Search results for: liquid liquid extraction

Authors: Blaga Alexandra Cristina, Kloetzer Lenuta, Bompa Amalia Stela, Galaction Anca Irina, Cascaval Dan

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Vitamin B9 is an important member of vitamins B group, being a growth factor, important for making genetic material as DNA and RNA, red blood cells, for building muscle tissues, especially during periods of infancy, adolescence and pregnancy. Its production by biosynthesis is based on the high metabolic potential of mutant Bacillus subtilis, due to a superior biodisponibility compared to that obtained by chemical pathways. Pertraction, defined as the extraction and transport through liquid membranes consists in the transfer of a solute between two aqueous phases of different pH-values, phases that are separated by a solvent layer of various sizes. The pertraction efficiency and selectivity could be significantly enhanced by adding a carrier in the liquid membrane, such as organophosphoric compounds, long chain amines or crown-ethers etc., the separation process being called facilitated pertraction. The aim of the work is to determine the impact of the presence of two extractants/carriers in the bulk liquid membrane, i.e. di(2-ethylhexyl) phosphoric acid (D2EHPA) and lauryltrialkylmetilamine (Amberlite LA2) on the transport kinetics of vitamin B9. The experiments have been carried out using two pertraction equipments for a free liquid membrane or bulk liquid membrane. One pertraction cell consists on a U-shaped glass pipe (used for the dichloromethane membrane) and the second one is an H-shaped glass pipe (used for h-heptane), having 45 mm inner diameter of the total volume of 450 mL, the volume of each compartment being of 150 mL. The aqueous solutions are independently mixed by means of double blade stirrers with 6 mm diameter and 3 mm height, having the rotation speed of 500 rpm. In order to reach high diffusional rates through the solvent layer, the organic phase has been mixed with a similar stirrer, at a similar rotation speed (500 rpm). The area of mass transfer surface, both for extraction and for reextraction, was of 1.59x10-³ m2. The study on facilitated pertraction with the mixture of two carriers, namely D2EHPA and Amberlite LA-2, dissolved in two solvents with different polarities: n-heptane and dichloromethane, indicated the possibility to obtain the synergic effect. The synergism has been analyzed by considering the vitamin initial and final mass flows, as well as the permeability factors through liquid membrane. The synergic effect has been observed at low D2EHPA concentrations and high Amberlite LA-2 concentrations, being more important for the low-polar solvent (n-heptane). The results suggest that the mechanism of synergic pertraction consists on the reaction between the organophosphoric carrier and vitamin B9 at the interface between the feed and membrane phases, while the aminic carrier enhances the hydrophobicity of this compound by solvation. However, the formation of this complex reduced the reextraction rate and, consequently, affects the synergism related to the final mass flows and permeability factor. For describing the influences of carriers concentrations on the synergistic coefficients, some equations have been proposed by taking into account the vitamin mass flows or permeability factors, with an average deviations between 4.85% and 10.73%.

Keywords: pertraction, synergism, vitamin B9, Amberlite LA-2, di(2-ethylhexyl) phosphoric acid

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Authors: Hongyan Chen, Megan Jobson, Andrew J. Masters, Maria Gonzalez-Miquel, Simon Halstead, Mayri Diaz de Rienzo

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Ionic liquids offer excellent advantages over conventional solvents for industrial extraction of metals from aqueous solutions, where such extraction processes bring opportunities for recovery, reuse, and recycling of valuable resources and more sustainable production pathways. Recent research on the use of ionic liquids for extraction confirms their high selectivity and low volatility, but there is relatively little focus on how their properties can be best exploited in practice. This work addresses gaps in research on process modelling and simulation, to support development, design, and optimisation of these processes, focusing on the separation of the highly similar transition metals, cobalt, and nickel. The study exploits published experimental results, as well as new experimental results, relating to the separation of Co and Ni using trihexyl (tetradecyl) phosphonium chloride. This extraction agent is attractive because it is cheaper, more stable and less toxic than fluorinated hydrophobic ionic liquids. This process modelling work concerns selection and/or development of suitable models for the physical properties, distribution coefficients, for mass transfer phenomena, of the extractor unit and of the multi-stage extraction flowsheet. The distribution coefficient model for cobalt and HCl represents an anion exchange mechanism, supported by the literature and COSMO-RS calculations. Parameters of the distribution coefficient models are estimated by fitting the model to published experimental extraction equilibrium results. The mass transfer model applies Newman’s hard sphere model. Diffusion coefficients in the aqueous phase are obtained from the literature, while diffusion coefficients in the ionic liquid phase are fitted to dynamic experimental results. The mass transfer area is calculated from the surface to mean diameter of liquid droplets of the dispersed phase, estimated from the Weber number inside the extractor. New experiments measure the interfacial tension between the aqueous and ionic phases. The empirical models for predicting the density and viscosity of solutions under different metal loadings are also fitted to new experimental data. The extractor is modelled as a continuous stirred tank reactor with mass transfer between the two phases and perfect phase separation of the outlet flows. A multistage separation flowsheet simulation is set up to replicate a published experiment and compare model predictions with the experimental results. This simulation model is implemented in gPROMS software for dynamic process simulation. The results of single stage and multi-stage flowsheet simulations are shown to be in good agreement with the published experimental results. The estimated diffusion coefficient of cobalt in the ionic liquid phase is in reasonable agreement with published data for the diffusion coefficients of various metals in this ionic liquid. A sensitivity study with this simulation model demonstrates the usefulness of the models for process design. The simulation approach has potential to be extended to account for other metals, acids, and solvents for process development, design, and optimisation of extraction processes applying ionic liquids for metals separations, although a lack of experimental data is currently limiting the accuracy of models within the whole framework. Future work will focus on process development more generally and on extractive separation of rare earths using ionic liquids.

