Search results for: solvent evaporation

Authors: Kuheli Chakrabarty, Animesh Ghosh, Atanu Roy, Gourab Kanti Das

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Aldol reaction is an important class of carbon-carbon bond forming reactions. One of the popular ways to impose asymmetry in aldol reaction is the introduction of chiral auxiliary that binds the approaching reactants and create dissymmetry in the reaction environment, which finally evolves to enantiomeric excess in the aldol products. The last decade witnesses the usage of natural amino acids as chiral auxiliary to control the stereoselectivity in various carbon-carbon bond forming processes. In this context, L-proline was found to be an effective organocatalyst in asymmetric aldol additions. In last few decades the use of water as solvent or co-solvent in asymmetric organocatalytic reaction is increased sharply. Simple amino acids like L-proline does not catalyze asymmetric aldol reaction in aqueous medium not only that, In organic solvent medium high catalytic loading (~30 mol%) is required to achieve moderate to high asymmetric induction. In this context, huge efforts have been made to modify L-proline and 4-hydroxy-L-proline to prepare organocatalyst for aqueous medium asymmetric aldol reaction. Here, we report the result of our DFT calculations on asymmetric aldol reaction of benzaldehyde, p-NO2 benzaldehyde and t-butyraldehyde with a number of ketones using L-proline hydrazide as organocatalyst in wet solvent free condition. Gaussian 09 program package and Gauss View program were used for the present work. Geometry optimizations were performed using B3LYP hybrid functional and 6-31G(d,p) basis set. Transition structures were confirmed by hessian calculation and IRC calculation. As the reactions were carried out in solvent free condition, No solvent effect were studied theoretically. Present study has revealed for the first time, the direct involvement of two water molecules in the aldol transition structures. In the TS, the enamine and the aldehyde is connected through hydrogen bonding by the assistance of two intervening water molecules forming a supramolecular network. Formation of this type of supramolecular assembly is possible due to the presence of protonated -NH2 group in the L-proline hydrazide moiety, which is responsible for the favorable entropy contribution to the aldol reaction. It is also revealed from the present study that, water assisted TS is energetically more favorable than the TS without involving any water molecule. It can be concluded from this study that, insertion of polar group capable of hydrogen bond formation in the L-proline skeleton can lead to a favorable aldol reaction with significantly high enantiomeric excess in wet solvent free condition by reducing the activation barrier of this reaction.

Keywords: aldol reaction, DFT, organocatalysis, transition structure

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Authors: Dariush Jafari, S. Mostafa Nowee

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In this study a ternary system containing sodium chloride as solute, water as primary solvent and ethanol as the antisolvent was considered to investigate the application of artificial neural network (ANN) in prediction of sodium solubility in the mixture of water as the solvent and ethanol as the antisolvent. The system was previously studied using by Extended UNIQUAC model by the authors of this study. The comparison between the results of the two models shows an excellent agreement between them (R2=0.99), and also approves the capability of ANN to predict the thermodynamic behavior of ternary electrolyte systems which are difficult to model.

Keywords: thermodynamic modeling, ANN, solubility, ternary electrolyte system

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Authors: Alaa Y. Ali, Natalie P. Holmes, John Holdsworth, Warwick Belcher, Paul Dastoor, Xiaojing Zhou

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Multi-layered graphene has been produced under low temperature chemical vapour deposition (CVD) growth conditions by utilizing an organic solvent and polymer film source. Poly(methylmethacrylate) (PMMA) was dissolved in chlorobenzene solvent and used as a drop-cast film carbon source on a quartz slide. A source temperature (T_source) of 180 °C provided sufficient carbon to grow graphene, as identified by Raman spectroscopy, on clean copper foil catalytic surfaces.  Systematic variation of hydrogen gas (H₂) flow rate from 25 standard cubic centimeters per minute (sccm) to 100 sccm and CVD temperature (T_growth) from 400 to 800 °C, yielded graphene films of varying quality as characterized by Raman spectroscopy. The optimal graphene growth parameters were found to occur with a hydrogen flow rate of 75 sccm sweeping the 180 °C source carbon past the Cu foil at 600 °C for 1 min. The deposition at 600 °C with a H₂ flow rate of 75 sccm yielded a 2D band peak with ~53.4 cm^-1 FWHM and a relative intensity ratio of the G to 2D bands (I_G/I_2D) of 0.21. This recipe fabricated a few layers of good quality graphene.

