended plot of the MD data points in the mesophase of 7 critical and supercritical isotherms in highlight this narrowing in density of the linear-slope region of the mesophase as temperature is increased above the critical. This linearity in the mesophase implies the existence of a linear combination rule between gas and liquid which is an extension of the Lever rule in the subcritical region, and can be used to obtain critical parameters without resorting to experimental data in the two-phase region. Using this combination rule, the calculated critical parameters Tc = 0.2007 and Pc = 0.0278 are found be agree with the values found by of Largo and coworkers. The properties of this supercritical mesophase are shown to be consistent with an alternative description of the phenomenon of critical opalescence seen in the supercritical region of both molecular and colloidal-protein supercritical fluids.

Keywords: critical opalescence, supercritical, square-well, percolation transition, critical parameters.

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Authors: M. A. El-Sayed, S. A. Aziz

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Centrifugal casting is a standard casting technique for the manufacture of hollow, intricate and sound castings without the use of cores. The molten metal or alloy poured into the rotating mold forms a hollow casting as the centrifugal forces lift the liquid along the mold inner surface. The rotational speed of the die was suggested to greatly affect the manner in which the molten metal flows within the mould and consequently the probability of the formation of a uniform cylinder. In this work the flow of the liquid metal at various speeds and its effect during casting were studied. The results suggested that there was a critical range for the speed, within which the produced castings exhibited best uniformity and maximum mechanical properties. When a mould was rotated at speeds below or beyond the critical range defects were found in the final castings, which affected the uniformity and significantly lowered the mechanical properties.

Keywords: centrifugal casting, rotational speed, critical speed range, mechanical properties

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Authors: Hemant Upadhyay, Tarun Kumar Kundu

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It is utmost important for a blast furnace operator to understand the mechanisms governing the liquid flow, accumulation, drainage and heat transfer between various phases in blast furnace hearth for a stable and efficient blast furnace operation. Abnormal drainage behavior may lead to high liquid build up in the hearth. Operational problems such as pressurization, low wind intake, and lower material descent rates, normally be encountered if the liquid levels in the hearth exceed a critical limit when Hearth coke and Deadman start to float. Similarly, hot metal temperature is an important parameter to be controlled in the BF operation; it should be kept at an optimal level to obtain desired product quality and a stable BF performance. It is not possible to carry out any direct measurement of above due to the hostile conditions in the hearth with chemically aggressive hot liquids. The objective here is to develop a mathematical model to simulate the variation in hot metal / slag accumulation and temperature during the tapping of the blast furnace based on the computed drainage rate, production rate, mass balance, heat transfer between metal and slag, metal and solids, slag and solids as well as among the various zones of metal and slag itself. For modeling purpose, the BF hearth is considered as a pressurized vessel, filled with solid coke particles. Liquids trickle down in hearth from top and accumulate in voids between the coke particles which are assumed thermally saturated. A set of generic mass balance equations gives the amount of metal and slag intake in hearth. A small drainage (tap hole) is situated at the bottom of the hearth and flow rate of liquids from tap hole is computed taking in account the amount of both the phases accumulated their level in hearth, pressure from gases in the furnace and erosion behaviors of tap hole itself. Heat transfer equations provide the exchange of heat between various layers of liquid metal and slag, and heat loss to cooling system through refractories. Based on all that information a dynamic simulation is carried out which provides real time information of liquids accumulation in hearth before and during tapping, drainage rate and its variation, predicts critical event timings during tapping and expected tapping temperature of metal and slag on preset time intervals. The model is in use at JSPL, India BF-II and its output is regularly cross-checked with actual tapping data, which are in good agreement.

Keywords: blast furnace, hearth, deadman, hotmetal

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Authors: Payman Davoodi-Nasab, Ahmad Rahbar-Kelishami, Jaber Safdari, Hossein Abolghasemi

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The high purity rare earth elements (REEs) have been vastly used in the field of chemical engineering, metallurgy, nuclear energy, optical, magnetic, luminescence and laser materials, superconductors, ceramics, alloys, catalysts, and etc. Neodymium is one of the most abundant rare earths. By development of a neodymium–iron–boron (Nd–Fe–B) permanent magnet, the importance of neodymium has dramatically increased. Solvent extraction processes have many operational limitations such as large inventory of extractants, loss of solvent due to the organic solubility in aqueous solutions, volatilization of diluents, etc. One of the promising methods of liquid membrane processes is emulsion liquid membrane (ELM) which offers an alternative method to the solvent extraction processes. In this work, a study on Nd extraction through multi-walled carbon nanotubes (MWCNTs) assisted ELM using response surface methodology (RSM) has been performed. The ELM composed of diisooctylphosphinic acid (CYANEX 272) as carrier, MWCNTs as nanoparticles, Span-85 (sorbitan triooleate) as surfactant, kerosene as organic diluent and nitric acid as internal phase. The effects of important operating variables namely, surfactant concentration, MWCNTs concentration, and treatment ratio were investigated. Results were optimized using a central composite design (CCD) and a regression model for extraction percentage was developed. The 3D response surfaces of Nd(III) extraction efficiency were achieved and significance of three important variables and their interactions on the Nd extraction efficiency were found out. Results indicated that introducing the MWCNTs to the ELM process led to increasing the Nd extraction due to higher stability of membrane and mass transfer enhancement. MWCNTs concentration of 407 ppm, Span-85 concentration of 2.1 (%v/v) and treatment ratio of 10 were achieved as the optimum conditions. At the optimum condition, the extraction of Nd(III) reached the maximum of 99.03%.