Keywords: distribution coefficient, mass transfer, COSMO-RS, flowsheet simulation, phosphonium

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Authors: T. R. Bandara, H. Jaelani, G. J. Griffin

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The conversion of lignocellulosic waste materials, such as sugar cane bagasse, to biofuels such as ethanol has attracted significant interest as a potential element for transforming transport fuel supplies to totally renewable sources. However, the refractory nature of the cellulosic structure of lignocellulosic materials has impeded progress on developing an economic process, whereby the cellulose component may be effectively broken down to glucose monosaccharides and then purified to allow downstream fermentation. Ionic liquid (IL) treatment of lignocellulosic biomass has been shown to disrupt the crystalline structure of cellulose thus potentially enabling the cellulose to be more readily hydrolysed to monosaccharides. Furthermore, conventional hydrolysis of lignocellulosic materials yields byproducts that are inhibitors for efficient fermentation of the monosaccharides. However, selective extraction of monosaccharides from an aqueous/IL phase into an organic phase utilizing a combination of boronic acids and quaternary amines has shown promise as a purification process. Hydrolysis of sugar cane bagasse immersed in an aqueous solution with IL (1-ethyl-3-methylimidazolium acetate) was conducted at different pH and temperature below 100 ºC. It was found that the use of a high concentration of hydrochloric acid to acidify the solution inhibited the hydrolysis of bagasse. At high pH (i.e. basic conditions), using sodium hydroxide, catalyst yields were reduced for total reducing sugars (TRS) due to the rapid degradation of the sugars formed. For purification trials, a supported liquid membrane (SLM) apparatus was constructed, whereby a synthetic solution containing xylose and glucose in an aqueous IL phase was transported across a membrane impregnated with phenyl boronic acid/Aliquat 336 to an aqueous phase. The transport rate of xylose was generally higher than that of glucose indicating that a SLM scheme may not only be useful for purifying sugars from undesirable toxic compounds, but also for fractionating sugars to improve fermentation efficiency.

Keywords: biomass, bagasse, hydrolysis, monosaccharide, supported liquid membrane, purification

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Authors: C. Lanzerstorfer

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Liquid sprays of water are frequently used in air pollution control for gas cooling purposes and for gas cleaning. Twin-fluid nozzles with internal mixing are often used for these purposes because of the small size of the drops produced. In these nozzles the liquid is dispersed by compressed air or another pressurized gas. In high efficiency scrubbers for particle separation, several nozzles are operated in parallel because of the size of the cross section. In such scrubbers, the scrubbing water has to be re-circulated. Precipitation of some solid material can occur in the liquid circuit, caused by chemical reactions. When such precipitations are detached from the place of formation, they can partly or totally block the liquid flow to a nozzle. Due to the resulting unbalanced supply of the nozzles with water and gas, the efficiency of separation decreases. Thus, the nozzles have to be cleaned if a certain fraction of blockages is reached. The aim of this study was to provide a tool for continuously monitoring the status of the nozzles of a scrubber based on the available operation data (water flow, air flow, water pressure and air pressure). The difference between the air pressure and the water pressure is not well suited for this purpose, because the difference is quite small and therefore very exact calibration of the pressure measurement would be required. Therefore, an equation for the reference air flow of a nozzle at the actual water flow and operation pressure was derived. This flow can be compared with the actual air flow for assessment of the status of the nozzles.

Keywords: condition monitoring, dual flow nozzles, flow equation, operation data

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Authors: Davoud Dorranian, Hajar Sadeghi, Elmira Solati

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Carbon nanostructures in various forms were synthesized using pulsed laser ablation of a graphite target in different liquid environment. The beam of a Q-switched Nd:YAG laser of 1064-nm wavelength at 7-ns pulse width is employed to irradiate the solid target in water, acetone, alcohol, and cetyltrimethylammonium bromide (CTAB). Then the effect of the liquid environment on the characteristic of carbon nanostructures produced by laser ablation was investigated. The optical properties of the carbon nanostructures were examined at room temperature by UV–Vis-NIR spectrophotometer. The crystalline structure of the carbon nanostructures was analyzed by X-ray diffraction (XRD). The morphology of samples was investigated by field emission scanning electron microscope (FE-SEM). Transmission electron microscope (TEM) was employed to investigate the form of carbon nanostructures. Raman spectroscopy was used to determine the quality of carbon nanostructures. Results show that different carbon nanostructures such as nanoparticles and few-layer graphene were formed in various liquid environments. The UV-Vis-NIR absorption spectra of samples reveal that the intensity of absorption peak of nanoparticles in alcohol is higher than the other liquid environments due to the larger number of nanoparticles in this environment. The red shift of the absorption peak of the sample in acetone confirms that produced carbon nanoparticles in this liquid are averagely larger than the other medium. The difference in the intensity and shape of the absorption peak indicated the effect of the liquid environment in producing the nanoparticles. The XRD pattern of the sample in water indicates an amorphous structure due to existence the graphene sheets. X-ray diffraction pattern shows that the degree of crystallinity of sample produced in CTAB is higher than the other liquid environments. Transmission electron microscopy images reveal that the generated carbon materials in water are graphene sheet and in the other liquid environments are graphene sheet and spherical nanostructures. According to the TEM images, we have the larger amount of carbon nanoparticles in the alcohol environment. FE-SEM micrographs indicate that in this liquids sheet like structures are formed however in acetone, produced sheets are adhered and these layers overlap with each other. According to the FE-SEM micrographs, the surface morphology of the sample in CTAB was coarser than that without surfactant. From Raman spectra, it can be concluded the distinct shape, width, and position of the graphene peaks and corresponding graphite source.

