Search results for: liquid ammonia

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: Emma Castiglioni, Nigel Scrutton, Derren Heyes, Alistair Fielding

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By using light as trigger, it is possible to study many biological processes, such as the activity of genes, proteins, and other molecules, with precise spatiotemporal control. Caged compounds, where biologically active molecules are generated from an inert precursor upon laser photolysis, offer the potential to initiate such biological reactions with high temporal resolution. As light acts as the trigger for cleaving the protecting group, the ‘caging’ technique provides a number of advantages as it can be intracellular, rapid and controlled in a quantitative manner. We are developing caging strategies to study the catalytic cycle of a number of enzyme systems, such as nitric oxide synthase and ethanolamine ammonia lyase. These include the use of caged substrates, caged electrons and the possibility of caging the enzyme itself. In addition, we are developing a novel freeze-quench instrument to study these reactions, which combines rapid mixing and flashing capabilities. Reaction intermediates will be trapped at low temperatures and will be analysed by using electron paramagnetic resonance (EPR) spectroscopy to identify the involvement of any radical species during catalysis. EPR techniques typically require relatively long measurement times and very often, low temperatures to fully characterise these short-lived species. Therefore, common rapid mixing techniques, such as stopped-flow or quench-flow are not directly suitable. However, the combination of rapid freeze-quench (RFQ) followed by EPR analysis provides the ideal approach to kinetically trap and spectroscopically characterise these transient radical species. In a typical RFQ experiment, two reagent solutions are delivered to the mixer via two syringes driven by a pneumatic actuator or stepper motor. The new mixed solution is then sprayed into a cryogenic liquid or surface, and the frozen sample is then collected and packed into an EPR tube for analysis. The earliest RFQ instrument consisted of a hydraulic ram unit as a drive unit with direct spraying of the sample into a cryogenic liquid (nitrogen, isopentane or petroleum). Improvements to the RFQ technique have arisen from the design of new mixers in order to reduce both the volume and the mixing time. In addition, the cryogenic isopentane bath has been coupled to a filtering system or replaced by spraying the solution onto a surface that is frozen via thermal conductivity with a cryogenic liquid. In our work, we are developing a novel RFQ instrument which combines the freeze-quench technology with flashing capabilities to enable the studies of both thermally-activated and light-activated biological reactions. This instrument also uses a new rotating plate design based on magnetic couplings and removes the need for mechanical motorised rotation, which can otherwise be problematic at cryogenic temperatures.

Keywords: caged compounds, freeze-quench apparatus, photolysis, radicals

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Authors: Lawrence Koech, Hilary Rutto, Olga Mothibedi

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Worldwide demand for copper has led to intensive search for methods of extraction and recovery of copper from different sources. The study investigates the leaching properties of a low-grade copper ore by optimizing the leaching variables using response surface methodology. The effects of key parameters, i.e., temperature, solid to liquid ratio, stirring speed and pH, on the leaching rate constant was investigated using a pH stat apparatus. A Central Composite Design (CCD) of experiments was used to develop a quadratic model which specifically correlates the leaching variables and the rate constant. The results indicated that the model is in good agreement with the experimental data with a correlation coefficient (R2) of 0.93. The temperature and solid to liquid ratio were found to have the most substantial influence on the leaching rate constant. The optimum operating conditions for copper leaching from the ore were identified as temperature at 65C, solid to liquid ratio at 1.625 and stirring speed of 325 rpm which yielded an average leaching efficiency of 93.16%.

Keywords: copper, leaching, CCD, rate constant

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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: Rezala Houria, Valverde Jose Luis, Romero Amaya, Molinari Alessandra, Maldotti Andrea

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The escalation of oil prices in 1973 confronted the oil industry with the problem of how to maximize the processing of crude oil, especially the heavy fractions, to give gasoline components. Strong impetus was thus given to the development of catalysts with relatively large pore sizes, which were able to deal with larger molecules than the existing molecular sieves, and with good thermal and hydrothermal stability. The oil embargo in 1973 therefore acted as a stimulus for the investigation and development of pillared clays. Iron doped titania-pillared montmorillonite clays was prepared using bentonite from deposits of Maghnia in western-Algeria. The preparation method consists of differents steps (purification of the raw bentonite, preparation of a pillaring agent solution and exchange of the cations located between the clay layers with the previously formed iron/titanium solution). The characterization of this material was carried out by X-ray fluorescence spectrometry, X-ray diffraction, textural measures by BET method, inductively coupled plasma atomic emission spectroscopy, diffuse reflectance UV visible spectroscopy, temperature- programmed desorption of ammonia and atomic absorption.This new material was investigated as photocatalyst for selective oxygenation of the liquid alkylaromatics such as: toluene, paraxylene and orthoxylene and the photocatalytic properties of it were compared with those of the titanium-pillared clays.