Keywords: emulsion liquid membrane, extraction of neodymium, multi-walled carbon nanotubes, response surface method

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Authors: Sagheer A. Onaizi

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The adsorption of anionic biosurfactant (surfactin) and anionic synthetic surfactant (sodium dodecylbenzenesulphonate, abbreviated as SDOBS) from phosphate buffer containing high concentrations of co- and counter-ions to the air-buffer interface has been investigated. The self-assembly of the two surfactants at the interface has been monitored through dynamic surface tension measurements. The equilibrium surface pressure-surfactant concentration data in the premicellar region were regressed using Gibbs adsorption equation. The predicted surface saturations for SDOBS and surfactin are and, respectively. The occupied area per an SDOBS molecule at the interface saturation condition is while that occupied by a surfactin molecule is. The surface saturations reported in this work for both surfactants are in a very good agreement with those obtained using expensive techniques such as neutron reflectometry, suggesting that the surface tension measurements coupled with appropriate theoretical analysis could provide useful information comparable to those obtained using highly sophisticated techniques.

Keywords: adsorption, air-liquid interface, biosurfactant, surface tension

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Authors: I. A. Ibrahim, T. A. Elbarbary, N. Abdelaty, A. T. Kandil, H. K. Farhan

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The present work aims to study the leaching of Abu Ghalaga ilmenite ore by hydrochloric acid and simultaneous reduction by iron powder method to dissolve its titanium and iron contents. Iron content in the produced liquor is separated by solvent extraction using TBP as a solvent. All parameters affecting the efficiency of the dissolution process were separately studied including the acid concentration, solid/liquid ratio which controls the ilmenite/acid molar ratio, temperature, time and grain size. The optimum conditions at which maximum leaching occur are 30% HCl acid with a solid/liquid ratio of 1/30 at 80 °C for 4 h using ore ground to -350 mesh size. At the same time, all parameters affecting on solvent extraction and stripping of iron content from the produced liquor were studied. Results show that the best extraction is at solvent/solution 1/1 by shaking at 240 RPM for 45 minutes at 30 °C whereas best striping of iron at H₂O/solvent 2/1.

Keywords: ilmenite ore, leaching, titanium solvent extraction, Abu Ghalaga ilmenite ore

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Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

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The process of assembling metal nanoparticles at the interface of two liquids has received a great deal of attention over the past few years due to a wide range of important applications and their unusual properties as compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: Firstly, to describe the achievement of a closed loop recycling for producing cadmium sulfide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulfides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferrofluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Coinage metals like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: metal nanoparticles, core/shell structures and semiconductors, ferromagnetic properties, closed loop recycling, liquid/liquid interface

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Authors: Xiaohui Wang, Zhichuan Guan, Roman Shor, Chuanbin Xu

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Early monitoring and real-time quantitative description of gas intrusion under the premise of ensuring the integrity of the drilling fluid circulation system will greatly improve the accuracy and effectiveness of deepwater gas-kick monitoring. Therefore, in order to study the propagation characteristics of ultrasonic waves in the gas-liquid two-phase flow within the marine riser, in this paper, a numerical simulation method of ultrasonic propagation in the annulus of the riser was established, and the credibility of the numerical analysis was verified by the experimental results of the established gas intrusion monitoring simulation experimental device. The numerical simulation can solve the sound field in the gas-liquid two-phase flow according to different physical models, and it is easier to realize the single factor control. The influence of each parameter on the received signal can be quantitatively investigated, and the law with practical guiding significance can be obtained.