Keywords: carbon nanostructures, graphene, pulsed laser ablation, graphite

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Authors: Ming-Wei Wu, Yu-Jin Tsai, Ching-Huai Chang

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Liquid phase sintering (LPS) is a versatile technique for achieving effective densification of powder metallurgy (PM) steels and other materials. The aim of this study was to examine the influences of 0.6 wt% boron on the microstructure and LPS behavior of boron-alloyed 410 martensitic stainless steel. The results showed that adding 0.6 wt% boron can obviously promote the LPS due to a eutectic reaction and increase the sintered density of 410 stainless steel. The density was much increased by 1.06 g/cm³ after 1225ºC sintering. Increasing the sintering temperature from 1225ºC to 1275ºC did not obviously improve the sintered density. After sintering at 1225ºC~1275ºC, the matrix was fully martensitic, and intragranular borides were extensively found due to the solidification of eutectic liquid. The microstructure after LPS consisted of the martensitic matrix and (Fe, Cr)2B boride, as identified by electron backscatter diffraction (EBSD) and electron probe micro-analysis (EPMA).

Keywords: powder metallurgy, liquid phase sintering, stainless steel, martensite, boron, microstructure

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Authors: Benedict O. Ayomanor, Cookey Iyen, Ifeoma S. Iyen

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Rice hull (RH) biomass product gives feasible silica for exact temperature and period. The minimal fabrication price turns its best feasible produce to metallurgical grade silicon (MG-Si). In this work, to avoid ecological worries extending from CO₂ release to oil leakage on water and land, or nuclear left-over pollution, all finally add to the immense topics of ecological squalor; high purity silicon > 98.5% emerge set from rice hull ash (RHA) by solid-liquid removal. The RHA derived was purified by nitric and hydrochloric acid solutions. Leached RHA sieved, washed in distilled water, and desiccated at 1010ºC for 4h. Extra cleansing was achieved by carefully mixing the SiO₂ ash through Mg dust at a proportion of 0.9g SiO₂ to 0.9g Mg, galvanised at 1010ºC to formula magnesium silicide. The solid produced was categorised by X-ray fluorescence (XRF), X-ray diffractometer (XRD), and Fourier transformation infrared (FTIR) spectroscopy. Elemental analysis using XRF found the percentage of silicon in the material is approximately 98.6%, main impurities are Mg (0.95%), Ca (0.09%), Fe (0.3%), K (0.25%), and Al (0.40%).

Keywords: siliceous, leached, biomass, solid-liquid extraction

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Authors: V. Marzal, J. C. Torres, B. Garcia-Camara, Manuel Cano-Garcia, Xabier Quintana, I. Perez Garcilopez, J. M. Sanchez-Pena

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At the present time, the use of nanostructures in complex media, like liquid crystals, is widely extended to manipulate their properties, either electrical or optical. In addition, these media can also be used to control the optical properties of the nanoparticles, for instance when they are resonant. In this work, the change on electrical properties of a liquid crystal cell by adding TiO₂ nanoparticles on one of the alignment layers has been analyzed. These nanoparticles, with a diameter of 100 nm and spherical shape, were deposited in one of the substrates (ITO + polyimide) by spin-coating in order to produce a homogeneous layer. These substrates were checked using an optical microscope (objective x100) to avoid potential agglomerates. The liquid crystal cell is then fabricated, using one of these substrates and another without nanoparticles, and filled with E7. The study of the electrical response was done through impedance measurements in a long range of frequencies (3 Hz- 6 MHz) and at ambient temperature. Different nanoparticle concentrations were considered, as well as pure E7 and an empty cell for comparison purposes. Results about the effective dielectric permittivity and conductivity are presented along with models of equivalent electric circuits and its physical interpretation. As a summary, it has been observed the clear influence of the presence of the nanoparticles, strongly modifying the electric response of the device. In particular, a variation of both the effective permittivity and the conductivity of the device have been observed. This result requires a deep analysis of the effect of these nanoparticles on the trapping of free ions in the device, allowing a controlled manipulation and frequency tuning of the electrical response of these devices.

Keywords: alignment layer, electrical behavior, liquid crystal, TiO₂ nanoparticles

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Authors: Najwa Othman, Norhidayah Suleiman, Gun Hean Chong

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Palm fatty acid distillate (PFAD) is a by-product of palm oil refineries which contains valuable compounds such as phytosterols, squalene, polycosanol, co-enzyme Q10 and vitamin E (tocopherols and tocotrienols). Approximately 0.7-1.0% of vitamin E accumulates in PFAD, and it functions as antioxidants and anti-inflammatory. The objective of this research is to evaluate the effect of manipulated variables in supercritical carbon dioxide towards the recovery of tocotrienols in PFAD. The vitamin E concentrate isolated varies depending on the pre-treatment of sample and extraction techniques. In this research, tocotrienols in PFAD was concentrated by removing the extraneous matters, especially free fatty acid (FFA) and acylglycerols. Pre-treatment method such as enzymatic hydrolysis by using lipase from Candida rugosa as an enzyme was used to remove FFA and improve recovery of vitamin E. After that, treated PFAD was extracted by using supercritical fluid extraction in co-current glass beads packed column (22 cm x 75 cm i.d) at different temperatures (40-60°C) and pressures (100-300 bar) for 5 hours. After the extraction, the sample was analyzed by using high-pressure liquid chromatography (HPLC) system to quantify the tocotrienols. The results indicated that a combined pressure (200 bar) and temperature (60°C) was predicted to provide highest tocotrienols yield and the extraction yield obtained was 106.45%.