Keywords: iron doping, montmorillonite clays, pillared clays, oil industry

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Authors: Mustapha Bouhoun Ali, Ahmed Yacine Badjah Hadj Ahmed, Mouloud Attou, Abdel Hamid Elias, Mohamed Amine Didi

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The extraction of uranium(VI) from aqueous solutions has been investigated using 1-hydroxyhexadecylidene-1,1-diphosphonic acid (HHDPA) and 1-hydroxydodecylidene-1,1-diphosphonic acid (HDDPA), which were synthesized and characterized by elemental analysis and by FT-IR, 1H NMR, 31P NMR spectroscopy. In this paper, we propose a tentative assignment for the shifts of those two ligands and their specific complexes with uranium(VI). We carried out the extraction of uranium(VI) by HHDPA and HDDPA from [carbon tetrachloride + 2-octanol (v/v: 90%/10%)] solutions. Various factors such as contact time, pH, organic/aqueous phase ratio and extractant concentration were considered. The optimum conditions obtained were: contact time = 20 min, organic/aqueous phase ratio = 1, pH value = 3.0 and extractant concentration = 0.3M. The extraction yields are more significant in the case of the HHDPA which is equipped with a hydrocarbon chain, longer than that of the HDDPA. Logarithmic plots of the uranium(VI) distribution ratio vs. pHeq and the extractant concentration showed that the ratio of extractant to extracted uranium(VI) (ligand/metal) is 2:1. The formula of the complex of uranium(VI) with the HHDPA and the DHDPA is UO2(H3L)2 (HHDPA and DHDPA are denoted as H4L). A spectroscopic analysis has showed that coordination of uranium(VI) takes place via oxygen atoms.

Keywords: liquid-liquid extraction, uranium(VI), 1-hydroxyalkylidene-1, 1-diphosphonic acids, HHDPA, HDDPA, aqueous solution

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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: Elvis Medina, Alejandro Karelovic, Romel Jiménez

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Catalytic ammonia decomposition represents an attractive alternative due to its high H₂ content (17.8% w/w), a product stream free of COₓ, among others; however, challenges need to be addressed for its consolidation as an H₂ chemical storage technology, especially, those focused on the synthesis of efficient bimetallic catalytic systems, as an alternative to the price and scarcity of ruthenium, the most active catalyst reported. In this sense, from the perspective of rational catalyst design, adjusting the main catalytic activity descriptor, a screening of supported catalysts with different compositional settings of cobalt-molybdenum metals is presented to evaluate their effect on the catalytic decomposition rate of ammonia. Subsequently, a kinetic study on the supported monometallic Co and Mo catalysts, as well as on the bimetallic CoMo catalyst with the highest activity is shown. The synthesis of catalysts supported on γ-alumina was carried out using the Charge Enhanced Dry Impregnation (CEDI) method, all with a 5% w/w loading metal. Seeking to maintain uniform dispersion, the catalysts were oxidized and activated (In-situ activation) using a flow of anhydrous air and hydrogen, respectively, under the same conditions: 40 ml min⁻¹ and 5 °C min⁻¹ from room temperature to 600 °C. Catalytic tests were carried out in a fixed-bed reactor, confirming the absence of transport limitations, as well as an Approach to equilibrium (< 1 x 10⁻⁴). The reaction rate on all catalysts was measured between 400 and 500 ºC at 53.09 kPa NH3. The synergy theoretically (DFT) reported for bimetallic catalysts was confirmed experimentally. Specifically, it was observed that the catalyst composed mainly of 75 mol% cobalt proved to be the most active in the experiments, followed by the monometallic cobalt and molybdenum catalysts, in this order of activity as referred to in the literature. A kinetic study was performed at 10.13 – 101.32 kPa NH3 and at four equidistant temperatures between 437 and 475 °C the data were adjusted to an LHHW-type model, which considered the desorption of nitrogen atoms from the active phase surface as the rate determining step (RDS). The regression analysis were carried out under an integral regime, using a minimization algorithm based on SLSQP. The physical meaning of the parameters adjusted in the kinetic model, such as the RDS rate constant (k₅) and the lumped adsorption constant of the quasi-equilibrated steps (α) was confirmed through their Arrhenius and Van't Hoff-type behavior (R² > 0.98), respectively. From an energetic perspective, the activation energy for cobalt, cobalt-molybdenum, and molybdenum was 115.2, 106.8, and 177.5 kJ mol⁻¹, respectively. With this evidence and considering the volcano shape described by the ammonia decomposition rate in relation to the metal composition ratio, the synergistic behavior of the system is clearly observed. However, since characterizations by XRD and TEM were inconclusive, the formation of intermetallic compounds should be still verified using HRTEM-EDS. From this point onwards, our objective is to incorporate parameters into the kinetic expressions that consider both compositional and structural elements and explore how these can maximize or influence H₂ production.