Keywords: graphene, chemical vapor deposition, carbon source, low temperature growth

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Authors: Sara Camino, Fernando Vega, Mercedes Cano, Benito Navarrete, José A. Camino

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Carbon capture and storage (CCS) technologies should play a relevant role towards low-carbon systems in the European Union by 2030. Partial oxy-combustion emerges as a promising CCS approach to mitigate anthropogenic CO₂ emissions. Its advantages respect to other CCS technologies rely on the production of a higher CO₂ concentrated flue gas than these provided by conventional air-firing processes. The presence of more CO₂ in the flue gas increases the driving force in the separation process and hence it might lead to further reductions of the energy requirements of the overall CO₂ capture process. A higher CO₂ concentrated flue gas should enhance the CO₂ capture by chemical absorption in solvent kinetic and CO₂ cyclic capacity. They have impact on the performance of the overall CO₂ absorption process by reducing the solvent flow-rate required for a specific CO₂ removal efficiency. Lower solvent flow-rates decreases the reboiler duty during the regeneration stage and also reduces the equipment size and pumping costs. Moreover, R&D activities in this field are focused on novel solvents and blends that provide lower CO₂ absorption enthalpies and therefore lower energy penalties associated to the solvent regeneration. In this respect, sterically hindered amines are considered potential solvents for CO₂ capture. They provide a low energy requirement during the regeneration process due to its molecular structure. However, its absorption kinetics are slow and they must be promoted by blending with faster solvents such as monoethanolamine (MEA) and piperazine (PZ). In this work, the kinetic behavior of two sterically hindered amines were studied under partial oxy-combustion conditions and compared with MEA. A lab-scale semi-batch reactor was used. The CO₂ composition of the synthetic flue gas varied from 15%v/v – conventional coal combustion – to 60%v/v – maximum CO₂ concentration allowable for an optimal partial oxy-combustion operation. Firstly, 2-amino-2-methyl-1-propanol (AMP) showed a hybrid behavior with fast kinetics and a low enthalpy of CO₂ absorption. The second solvent was Isophrondiamine (IF), which has a steric hindrance in one of the amino groups. Its free amino group increases its cyclic capacity. In general, the presence of higher CO₂ concentration in the flue gas accelerated the CO₂ absorption phenomena, producing higher CO₂ absorption rates. In addition, the evolution of the CO2 loading also exhibited higher values in the experiments using higher CO₂ concentrated flue gas. The steric hindrance causes a hybrid behavior in this solvent, between both fast and slow kinetic solvents. The kinetics rates observed in all the experiments carried out using AMP were higher than MEA, but lower than the IF. The kinetic enhancement experienced by AMP at a high CO2 concentration is slightly over 60%, instead of 70% – 80% for IF. AMP also improved its CO₂ absorption capacity by 24.7%, from 15%v/v to 60%v/v, almost double the improvements achieved by MEA. In IF experiments, the CO₂ loading increased around 10% from 15%v/v to 60%v/v CO₂ and it changed from 1.10 to 1.34 mole CO₂ per mole solvent, more than 20% of increase. This hybrid kinetic behavior makes AMP and IF promising solvents for partial oxy–combustion applications.

Keywords: absorption, carbon capture, partial oxy-combustion, solvent

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Authors: Mohamed Abdoul-Hakim, A. Zeroual, H. Garmes

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In this work, we theoretically evaluated the reactivity of four 4-methyl-3-oxo-1,2-pyrazolidinium ylides with 2-Chlorobenzimidazole in MeOH in basic medium using DFT at the B3LYP/6-311+G(d,p) level. The analysis of the results shows that apart from its ability to retain its electrons, the deprotonated 2-Chlorobenzimidazole has a higher nucleophilic character. The reaction requires energy input to initiate the nucleophilic attack of the 2-Chlorobenzimidazole anion, and the inclusion of the solvent effect facilitates the formation of two regioisomers via an intramolecular vinyl nucleophilic substitution (SNVi). The transition states of this latter step are stabilized by charge transfer interactions σ(N-C) →σ*(C-Cl) for the more favorable regioisomer and n(N)→σ*(C-Cl) for the other regioisomer.