Keywords: enzymatic hydrolysis, palm fatty acid distillate, supercritical fluid extraction, tocotrienols

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Authors: Mohamed A. Deyab, Ahmed E. Awadallah

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Under various conditions, we present a promising method for producing pure hydrogen energy from the electrochemical reaction of Mg metal in waste oilfield water (WOW). Mg metal and WOW are primarily consumed in this process. The results show that the hydrogen gas output is highly dependent on temperature and solution pH. The best conditions for hydrogen production were found to be a low pH (2.5) and a high temperature (338 K). For the first time, the Allyl methylimidazolium bis-trifluoromethyl sulfonyl imide) (IL) ionic liquid is used to regulate the rate of hydrogen generation. It has been confirmed that increasing the solution temperature and decreasing the solution pH accelerates Mg dissolution and produces more hydrogen per unit of time. The adsorption of IL on the active sites of the Mg surface is unrestricted by mixing physical and chemical orientation. Inspections using scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and FT-IR spectroscopy were used to identify and characterise surface corrosion of Mg in WOW. This process is also completely safe and can create energy on demand.

Keywords: hydrogen production, Mg, wastewater, ionic liquid

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Authors: Victor Ananth Paramananth, Rashid Muniginin, Mahaya Abd Rahman, Siti Afifah Ismail

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Safety issues, scene protection, and appropriate evidence collection must be handled in any bio crime scene. There will be a scene or multi-scene to be cordoned for investigation in any bio-incident or bio crime event. Evidence collection is critical in determining the type of microbial or toxin, its lethality, and its source. As a consequence, from the start of the investigation, a proper sampling method is required. The most significant challenges for the crime scene officer would be deciding where to obtain samples, the best sampling method, and the sample sizes needed. Since there could be evidence in liquid, viscous, or powder shape at a crime scene, crime scene officers have difficulty determining which tools to use for sampling. To maximize sample collection, the appropriate tools for sampling methods are necessary. This study aims to assist the crime scene officer in collecting liquid, viscous, and powder biological samples in sufficient quantity while preserving sample quality. Observational tests on sample collection using liquid, viscous, and powder samples for adequate quantity and sample quality were performed using UV light in this research. The density of the light emission varies upon the method of collection and sample types. The best tools for collecting sufficient amounts of liquid, viscous, and powdered samples can be identified by observing UV light. Instead of active microorganisms, the invisible powder is used to assess sufficient sample collection during a crime scene investigation using various collection tools. The liquid, powdered and viscous samples collected using different tools were analyzed using Fourier transform infrared - attenuate total reflection (FTIR-ATR). FTIR spectroscopy is commonly used for rapid discrimination, classification, and identification of intact microbial cells. The liquid, viscous and powdered samples collected using various tools have been successfully observed using UV light. Furthermore, FTIR-ATR analysis showed that collected samples are sufficient in quantity while preserving their quality.

Keywords: biological sample, crime scene, collection tool, UV light, forensic

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Authors: M. Brik, S. Harmand, I. Zaaroura

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This report, an experimental investigation, concerns the sessile daughter drop remaining during the coalescence of water drops in a liquid-liquid (LL) system. The two drops are initially vertically aligned where the sessile drop is deposited on a chemically treated super-hydrophobic surface of a cube fill of silicone oil. In order to analyze the coalescence dynamics, a series of experiments have been performed using a generation droplets system (KRUSS) that measures contact angles as well coupled with a high-speed camera (Keyence VW-9000E) to record the process at a frame rate of 15000s-1. It’s depicted that in such configuration, the head drop volume has a primordial impact on the dynamics of the coalescence process, especially at the last stage. It’s found that for a sessile drop deposited on a super-hydrophobic surface, where the contact angle is about θ ≈ 145°, the coalescence process is remarked to be complete without any recoiling of the coalesced drop or a generation of a sessile daughter drop at the super-hydrophobic surface when the head drop volume is small enough (Vₐᵦ< Vₛ up to Vₐᵦ = 3Vₛ). On the other side, the coalescence process starts to be followed by jumping off the resulted drop as well as a remaining of a small sessile daughter drop on the bottom surface of the cube from a head drop volume Vₐᵦ of about 4 times than that of the sessile drop Vₛ.

Keywords: drops coalescence, dispersed multiphase flow, drops dynamics, liquid-liquid system

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Authors: Muhammad Idrees, Masroor Abro, Sikandar Almani

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Presently, the increasing CO₂ concentration in the atmosphere has been taken as one of the major challenges faced by the modern world. The average CO₂ in the atmosphere reached the highest value of 414.72 ppm in 2021, as reported in a conference of the parties (COP26). This study focuses on (i) the comparative study of MEA, NaOH, Acetic acid, and Na₂CO₃ in terms of their CO₂ capture performance, (ii) the significance of adding various frothing agents achieving improved absorption capacity of Na₂CO₃ and (iii) the overall economic evaluation of process with the help of Aspen Plus. The results obtained suggest that the addition of frothing agents significantly increased the absorption rate of dilute sodium carbonate such that from 45% to 99.9%. The effect of temperature, pressure and flow rate of liquid and flue gas streams on CO₂ absorption capacity was also investigated. It was found that the absorption capacity of Na₂CO₃ decreased with increasing temperature of the liquid stream and decreasing flow rate of the liquid stream and pressure of the gas stream.