Keywords: CEDI, hydrogen carrier, LHHW, RDS

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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: V. Lokesh, M. Manjunathan, S. Sairam, K. Saithsh Kumar, R. Anantharaj

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The densities of pure and its binary mixtures of 1-Butyl-3-methyl imidazolium bis (trifluoro methyl sulfonyl) imide and 1–Ethyl-3-methyl imidazolium ethyl sulphate at different temperature, over the entire composition range were measured at 293.15, 298.15, 303.15, 308.15, 313.15, 318.15, 323.15, 328.15, 33.15, 338.15, 343.15 K. In this study, the liquid-liquid extraction procedure was used. From this experimental data, the excess molar volumes, apparent molar volume, partial molar volumes and the excess partial molar volumes have been calculated for over the whole composition range. Hence, the effect of temperature and composition on all derived thermodynamic properties of this binary mixture will be discussed in terms of intermolecular interactions.

Keywords: ionic liquid, interaction energy, effect of temperature, effect of composition

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Authors: Rozalina Keremedchieva, Ivan Svinyarov, Milen G. Bogdanov

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In continuation of a research project on the application of ionic liquids (ILs) as an alternative to the conventional organic solvents used in the recovery of value added chemicals of industrial interest1-3 we developed a procedure for back extraction and isolation in pure form of the biologically active alkaloid glaucine from IL-based aqueous solutions. One of the approaches applied was the formation of two-phase systems (IL-ATPS) by the addition of kosmotropic salts to the plant extract. The ability of the salts (Na2CO3, MgSO4, (NH4)2SO4, NaH2PO4) to induce the formation of two-phase systems and the influence of pH value on the partition coefficients of glaucine was comprehensively studied. As a result, it was found that the target alkaloid is preferably partitioned into the IL-rich phase regardless of the pH value of the medium and thus shows the inapplicability of the approach used for the isolation of the target compound from the ionic liquid. However, the results obtained can be used as a platform for the development of an analytical method for the quantitative determination of low concentrations of glaucine in biological samples. We further examined the ability of a series of organic solvents such as diethyl ether, Tert-butylmethyl ether, ethyl acetate, butyl acetate, toluene, chloroform, dichloromethane to recover glaucine form raw IL-based aqueous extracts. Optimal conditions for quantitative extraction of glaucine into chloroform were found from which, after removal of the solvent and subsequent recrystallization from ethanol, the target compound was isolated in a high purity as a hydrobromide salt – The form in which it entrance as an active ingredient in various medicines.