Keywords: benzonitrile N-oxide, DFT, intramolecular vinyl nucleophilic substitution (SNVi), 4-methyl-3-OXO-1, 2-pyrazolidinium ylides

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Authors: Maria Bercea, Bernhard A. Wolf

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The thermodynamic behavior for solutions of poly (methyl methacrylate-ran-t-butyl methacrylate) of variable composition as compared with the corresponding homopolymers was investigated by light scattering measurements carried out for dilute solutions and vapor pressure measurements of concentrated solutions. The complex dependencies of the Flory Huggins interaction parameter on concentration and copolymer composition in solvents of different polarity (toluene and chloroform) can be understood by taking into account the ability of the polymers to rearrange in a response to changes in their molecular surrounding. A recent unified thermodynamic approach was used for modeling the experimental data, being able to describe the behavior of the different solutions by means of two adjustable parameters, one representing the effective number of solvent segments and another one accounting for the interactions between the components. Thus, it was investigated how the solvent quality changes with the composition of the copolymers through the Gibbs energy of mixing as a function of polymer concentration. The largest reduction of the Gibbs energy at a given composition of the system was observed for the best solvent. The present investigation proves that the new unified thermodynamic approach is a general concept applicable to homo- and copolymers, independent of the chain conformation or shape, molecular and chemical architecture of the components and of other dissimilarities, such as electrical charges.

Keywords: random copolymers, Flory Huggins interaction parameter, Gibbs energy of mixing, chemical architecture

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Authors: Kamalesh Kumar Singh

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Due to increasing trends of electronic waste, specially the ICT related gadgets, their green recycling is still a greater challenge. This article presents a two-stage, eco-friendly hydrometallurgical route for the recovery of gold from the delaminated metallic layers of waste mobile phone Printed Circuit Boards (PCBs). Initially, mobile phone PCBs are downsized (1x1 cm²) and treated with an organic solvent dimethylacetamide (DMA) for the separation of metallic fraction from non-metallic glass fiber. In the first stage, liberated metallic sheets are used for the selective dissolution of copper in an aqueous leaching reagent. Influence of various parameters such as type of leaching reagent, the concentration of the solution, temperature, time and pulp density are optimized for the effective leaching (almost 100%) of copper. Results have shown that 3M nitric acid is a suitable reagent for copper leaching at room temperature and considering chemical features, gold remained in solid residue. In the second stage, the separated residue is used for the recovery of gold by using sulphuric acid with a combination of halide salt. In this halide leaching, Cl₂ or Br₂ is generated as an in-situ oxidant to improve the leaching of gold. Results have shown that almost 92 % of gold is recovered at the optimized parameters.

Keywords: printed circuit boards, delamination, leaching, solvent extraction, recovery

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Authors: A. Brinda Lakshmi, J. Lakshmi Priya

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Cantaloupes (muskmelon and watermelon) contain biologically active molecules such as carotenoids which are natural pigments used as food colorants and afford health benefits. ß-carotene is the major source of carotenoids present in muskmelon and watermelon shell. Carotenoids were extracted using Microwave assisted extraction (MAE) and Ultrasound assisted extraction (UAE) utilising organic lipophilic solvents such as acetone, methanol, and hexane. Extraction conditions feed-solvent ratio, microwave power, ultrasound frequency, temperature and particle size were varied and optimized. It was found that the yield of carotenoids was higher using UAE than MAE, and muskmelon had the highest yield of carotenoids when was ethanol used as a solvent for 0.5 mm particle size.