Keywords: CO₂, absorbents, frothing agents, process simulation

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Authors: Sung-Pill Kim, Dae-Gyu Sung, Hee-Sung Shin, Jong-Chun Park

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When a sloshing tank filled partially with liquid is excited with the motion of platform, it can be observed that the center of mass inside the tank is changed and impact loads is instantaneously applied to the wall, which causes dynamic loads additionally to the supporting links of platform. In this case, therefore, the dynamic behavior of platform associated with fluid motion should be considered in the early stage of design for safety and economics of the system. In this paper, the dynamic loads due to liquid sloshing motion in a rectangular tank which is loaded up on the upper deck of a Stewart platform are simulated using a coupled analysis of Moving Particle Simulation (MPS) and Flexible Multi-Body Dynamics (FMBD). The co-simulation is performed using two commercial softwares, Recurdyn for solving FMBD and Particleworks for analyzing fluid motion based on MPS method. For validating the present coupled system, a rectangular sloshing tank being enforced with inline sway motion by 1-DOF motion platform is assumed, and time-varied free-surface elevation and reaction force at a fixed joint are compared with experiments.

Keywords: dynamic loads, liquid sloshing tank, Stewart platform, moving particle semi-implicit (MPS) method, flexible multi-body dynamics (FMBD)

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Authors: Yih-Chien Chen, Tse-Lung Lin

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The microwave characteristics of NdTi₍₀.₅₋ₓ₎GeₓMo₀.₅O₄ are studied to determine the feasibility of their use in the liquid sensor. The microwave characteristics of NdTi₍₀.₅₋ₓ₎GeₓMo₀.₅O₄ are determined using X-ray diffraction (XRD) patterns. The permittivity (𝜀r) of NdTi₍₀.₄₉₎Ge₀.₀₁Mo₀.₅O₄ that is sintered at 1425 ℃ for 4 h is 17.6, the unloaded quality factor (Qu×f) is 33,400 GHz, and it has a temperature coefficient at the resonance frequency (TCF) of -30.7 ppm/℃. The proposed liquid sensor is at the 5G FR1 bands.

Keywords: NdTi₍₀.₅₋ₓ₎GeₓMo₀.₅O₄, X-ray diffraction pattern, permittivity, Unloaded quality factor

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Authors: Bamikole J. Adeyemi, Prashant Jadhawar, Lateef Akanji

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Theoretically, there exist two mathematical interfaces (fluid-solid and fluid-fluid) when a liquid film is present on solid surfaces. These interfaces overlap if the mineral surface is oil-wet or mixed wet, and therefore, the effects of disjoining pressure are significant on both boundaries. Hence, dewetting is a necessary process that could detach oil from the mineral surface. However, if the thickness of the thin water film directly in contact with the surface is large enough, disjoining pressure can be thought to be zero at the liquid-liquid interface. Recent studies show that the integration of fluid-fluid interactions with fluid-rock interactions is an important step towards a holistic approach to understanding smart water effects. Experiments have shown that the brine solution can alter the micro forces at oil-water interfaces, and these ion-specific interactions lead to oil emulsion formation. The natural emulsifiers present in crude oil behave as polyelectrolytes when the oil interfaces with low salinity water. Wettability alteration caused by low salinity waterflooding during Enhanced Oil Recovery (EOR) process results from the activities of divalent ions. However, polyelectrolytes are said to lose their viscoelastic property with increasing cation concentrations. In this work, the influence of cation concentrations on the dynamics of viscoelastic liquid-liquid interfaces is numerically investigated. The resultant ion concentrations at the crude oil/brine interfaces were estimated using a surface complexation model. Subsequently, the ion concentration parameter is integrated into a mathematical model to describe its effects on the dynamics of a viscoelastic interfacial thin film. The film growth, stability, and rupture were measured after different time steps for three types of fluids (Newtonian, purely elastic and viscoelastic fluids). The interfacial films respond to exposure time in a similar manner with an increasing growth rate, which resulted in the formation of more droplets with time. Increased surfactant accumulation at the interface results in a higher film growth rate which leads to instability and subsequent formation of more satellite droplets. Purely elastic and viscoelastic properties limit film growth rate and consequent film stability compared to the Newtonian fluid. Therefore, low salinity and reduced concentration of the potential determining ions in injection water will lead to improved interfacial viscoelasticity.

Keywords: liquid-liquid interfaces, surfactant concentrations, potential determining ions, residual oil mobilization

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Authors: G. Blázquez, A. Gálvez-Pérez, M. Calero, I. Iáñez-Rodríguez, M. A. Martín-Lara, A. Pérez

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The production of olive oil is considered as one of the most important agri-food industries. However, some of the by-products generated in the process are potential pollutants and cause environmental problems. Consequently, the management of these by-products is currently considered as a challenge for the olive oil industry. In this context, several technologies have been developed and tested. In this sense, the autohydrolysis of these by-products could be considered as a promising technique. Therefore, this study focused on autohydrolysis treatments of a solid residue from the olive oil industry denominated olive cake. This one comes from the olive pomace extraction with hexane. Firstly, a water washing was carried out to eliminate the water soluble compounds. Then, an experimental design was developed for the autohydrolysis experiments carried out in the hydrothermal pressure reactor. The studied variables were temperature (30, 60 and 90 ºC) and time (30, 60, 90 min). On the other hand, aliquots of liquid obtained fractions were analysed by HPLC to determine the fructose and sucrose contents present in the liquid fraction. Finally, the obtained results of sugars contents and the yields of the different experiments were fitted to a neuro-fuzzy and to a polynomial model.