Keywords: gas-kick detection, ultrasonic, void fraction, coda wave velocity

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Authors: Laure Wiest, Barbara Giroud, Azziz Assoumani, Francois Lestremau, Emmanuelle Vulliet

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Due to their production at high tonnages and their extensive use, surfactants are contaminants among those determined at the highest concentrations in wastewater. However, analytical methods and data regarding their occurrence in river water are scarce and concern only a few families, mainly anionic surfactants. The objective of this study was to develop an analytical method to extract and analyze a wide variety of surfactants in a minimum of steps, with a sensitivity compatible with the detection of ultra-traces in surface waters. 27 substances, from 12 families of surfactants, anionic, cationic and non-ionic were selected for method optimization. Different retention mechanisms for the extraction by solid phase extraction (SPE) were tested and compared in order to improve their detection by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The best results were finally obtained with a C18 grafted silica LC column and a polymer cartridge with hydrophilic lipophilic balance (HLB), and the method developed allows the extraction of the three types of surfactants with satisfactory recoveries. The final analytical method comprised only one extraction and two LC injections. It was validated and applied for the quantification of surfactants in 36 river samples. The method's limits of quantification (LQ), intra- and inter-day precision and accuracy were evaluated, and good performances were obtained for the 27 substances. As these compounds have many areas of application, contaminations of instrument and method blanks were observed and considered for the determination of LQ. Nevertheless, with LQ between 15 and 485 ng/L, and accuracy of over 80%, this method was suitable for monitoring surfactants in surface waters. Application on French river samples revealed the presence of anionic, cationic and non-ionic surfactants with median concentrations ranging from 24 ng/L for octylphenol ethoxylates (OPEO) to 4.6 µg/L for linear alkylbenzenesulfonates (LAS). The analytical method developed in this work will therefore be useful for future monitoring of surfactants in waters. Moreover, this method, which shows good performances for anionic, non-ionic and cationic surfactants, may be easily adapted to other surfactants.

Keywords: anionic surfactant, cationic surfactant, LC-MS/MS, non-ionic surfactant, SPE, surface water

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Authors: Chane-Yu Lai, Xiang-Yu Huang

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This study conducted an assessment of sampling result by using the new development rotation filtration device (RFD) filled with porous media filters integrating the method of cyclone centrifugal spins. The testing system established for the experiment used corn oil and potassium sodium tartrate tetrahydrate (PST) as challenge aerosols and were produced by using an Ultrasonic Atomizing Nozzle, a Syringe Pump, and a Collison nebulizer. The collection efficiency of RFD for oil aerosol was assessed by using an Aerodynamic Particle Sizer (APS) and a Fidas® Frog. The results of RFD for the liquid particles condition indicated the cutoff size was 1.65 µm and 1.02 µm for rotation of 0 rpm and 9000 rpm, respectively, under an 80 PPI (pores per inch）foam with a thickness of 80 mm, and sampling velocity of 13.5 cm/s. As the experiment increased the foam thickness of RFD, the cutoff size reduced from 1.62 µm to 1.02 µm. However, when increased the foam porosity of RFD, the cutoff size reduced from 1.26 µm to 0.96 µm. Moreover, as increased the sampling velocity of RFD, the cutoff size reduced from 1.02 µm to 0.76 µm. These discrepancies of above cutoff sizes of RFD all had statistical significance (P < 0.05). The cutoff size of RFD for three experimental conditions of generated liquid oil particles, solid PST particles or both liquid oil and solid PST particles was 1.03 µm, 1.02 µm, or 0.99 µm, respectively, under a 80 PPI foam with thickness of 80 mm, rotation of 9000 rpm, and sampling velocity of 13.5 cm/s. In addition, under the best condition of the experiment, two hours of sampling loading, the RFD had better collection efficiency for particle diameter greater than 0.45 µm, under a 94 PPI nickel mesh with a thickness of 68 mm, rotation of 9000 rpm, and sampling velocity of 108.3 cm/s. The experiment concluded that increased the thickness of porous media, face velocity, and porosity of porous media of RFD could increase the collection efficiency of porous media for sampling oil particles. Moreover, increased the rotation speed of RFD also increased the collection efficiency for sampling oil particles. Further investigation is required for those above operation parameters for RFD in this study in the future.

Keywords: oil aerosol, porous media filter, rotation, filtration

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Authors: Hilary Rutto, John Kabuba

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Sulphur dioxide is a harmful gaseous product that needs to be minimized in the atmosphere. This research work investigates the use of zeolite as a possible additive that can improve the sulphur dioxide capture in wet flue gas desulphurisation dissolution process. This work determines the effect of temperature, solid to liquid ratio, acid concentration and stirring speed on the leaching of zeolite using a pH stat apparatus. The atomic absorption spectrometer was used to measure the calcium ions from the solution. It was found that the dissolution rate of zeolite decreased with increase in solid to liquid ratio and increases with increase in temperature, stirring speed and acid concentration. The activation energy for the dissolution rate of zeolite in hydrochloric acid was found to be 9.29kJ/mol. and therefore the product layer diffusion was the rate limiting step.