Keywords: carotenoids, extraction, muskmelon shell, watermelon shell

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Authors: Endalamaw Ewnu Kassa, Ade Kurniawan, Ya-Fen Wu, Sajal Biring

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Perovskite-based gas sensors represent a highly promising materials within the realm of gas sensing technology, with a particular focus on detecting ammonia (NH3) due to its potential hazards. Our work conducted thorough comparison of various solvents, including dimethylformamide (DMF), DMF-dimethyl sulfoxide (DMSO), dimethylacetamide (DMAC), and DMAC-DMSO, for the preparation of our perovskite solution (MAPbI3). Significantly, we achieved an exceptional response at 10 ppm of ammonia gas by employing a binary solvent mixture of DMAC-DMSO. In contrast to prior reports that relied on single solvents for MAPbI3 precursor preparation, our approach using mixed solvents demonstrated a marked improvement in gas sensing performance. We attained enhanced surface coverage, a reduction in pinhole occurrences, and precise control over grain size in our perovskite films through the careful selection and mixtures of appropriate solvents. This study shows a promising potential of employing binary and multi-solvent mixture strategies as a means to propel advancements in gas sensor technology, opening up new opportunities for practical applications in environmental monitoring and industrial safety.

Keywords: sensors, binary solvents, ammonia, sensitivity, grain size, pinholes, surface coverage

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Authors: Seema Paul, Jesper Oppelstrup, Roger Thunvik, Vladimir Cvetkovic

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Lake Victoria is the second largest fresh water body in the world, located in East Africa with a catchment area of 250,000 km², of which 68,800 km² is the actual lake surface. The hydrodynamic processes of the shallow (40–80 m deep) water system are unique due to its location at the equator, which makes Coriolis effects weak. The paper describes a St.Venant shallow water model of Lake Victoria developed in COMSOL Multiphysics software, a general purpose finite element tool for solving partial differential equations. Depth soundings taken in smaller parts of the lake were combined with recent more extensive data to resolve the discrepancies of the lake shore coordinates. The topography model must have continuous gradients, and Delaunay triangulation with Gaussian smoothing was used to produce the lake depth model. The model shows large-scale flow patterns, passive tracer concentration and water level variations in response to river and tracer inflow, rain and evaporation, and wind stress. Actual data of precipitation, evaporation, in- and outflows were applied in a fifty-year simulation model. It should be noted that the water balance is dominated by rain and evaporation and model simulations are validated by Matlab and COMSOL. The model conserves water volume, the celerity gradients are very small, and the volume flow is very slow and irrotational except at river mouths. Numerical experiments show that the single outflow can be modelled by a simple linear control law responding only to mean water level, except for a few instances. Experiments with tracer input in rivers show very slow dispersion of the tracer, a result of the slow mean velocities, in turn, caused by the near-balance of rain with evaporation. The numerical and hydrodynamical model can evaluate the effects of wind stress which is exerted by the wind on the lake surface that will impact on lake water level. Also, model can evaluate the effects of the expected climate change, as manifest in changes to rainfall over the catchment area of Lake Victoria in the future.

Keywords: bathymetry, lake flow and steady state analysis, water level validation and concentration, wind stress

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Authors: S. M. Anisuzzaman, Sariah Abang, Awang Bono, D. Krishnaiah, N. M. Ismail, G. B. Sandrison

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Wax and asphaltene are high molecular weighted compounds that contribute to the stability of crude oil at a dispersed state. Transportation of crude oil along pipelines from the oil rig to the refineries causes fluctuation of temperature which will lead to the coagulation of wax and flocculation of asphaltenes. This paper focuses on the prevention of wax and asphaltene precipitate deposition on the inner surface of the pipelines by using a wax inhibitor and an asphaltene dispersant. The novelty of this prevention method is the combination of three substances; a wax inhibitor dissolved in a wax inhibitor solvent and an asphaltene solvent, namely, ethylene-vinyl acetate (EVA) copolymer dissolved in methylcyclohexane (MCH) and toluene (TOL) to inhibit the precipitation and deposition of wax and asphaltene. The objective of this paper was to optimize the percentage composition of each component in this inhibitor which can maximize the viscosity reduction of crude oil. The optimization was divided into two stages which are the laboratory experimental stage in which the viscosity of crude oil samples containing inhibitor of different component compositions is tested at decreasing temperatures and the data optimization stage using response surface methodology (RSM) to design an optimizing model. The results of experiment proved that the combination of 50% EVA + 25% MCH + 25% TOL gave a maximum viscosity reduction of 67% while the RSM model proved that the combination of 57% EVA + 20.5% MCH + 22.5% TOL gave a maximum viscosity reduction of up to 61%.