Keywords: ANFIS, olive cake, polyols, saccharides

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Authors: Amokrane Boufares, Elise Provost, Veronique Osswald, Pascal Clain, Anthony Delahaye, Laurence Fournaison, Didier Dalmazzone

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Gas hydrates have long been considered as problematic for flow assurance in natural gas and oil transportation. On the other hand, they are now seen as future promising materials for various applications (i.e. desalination of seawater, natural gas and hydrogen storage, gas sequestration, gas combustion separation and cold storage and transport). Nonetheless, a better understanding of the crystallization mechanism of gas hydrate and of their formation kinetics is still needed for a better comprehension and control of the process. To that purpose, measuring the real-time evolution of the dissolved gas concentration in the aqueous phase during hydrate formation is required. In this work, CO₂ hydrates were formed in a stirred reactor equipped with an Attenuated Total Reflection (ATR) probe coupled to a Fourier Transform InfraRed (FTIR) spectroscopy analyzer. A method was first developed to continuously measure in-situ the CO₂ concentration in the liquid phase during solubilization, supersaturation, hydrate crystallization and dissociation steps. Thereafter, the measured concentration data were compared with those of equilibrium concentrations. It was observed that the equilibrium is instantly reached in the liquid phase due to the fast consumption of dissolved gas by the hydrate crystallization. Consequently, it was shown that hydrate crystallization kinetics is limited by the gas transfer at the gas-liquid interface. Finally, we noticed that the liquid-hydrate equilibrium during the hydrate crystallization is governed by the temperature of the experiment under the tested conditions.

Keywords: gas hydrate, dissolved gas, crystallization, infrared spectroscopy

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Authors: Dewi Selvia Fardhyanti, Astrilia Damayanti

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Coal tar is a liquid by-product of coal pyrolysis processes. This liquid oil mixture contains various kind of useful compounds such as benzoic aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. The coal tar was collected by pyrolysis process of coal obtained from PT Kaltim Prima Coal and Arutmin-Kalimantan. The experiments typically occurred at the atmospheric pressure in a laboratory furnace at temperatures ranging from 300 to 550oC with a heating rate of 10oC/min and a holding time of 1 hour at the pyrolysis temperature. Nitrogen gas has been used to obtain the inert condition and to carry the gaseous pyrolysis products. The pyrolysis transformed organic materials into gaseous components, small quantities of liquid, and a solid residue (coke) containing fixed amount of carbon and ash. The composition of gas which is produced from the pyrolysis is carbon monoxide, hydrogen, methane, and other hydrocarbon compounds. The gas was condensed and the liquid containing oil/tar and water was obtained. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the coal tar components. The obtained coal tar has the viscosity of 3.12 cp, the density of 2.78 g/cm3, the calorific value of 11,048.44 cal/g, and the molecular weight of 222.67. The analysis result showed that the coal tar contained more than 78 chemical compounds such as benzene, cresol, phenol, xylene, naphtalene, etc. The total phenolic compounds contained in coal tar is 33.25% (PT KPC) and 17.58% (Arutmin-Kalimantan). The total naphtalene compounds contained in coal tar is 14.15% (PT KPC) and 17.13% (Arutmin-Kalimantan).

Keywords: coal tar, pyrolysis, gas chromatography-mass spectroscopy

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Authors: Rui Tu, Yakui Bai, Huailin Li

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The lead-bismuth eutectic (LBE) alloy is a promising candidate of coolant in the fast neutron reactors and accelerator-driven systems (ADS) because of its good properties, such as low melting point, high neutron yields and high thermal conductivity. Although the corrosion of the structure materials caused by the liquid metal (LM) coolant is a challenge to the safe operating of a lead-bismuth eutectic nuclear reactor. Thermodynamic theories, experiential formulas and experimental data can be used for explaining the maintenance of the protective oxide layers on stainless steels under satisfaction oxygen concentration, but the atomic scale insights of such anti-corrosion mechanisms are little known. In the present work, the first-principles calculations are carried out to study the effects of oxygen partial pressure on the formation energies of the liquid metal coolant relevant impurity defects in the anti-corrosion oxide films on the surfaces of the structure materials. These approaches reveal the microscope mechanisms of the corrosion of the structure materials, especially for the influences from the oxygen partial pressure. The results are helpful for identifying a crucial oxygen concentration for corrosion control, which can ensure the systems to be operated safely under certain temperatures.

Keywords: oxygen partial pressure, liquid metal coolant, TDDFT, anti-corrosion layer, formation energy

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Authors: Rajinder Kaur, Atul Khanna

Abstract:

Transparent glass-ceramic and crystalline samples of the system: xSrO-(100-x)TeO2; x = 7.5 and 8.5 mol% were prepared by quenching the melts in the temperature range of 700 to 950oC. A very interesting effect of the temperature on the glass-forming ability (GFA) of strontium tellurite melts is observed,and it is found that the melts produce transparent glass-ceramics when it is solidified from lower temperatures in the range of 700-750oC, however, when the melts are cooled from higher temperatures in the range of 850-950oC, the GFA is significantly reduced andanti-glass and/or crystalline phases are produced on solidification.The effect of temperature on GFA of strontium tellurite melts is attributed to short-range structural transformations: TeO₄TeO₃ which procceds towards the right side with an increrase in temperature. This isomerization reaction lowers the melt viscosity and enhances the crystallization tedendency. It is concluded that the high-temperature strontium tellurite meltsfreeze faster into crystalline phases as compared to the melts at a lower temperature; the latter supercooland solidify into glassy phases.