Keywords: calcium ion, pH stat apparatus, wet flue gas desulphurization, zeolite

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Authors: Abdoulaye Maihatchi Ahamed, Zubin Arora, Benjamin Swobada, Jean-yves Lansot, Alexandre Chagnes

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Lithium-ion battery (LiB) is the technology of choice in the development of electric vehicles. But there are still many challenges, including the development of positive electrode materials exhibiting high cycle ability, high energy density, and low environmental impact. For this latter, LiBs must be manufactured in a circular approach by developing the appropriate strategies to reuse and recycle them. Presently, the recycling of LiBs is carried out by the pyrometallurgical route, but more and more processes implement or will implement the hydrometallurgical route or a combination of pyrometallurgical and hydrometallurgical operations. After producing the black mass by mineral processing, the hydrometallurgical process consists in leaching the black mass in order to uptake the metals contained in the cathodic material. Then, these metals are extracted selectively by liquid-liquid extraction, solid-liquid extraction, and/or precipitation stages. However, liquid-liquid extraction combined with precipitation/crystallization steps is the most implemented operation in the LiB recycling process to selectively extract copper, aluminum, cobalt, nickel, manganese, and lithium from the leaching solution and precipitate these metals as high-grade sulfate or carbonate salts. Liquid-liquid extraction consists in contacting an organic solvent and an aqueous feed solution containing several metals, including the targeted metal(s) to extract. The organic phase is non-miscible with the aqueous phase. It is composed of an extractant to extract the target metals and a diluent, which is usually aliphatic kerosene produced from the petroleum industry. Sometimes, a phase modifier is added in the formulation of the extraction solvent to avoid the third phase formation. The extraction properties of the diluent do not depend only on the chemical structure of the extractant, but it may also depend on the nature of the diluent. Indeed, the interactions between the diluent can influence more or less the interactions between extractant molecules besides the extractant-diluent interactions. Only a few studies in the literature addressed the influence of the diluent on the extraction properties, while many studies focused on the effect of the extractants. Recently, new low-carbon footprint aliphatic diluents were produced by catalytic dearomatisation and distillation of bio-based oil. This study aims at investigating the influence of the nature of the diluent on the extraction properties of three extractants towards cobalt, nickel, manganese, copper, aluminum, and lithium: Cyanex®272 for nickel-cobalt separation, DEHPA for manganese extraction, and Acorga M5640 for copper extraction. The diluents used in the formulation of the extraction solvents are (i) low-odor aliphatic kerosene produced from the petroleum industry (ELIXORE 180, ELIXORE 230, ELIXORE 205, and ISANE IP 175) and (ii) bio-sourced aliphatic diluents (DEV 2138, DEV 2139, DEV 1763, DEV 2160, DEV 2161 and DEV 2063). After discussing the effect of the diluents on the extraction properties, this conference will address the development of a low carbon footprint process based on the use of the best bio-sourced diluent for the production of high-grade cobalt sulfate, nickel sulfate, manganese sulfate, and lithium carbonate, as well as metal copper.

Keywords: diluent, hydrometallurgy, lithium-ion battery, recycling

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Authors: Faezah Shekh Abdullah, Mohd. Azizuddin Mohd. Yussof, Komathy Thiagarajan, Hasnoorina Husin, Noor Azreena Abd Aziz

Abstract:

Polycystic ovary syndrome has been associated with multiple disorders such as endocrine disorder, metabolic syndrome, infertility, and endometrial cancer. Women with polycystic ovary syndrome (PCOS) are anticipated to develop three times more chances for endometrial cancer than women without PCOS. This study, therefore, was conducted to determine the association between polycystic ovary syndrome and endometrial cancer and to determine the cervical cytology features of PCOS. Patients attending the Subfertility Clinic of the National Population and Family Development Board were recruited and examined physically by medical practitioners. They were categorized into two groups; i) the PCOS group if they met Rotterdam Criteria 2004 and ii) the control group if they did not meet Rotterdam Criteria 2004. Cervical sampling was done on all patients via the Liquid-Based Cytology (LBC) method in the pre-and post-subfertility treatment. A total of 167 patients participated in the study, of which 79 belonged to the PCOS group and 88 to the control group. The findings showed no cervical and endometrial cancer cases in both groups. The Liquid-Based Cytology results in the PCOS group displayed more cases with cellular changes, i.e., benign inflammation, atrophic smear and Candida sp. infection. To conclude, no association was found between polycystic ovary syndrome and endometrial cancer. A more holistic study with a higher number of participants can further determine the association between endometrial cancer and PCOS. Furthermore, a longer duration between LBC pre- and post-subfertility treatment should be implied to observe changes in the cervical cells.

Keywords: endometrial cancer, liquid-based cytology, PCOS, polycystic ovary syndrome

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