Keywords: asphaltene, ethylene-vinyl acetate, methylcyclohexane, toluene, wax

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Authors: Glemarie C. Hermosa, Sheng-Jie You, Chien Chih Hu

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Efficient separation technologies are required for the removal of carbon dioxide from natural gas streams. Membrane-based natural gas separation has emerged as one of the fastest growing technologies, due to the compactness, higher energy efficiency and economic advantages which can be reaped. The removal of Carbon dioxide from gas streams using membrane technology will also give the advantage like environmental friendly process compared to the other technologies used in gas separation. In this study, Polyimide membranes, which are mostly used in the separation of gases, are blended with a new kind of solvent: Deep Eutectic Solvents or simply DES. The three types of DES are used are choline chloride based mixed with three different hydrogen bond donors: Lactic acid, N-methylurea and Urea. The blending of the DESs to Polyimide gave out high permeability performance. The Gas Separation performance for all the membranes involving CO2/CH4 showed low performance while for CO2/N2 surpassed the performance of some studies. Among the three types of DES used the solvent Choline Chloride/Lactic acid exhibited the highest performance for both Gas Separation applications. The values are 10.5 for CO2/CH4 selectivity and 60.5 for CO2/N2. The separation results for CO2/CH4 may be due to the viscosity of the DESs affecting the morphology of the fabricated membrane thus also impacts the performance. DES/blended Polyimide membranes fabricated are novel and have the potential of a low-cost and environmental friendly application for gas separation.

Keywords: deep eutectic solvents, gas separation, polyimide blends, polyimide membranes

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Authors: Kirill D. Semavin, Norbert S. Chilingarov, Eugene.V. Skokan

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The ionic liquids (ILs) based on imidazolium cation are well known nowadays. The changing anions and substituents in imidazolium ring may lead to different physical and chemical properties of ILs. It is important that such ILs with halogen as anion are characterized by a low thermal stability. The data about thermal stability of 1-ethyl-3-methylimidazolium chloride are ambiguous. In the works of last years, thermal stability of this IL was investigated by thermogravimetric analysis and obtained results are contradictory. Moreover, in the last study, it was shown that the observed temperature of the beginning of decomposition significantly depends on the experimental conditions, for example, the heating rate of the sample. The vapor pressure of this IL is not presented at the literature. In this study, the vapor pressure of 1-ethyl-3-methylimidazolium chloride was obtained by Knudsen effusion mass-spectrometry (KEMS). The samples of [ЕMIm]Cl (purity > 98%) were supplied by Sigma–Aldrich and were additionally dried at dynamic vacuum (T = 60 0C). Preliminary procedures with Il were derived into glove box. The evaporation studies of [ЕMIm]Cl were carried out by KEMS with using original research equipment based on commercial MI1201 magnetic mass spectrometer. The stainless steel effusion cell had an effective evaporation/effusion area ratio of more than 6000. The cell temperature, measured by a Pt/Pt−Rh (10%) thermocouple, was controlled by a Termodat 128K5 device with an accuracy of ±1 K. In first step of this study, the optimal temperature of experiment and heating rate of samples were customized: 449 K and 5 K/min, respectively. In these conditions the sample is decomposed, but the experimental measurements of the vapor pressures are possible. The thermodynamic activity of [ЕMIm]Cl is close to 1 and products of decomposition don’t affect it at firstly 50 hours of experiment. Therefore, it lets to determine the saturated vapor pressure of IL. The electronic ionization mass-spectra shows that the decomposition of [ЕMIm]Cl proceeds with two ways. Nonetheless, the MALDI mass spectra of the starting sample and residue in the cell were similar. It means that the main decomposition products are gaseous under experimental conditions. This result allows us to obtain information about the kinetics of [ЕMIm]Cl decomposition. Thus, the original KEMS-based procedure made it possible to determine the IL vapor pressure under decomposition conditions. Also, the loss of sample mass due to the evaporation was obtained.