Keywords: natural products, ionic liquids, solid-liquid extraction, liquid-liquid extraction

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Authors: Azizza Mala, Babo Fadlalla, Elnour Mohamed, Siran Wang, Junfeng Li, Tao Shao

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Sweet sorghum is considered one of the best plants for silage production and is now a more important feed crop in many countries worldwide. It is simple to ensile because of its high water-soluble carbohydrates (WSC) concentration and low buffer capacity. This study investigated the effect of adding Pediococcus acidilactici AZZ5 and Lactobacillus plantarum AZZ4 isolated from elephant grass on the fermentation quality of sweet sorghum silage. One commercial bacteria Lactobacillus Plantarum, Ecosyl MTD/1(C.B.)), and two strains were used as additives Pediococcus acidilactici (AZZ5), Lactobacillus plantarum subsp. Plantarum (AZZ4) at 6 log colony forming units (cfu)/g of fresh sweet sorghum grass in laboratory silos (1000g). After 15, 30, and 60 days, the silos for each treatment were opened. All of the isolated strains enhanced the silage quality of sweet sorghum silage compared to the control, as evidenced by significantly (P < 0.05) lower ammonia nitrogen (NH3-N) content and undesirable microbial counts, as well as greater lactic acid (L.A.) contents and lactic acid/acetic acid (LA/AA) ratios. In addition, AZZ4 performed better than all other inoculants during ensiling, as evidenced by a significant (P < 0.05) reduction in pH and ammonia-N contents and a significant increase in lactic acid contents.

Keywords: fermentation, lactobacillus plantarum, lactic acid bacteria, pediococcus acidilactic, sweet sorghum

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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: 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

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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

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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: Khalid S. Hashim, Andy Shaw, Rafid Alkhaddar

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Dissolved oxygen concentration (DO) plays a key role in the electrocoagulation process (EC) as it oxidizes the heavy metals, ammonia, and cyanide into other forms that can be removed easily from water. For instance, the DO oxidises Fe (II) to Fe (III), As (III) to As (V), and cyanide to cyanate and then to ammonia. As well as, removal of nitrogenous compounds accomplishes by the presence of DO. Hence, many of the previous investigations used external aerators to provide the required DO inside EC reactors especially when the water being treated has low DO (such as leachate and highly polluted waters with organic matter); or when the DO depleted during the EC treatment. Although the external aeration process effectively enhances the DO concentration, it has a significant impact on energy consumption. Where, the presence of air bubbles increases the electrical resistance of the EC cell that increase the energy consumption in consequence. Thus, the present project aims to fill this gap by an innovative use of perforated flow columns in the designing of a new EC reactor (ECR1). The new reactor (ECR1) consisted of a Perspex made cylinder container having a controllable working volume of 0.5 to 1 L. It supplied with a flow column that consisted of perorated discoid electrodes that made from aluminium. In order to investigate the performance of ECR1; water samples with a controlled DO concentration were pumped at different flow rates (110, 220, and 440 ml/min) to the ECR1 for 10 min. The obtained results demonstrated that the ECR1 increased the DO concentration from 5.0 to 9.54, 10.53, and 11.0 mg/L which equivalent to 90.8%, 110.6%, and 120% at flow rates of 110, 220, and 440 mL/min respectively.

Keywords: dissolved oxygen, flow column, electrocoagulation, aluminium electrodes

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Authors: Nadia Allouache, Omar Rahli

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Many promising technologies have been developed to harness the sun's energy. These technologies help in economizing energy and environmental protection. The solar refrigerating systems are one of these important technologies. In addition to environmental benefits and energy saving, adsorption refrigerating systems have many advantages such as lack of moving parts, simplicity of construction and low operating costs. The work aimed to establish the main factors that affect the performances of an adsorption refrigerating system using different geometries of adsorbers and different adsorbent-adsorbate pairs. The numerical modeling of the heat and mass transfer in the system, using various working pairs, such as: activated carbon-ammonia, calcium chlorid-ammonia, activated carbon fiber- methanol and activated carbon AC35-methanol, show that the adsorber design can influence the system performances; The thermal performances of system are better in the annular configuration case. An optimal value of generating temperature is observed in annular adsorber case for which the thermal performance of the cooling system is maximal. While in the plate adsorber, above a certain value of generating temperature, the performance of the system remains almost constant. The environmental conditions such as solar radiation and pressure have a great influence in the system efficiency, and the choice of the working pair depends on the environmental conditions and the geometry of the adsorber.

Keywords: adsorber geometry, numerical modeling, optimal environmental conditions, working pairs.