Keywords: anti-glasss, ceramic, supercool liquid, raman spectroscopy

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Authors: Shweta K. Vyas, Rakesh Musale, Sanjeev R. Shukla

Abstract:

Eri silk is a non mulberry silk which is obtained without killing the silkworms and hence it is also known as Ahmisa silk. In the present study, the results on degumming of eri silk with alkaline peroxide have been compared with those obtained by using ionic liquid (IL) 1-Butyl-3-methylimidazolium chloride [BMIM]Cl. Experiments were designed to find out the optimum processing parameters for degumming of eri silk by response surface methodology. The statistical software, Design-Expert 6.0 was used for regression analysis and graphical analysis of the responses obtained by running the set of designed experiments. Analysis of variance (ANOVA) was used to estimate the statistical parameters. The polynomial equation of quadratic order was employed to fit the experimental data. The quality and model terms were evaluated by F-test. Three dimensional surface plots were prepared to study the effect of variables on different responses. The optimum conditions for IL treatment were selected from predicted combinations and the experiments were repeated under these conditions to determine the reproducibility.

Keywords: silk degumming, ionic liquid, response surface methodology, ANOVA

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Authors: Yuta Tachibana, Ayuko Itsuki

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The three strains of bacteria (Lysinibacillus xylanilyticus, Bacillus kochii, and Enterococcus sp.) were isolated from the fermented Indigo (Polygonum tinctorium) dyeing solution using the dilution plate method and some fermentation conditions were determined. High-Performance Liquid Chromatography (HPLC) was used to determine the indigo concentration. When the isolated bacteria were cultured in the indigo liquid culture containing various sugars, starch, and ethanol, the indigo culture solutions containing galactose, mannose, ribose, and ethanol were remarkably decreased. Comparison of decreasing indigo between three strains showed that Enterococcus sp. had the fastest growth and decrease of indigo. However, decreasing indigo per unit micro biomass did not correspond to the results of decreasing indigo―Bacillus kochii had higher indigo-reducing activity than Enterococcus sp. and Lysinibacillus xylanilyticus.

Keywords: fermentation condition, high-performance liquid chromatography (HPLC), indigo dyeing solution, indigo-reducing activity

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Authors: Haitham Qaralleh, Syed Z. Idid, Shahbudin Saad, Deny Susanti, Osama Althunibat

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This study was carried out to isolate the active antimicrobial compounds from Neopetrosia exigua using bio-guided assay isolation against Staphylococcus aureus. N. exigua was extracted using methanol and subjected to liquid-liquid extraction using solvents with different polarity (n-hexane, carbon tetrachloride, dichloromethane, n-butanol and water). Purification of the active components of n-butanol and dichloromethane fractions was done using Sephadex LH-20 and reverse phase chromatography. Based on the biological guided fractionation results, dichloromethane and n-butanol fractions showed the highest antimicrobial activity. Purification of the active components of n-butanol and dichloromethane fractions yielded three compounds. The structure of the isolated compounds were elucidated and found to be 5-hydroxy-1H-indole-3-carboxylic acid methyl ester, cyclo-1`-demethylcystalgerone and avarol derivative. Avarol was showed potent bactericidal effect against S. aureus. N. exigua appears to be rich source of natural antimicrobial agents. Further studies are needed to investigate the mode of action of these compounds.

Keywords: antimicrobial, avarol, Neopetrosia exigua, Staphylococcus aureus

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Authors: Sujitra Ruengdechawiwat, Robert Molloy, Jintana Siripitayananon, Runglawan Somsunan, Paul D. Topham, Brian J. Tighe

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The main aim of this research has been to design and synthesize some completely soluble liquid tin(II) alkoxide initiators for use in the ring-opening polymerisation (ROP) of cyclic ester monomers. This is in contrast to conventional tin(II) alkoxides in solid form which tend to be molecular aggregates and difficult to dissolve. The liquid initiators prepared were bis(tin(II) monooctoate) diethylene glycol ([Sn(Oct)]2DEG) and bis(tin(II) monooctoate) ethylene glycol ([Sn(Oct)]2EG). Their efficiencies as initiators in the bulk ROP of ε-caprolactone (CL) at 130oC were studied kinetically by dilatometry. Kinetic data over the 20-70% conversion range was used to construct both first-order and zero-order rate plots. It was found that the rate data fitted more closely to first-order kinetics with respect to the monomer concentration and gave higher first-order rate constants than the corresponding tin(II) octoate/diol initiating systems normally used to generate the tin(II) alkoxide in situ. Since the ultimate objective of this work is to produce copolymers suitable for biomedical use as absorbable monofilament surgical sutures, poly(L-lactide-co-ε-caprolactone) 75:25 mol %, P(LL-co-CL), copolymers were synthesized using both solid and liquid tin(II) alkoxide initiators at 130°C for 48 hrs. The statistical copolymers were obtained in near-quantitative yields with compositions (from 1H-NMR) close to the initial comonomer feed ratios. The monomer sequencing (from 13C-NMR) was partly random and partly blocky (gradient-type) due to the much differing monomer reactivity ratios (rLL >> rCL). From GPC, the copolymers obtained using the soluble liquid tin(II) alkoxides were found to have higher molecular weights (Mn = 40,000-100,000) than those from the only partially soluble solid initiators (Mn = 30,000-52,000).