Keywords: ionic liquids, Knudsen effusion mass spectrometry, thermal stability, vapor pressure

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Authors: Hee-Jae Suh, Mi-Na Hong, Min-Ji Kim, Yeon-Seong Jeong, Ok-Hwan Lee, Jae-Wook Shin, Hyang-Sook Chun, Chan Lee

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Brown HT is a bis-azo dye which is permitted in EU as a food colorant. So far, many studies have focused on HPLC using diode array detection (DAD) analysis for detection of this food colorant with different columns and mobile phases. Even though these methods make it possible to detect Brown HT, low recovery, reproducibility, and linearity are still the major limitations for the application in foods. The purpose of this study was to compare various methods for the analysis of Brown HT and to develop an improved analytical methods including pretreatment. Among tested analysis methods, best resolution of Brown HT was observed when the following solvent was applied as a eluent; solvent A of mobile phase was 0.575g NH4H2PO4, and 0.7g Na2HPO4 in 500mL water added with 500mL methanol. The pH was adjusted using phosphoric acid to pH 6.9 and solvent B was methanol. Major peak for Brown HT appeared at the end of separation, 13.4min after injection. This method exhibited relatively high recovery and reproducibility compared with other methods. LOD (0.284 ppm), LOQ (0.861 ppm), resolution (6.143), and selectivity (1.3) of this method were better than those of ammonium acetate solution method which was most frequently used. Precision and accuracy were verified through inter-day test and intra-day test. Various methods for sample pretreatments were developed for different foods and relatively high recovery over 80% was observed in all case. This method exhibited high resolution and reproducibility of Brown HT compared with other previously reported official methods from FSA and, EU regulation.

Keywords: analytic method, Brown HT, food colorants, pretreatment method

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Authors: J. Ticona Chambi, E. A. De Almeida, C. A. Andrade Raymundo Gaiotto, A. M. Do Espírito Santo, L. Infantes, S. L. Cuffini

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The solubility of active pharmaceutical ingredients (APIs) is challenging for the pharmaceutical industry. The new multicomponent crystalline forms as cocrystal and solvates present an opportunity to improve the solubility of APIs. Commonly, the procedure to obtain multicomponent crystalline forms of a drug starts by screening the drug molecule with the different coformers/solvents. However, it is necessary to develop methods to obtain multicomponent forms in an efficient way and with the least possible environmental impact. The Hansen Solubility Parameters (HSPs) is considered a tool to obtain theoretical knowledge of the solubility of the target compound in the chosen solvent. H-Bond Propensity (HBP), Molecular Complementarity (MC), Coordination Values (CV) are tools used for statistical prediction of cocrystals developed by the Cambridge Crystallographic Data Center (CCDC). The HSPs and the CCDC tools are based on inter- and intra-molecular interactions. The curcumin (Cur), target molecule, is commonly used as an anti‐inflammatory. The demethoxycurcumin (Demcur) and bisdemethoxycurcumin (Bisdcur) are natural analogues of Cur from turmeric. Those target molecules have differences in their solubilities. In this way, the work aimed to analyze and compare different tools for multicomponent forms prediction (solvates) of Cur, Demcur and Biscur. The HSP values were calculated for Cur, Demcur, and Biscur using the chemical group contribution methods and the statistical optimization from experimental data. The HSPmol software was used. From the HSPs of the target molecules and fifty solvents (listed in the HSP books), the relative energy difference (RED) was determined. The probability of the target molecules would be interacting with the solvent molecule was determined using the CCDC tools. A dataset of fifty molecules of different organic solvents was ranked for each prediction method and by a consensus ranking of different combinations: HSP, CV, HBP and MC values. Based on the prediction, 15 solvents were selected as Dimethyl Sulfoxide (DMSO), Tetrahydrofuran (THF), Acetonitrile (ACN), 1,4-Dioxane (DOX) and others. In a starting analysis, the slow evaporation technique from 50°C at room temperature and 4°C was used to obtain solvates. The single crystals were collected by using a Bruker D8 Venture diffractometer, detector Photon100. The data processing and crystal structure determination were performed using APEX3 and Olex2-1.5 software. According to the results, the HSPs (theoretical and optimized) and the Hansen solubility sphere for Cur, Demcur and Biscur were obtained. With respect to prediction analyses, a way to evaluate the predicting method was through the ranking and the consensus ranking position of solvates already reported in the literature. It was observed that the combination of HSP-CV obtained the best results when compared to the other methods. Furthermore, as a result of solvent selected, six new solvates, Cur-DOX, Cur-DMSO, Bicur-DOX, Bircur-THF, Demcur-DOX, Demcur-ACN and a new Biscur hydrate, were obtained. Crystal structures were determined for Cur-DOX, Biscur-DOX, Demcur-DOX and Bicur-Water. Moreover, the unit-cell parameter information for Cur-DMSO, Biscur-THF and Demcur-ACN were obtained. The preliminary results showed that the prediction method is showing a promising strategy to evaluate the possibility of forming multicomponent. It is currently working on obtaining multicomponent single crystals.