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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: Ghodsieh Isapour Toutizad, Aiyong Wang, Joonsoo Han, Derek Creaser, Louise Olsson, Magnus Skoglundh, Hanna HaRelind

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Nitrous oxide (N2O), which is generally formed as a byproduct of industrial chemical processes and fossil fuel combustion, has attracted considerable attention due to its destructive role in global warming and ozone layer depletion. From various developed technologies used for lean NOx reduction, the selective catalytic reduction (SCR) of NOx with ammonia is presently the most applied method. Therefore, the development of catalysts for efficient lean NOx reduction without forming N2O in the process, or only forming it to a very small extent from the exhaust gases is of crucial significance. One type of catalysts that nowadays are used for this aim are zeolite-based catalysts. It is owing to their remarkable catalytic performance under practical reaction conditions such as high thermal stability and high N2 selectivity. Among all zeolites, copper ion-exchanged zeolites, with CHA, MFI, and BEA framework structure (like SSZ-13, ZSM-5 and Beta, respectively), represent higher hydrothermal stability, high activity and N2 selectivity. This work aims at investigating the effect of the zeolite framework structure on the formation of N2O during NH3-SCR reaction conditions over three Cu-based zeolites ranging from small-pore to large-pore framework structure. In the zeolite framework, Cu exists in two cationic forms, that can catalyze the SCR reaction by activating NO to form NO+ and/or surface nitrate species. The nitrate species can thereafter react with NH3 to form another intermediate, ammonium nitrate, which seems to be one source for N2O formation at low temperatures. The results from in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) indicate that during the NO oxidation step, mainly NO+ and nitrate species are formed on the surface of the catalysts. The intensity of the absorption peak attributed to NO+ species is higher for the Cu-CHA sample compared to the other two samples, indicating a higher stability of this species in small cages. Furthermore, upon the addition of NH3, through the standard SCR reaction conditions, absorption peaks assigned to N-H stretching and bending vibrations are building up. At the same time, negative peaks are evolving in the O-H stretching region, indicating blocking/replacement of surface OH-groups by NH3 and NH4+. By removing NH3 and adding NO2 to the inlet gas composition, the peaks in the N-H stretching and bending vibration regions show a decreasing trend in intensity, with the decrease being more pronounced for increasing pore size. It can probably be owing to the higher accumulation of ammonia species in the small-pore size zeolite compared to the other two samples. Furthermore, it is worth noting that the ammonia surface species are strongly bonded to the CHA zeolite structure, which makes it more difficult to react with NO2. To conclude, the framework structure of the zeolite seems to play an important role in the formation and reactivity of surface species relevant for the SCR process. Here we intend to discuss the connection between the zeolite structure, the surface species, and the formation of N2O during ammonia-SCR.

Keywords: fast SCR, nitrous oxide, NOx, standard SCR, zeolites

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Authors: Mbongeni Mabaso, Kandasamy Moodley, Gan Redhi

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The recovery of industrially valuable organic solvents from liquid waste, generated in chemical processes, is economically crucial to countries which need to import organic solvents. In view of this, the main objective of this study was to determine the ability of selected ionic liquids, namely, 1-ethyl-3-methylimidazolium ethylsulphate, [EMIM] [ESO4] and 1-ethyl-3-methylpyridinium ethylsulphate, [EMpy][ESO4] to recover aromatic components from spent paint solvents. Preliminary studies done on the liquid waste, received from a paint manufacturing company, showed that the aromatic components were present in the range 6 - 21 % by volume. The separation of the aromatic components was performed with the ionic liquids listed above. The phases, resulting from the separation of the mixtures, were analysed with a Gas Chromatograph (GC) coupled to a FID detector. Chromatograms illustrate that the chosen ZB-Wax-Plus column gave excellent separation of all components of interest from the mixtures, including the isomers of xylene. The concentrations of aromatics recovered from the spent solvents were found to be the % ranges 13-33 and 23-49 respectively for imidazolium and pyridinium ionic liquids. These results also show that there is a significant correlation between π-character of ionic liquids and the level of extraction. It is therefore concluded that ionic liquids have the potential for macro-scale recovery of re-useable solvents present in liquid waste emanating from paint manufacture.

Keywords: synthesis, ionic liquid, imidazolium, pyridinium, extraction, aromatic solvents, spent paint organic solvents

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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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