Keywords: biodegradable polyesters, poly(L-lactide-co-ε-caprolactone), ring-opening polymerisation, tin(II) alkoxide

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Authors: Sudip Ghosh, Dipanwita Roy, Dipan Chatterjee, Paramita Bhattacharjee, Satadal Das

Abstract:

Highest yield of eugenol-rich fractions from Cinnamomum tamala (bay leaf) leaves were obtained by supercritical carbon dioxide (SC-CO2), compared to hydro-distillation, organic solvents, liquid CO2 and subcritical CO2 extractions. Optimization of SC-CO2 extraction parameters was carried out to obtain an extract with maximum eugenol content. This was achieved using a sample size of 10 g at 55°C, 512 bar after 60 min at a flow rate of 25.0 cm3/sof gaseous CO2. This extract has the best combination of phytochemical properties such as phenolic content (1.77 mg gallic acid/g dry bay leaf), reducing power (0.80 mg BHT/g dry bay leaf), antioxidant activity (IC50 of 0.20 mg/ml) and anti-inflammatory potency (IC50 of 1.89 mg/ml). Identification of compounds in this extract was performed by GC-MS analysis and its antimicrobial potency was also evaluated. The MIC values against E. coli, P. aeruginosa and S. aureus were 0.5, 0.25 and 0.5 mg/ml, respectively.

Keywords: antimicrobial potency, Cinnamomum tamala, eugenol, supercritical carbon dioxide extraction

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Authors: Yu-Ting Wang, Yun-Hsiang Cheng, Chien-Cheng Lin, Kun-Lin Lin

Abstract:

Using a transient liquid phase method, Al was successfully bonded with Al₂O₃, which deposited Ni, Cu, Ge, and Si at the surface of the Al₂O₃ substrate after annealing at the relatively low melting point of Al. No reaction interlayer existed at the interface of any Al/Al₂O₃ specimens. Al−Fe intermetallic compounds, such as Al₉Fe₂ and Al₃Fe, formed in the Al substrate because of the precipitation of Fe, which was an impurity of the Al foil, and the reaction with Al at the grain boundaries of Al during annealing processing. According to the evaluation results of mechanical and thermal properties, the Al/Al₂O₃ specimen deposited on the Ni film possessed the highest shear strength, thermal conductivity, and bonding area percentage, followed by the Cu, Ge, and Si films. The properties of the Al/Al₂O₃ specimens deposited with Ge and Si were relatively unsatisfactory, which could be because the deposited amorphous layers easily formed oxide, resulting in inferior adhesion between Al and Al₂O₃. Therefore, the optimal choice for use in high-power devices is Al/Al₂O₃, with the deposition of Ni film.

Keywords: direct-bonded aluminum, transient liquid phase, thermal conductivity, microstructures, shear strength

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Authors: Maor Farid, Oleg Gendelman

Abstract:

The following study deals with fluid vibration of a liquid in a partially filled vessel under periodic ground excitation. This external excitation might lead to hidraulic impact applied on the vessel inner walls. In order to model these sloshing dynamic regimes, several equivalent mechanical models were suggested in the literature, such as series of pendula or mass-spring systems that are able to impact the inner tank walls. In the following study, we use the latter methodology, use parameter values documented in literature corresponding to cylindrical tanks and consider structural elasticity of the tank. The hydraulic impulses are modeled by the high-exponent potential function. Additional system parameters are found with the help of Finite-Element (FE) analysis. Model-driven stress assessment method is developed. Finally, vibration mitigation performances of both tuned mass damper (TMD) and nonlinear energy sink (NES) are examined.

Keywords: nonlinear energy sink (NES), reduced-order modelling, liquid sloshing, vibration mitigation, vibro-impact dynamics

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Authors: Ke Lin, Steve Wu Qing Yang, Zhang Nan

Abstract:

The medicine and drugs has in the past been manufactured to the final products and then used laboratory analysis to verify their quality. However the industry needs crucially a monitoring technique for the final batch to batch quality check. The introduction of process analytical technology (PAT) provides an incentive to obtain real-time information about drugs on the production line, with the following optical techniques being considered: near-infrared (NIR) spectroscopy, Raman spectroscopy and imaging, mid-infrared spectroscopy with the use of chemometric techniques to quantify the final product. However, presents problems in that the spectra obtained will consist of many combination and overtone bands of the fundamental vibrations observed, making analysis difficult. In this work, we describe a non-destructive system and method for capsule and liquid medicine identification, more particularly, using terahertz time-domain spectroscopy and/or designed terahertz portable system for identifying different types of medicine in the package of capsule or in liquid medicine bottles. The target medicine can be detected directly, non-destructively and non-invasively.

Keywords: terahertz, non-destructive, non-invasive, chemical identification

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Authors: Julius Ilawe Osayi, Peter Osifo

Abstract:

Solid waste disposal, such as used tires is a global challenge as well as energy crisis due to rising energy demand amidst price uncertainty and depleting fossil fuel reserves. Therefore, the effectiveness of pyrolysis as a disposal method that can transform used tires into liquid fuel and other end-products has made the process attractive to researchers. Although used tires have been converted to liquid fuel using pyrolysis, there is the need to improve on the liquid fuel properties. Hence, this paper reports the investigation of zeolite NaY synthesized from kaolin, a locally abundant soil material in the Benin metropolis as a suitable catalyst and its effect on the properties of pyrolytic oil produced from used tires. The pyrolysis process was conducted for a range of 1 to 10 wt.% of catalyst concentration to used tire at a temperature of 600 oC, a heating rate of 15oC/min and particle size of 6mm. Although no significant increase in pyrolytic oil yield was observed compared to the previously investigated non-catalytic pyrolysis of a used tire. However, the Fourier transform infrared (FTIR), Nuclear Magnetic Resonance (NMR); and Gas chromatography-mass spectrometry (GC-MS) characterization results revealed the pyrolytic oil to possess an improved physicochemical and fuel properties alongside valuable industrial chemical species. This confirms the possibility of transforming kaolin into a catalyst suitable for improved fuel properties of the liquid fraction obtainable from thermal cracking of hydrocarbon materials.

Keywords: catalytic pyrolysis, fossil fuel, kaolin, pyrolytic oil, used tyres, Zeolite NaY

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