Keywords: curcumin, HSPs, prediction, solvates, solubility

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Authors: Wei-Song Hung

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We utilized pressure, vacuum, and evaporation-assisted self-assembly techniques through which graphene oxide (GO) was deposited on modified polyacrylonitrile (mPAN). The fabricated composite GO/mPAN membranes were applied to dehydrate 1-butanol mixtures by pervaporation. Varying driving forces in the self-assembly techniques induced different GO assembly layer microstructures. XRD results indicated that the GO layer d-spacing varied from 8.3 Å to 11.5 Å. The self-assembly technique with evaporation resulted in a heterogeneous GO layer with loop structures; this layer was shown to be hydrophobic, in contrast to the hydrophilic layer formed from the other two techniques. From the pressure-assisted technique, the composite membrane exhibited exceptional pervaporation performance at 30 C: concentration of water at the permeate side = 99.6 wt% and permeation flux = 2.54 kg m-2 h-1. Moreover, the membrane sustained its operating stability at a high temperature of 70 C: a high water concentration of 99.5 wt% was maintained, and a permeation flux as high as 4.34 kg m-2 h-1 was attained. This excellent separation performance stemmed from the dense, highly ordered laminate structure of GO.

Keywords: graphene oxide, self-assembly, alcohol dehydration, polyacrylonitrile (mPAN)

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Authors: Arash Azarpanah, Masoud Zadehbagheri, Shorangiz Javanmardi

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Abiotic stresses are the principle threat to plant growth and crop productivity all over the world. In order to improve the germination of corn seeds in drought stress conditions, effect of seed priming by various concentrations of salicylic acid (SA) (0.8 and 0.2 mM) on activities of catalase and peroxidase in Zea mays L. plant (Var-Sc.704) was evaluated at Agriculture Research Center located in Arsenjan city in Iran, during summer 2013. A farm research was done in RCBD as factorial with three replications. We considered four irrigation was carried out once the cumulative evaporation from Pan Class A come to 40, 60, 80 and 100 mm. Results illustrated that drought stress significantly increased activities of catalase and peroxidase and also treatment with salicylic acid significantly increased activities of catalase and peroxidase. In addition, treatment with salicylic acid enhances drought tolerance in Zea mays L. plant (Var-Sc.704) with increasing activities of antioxidant enzymes.

Keywords: catalase, corn, salicylic acid, water deficits stress, cumulative evaporation, Pan Class A

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Authors: S. A. Jumare, A. O. Tijani, M. F. Siraj, B. V. Babatunde

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This research investigated the comparative analysis of oil extracted from cotton and watermelon seeds using solvent extraction process. Normal ethyl-ether was used as solvent in the extraction process. The AOAC method of Analysis was employed in the determination of the physiochemical properties of the oil. The chemical properties of the oil determined include the saponification value, free fatty acid, iodine value, peroxide value and acid value. The physical properties of the oil determined include specific gravity, refractive index, colour, odour, taste and pH. The value obtained for cottonseed oil are saponification value (187mgKOH/g), free fatty acid (5.64mgKOH/g), iodine value (95.2g/100), peroxide value (9.33meq/kg), acid value (11.22mg/KOH/g), pH value (4.62), refractive index (1.46), and specific gravity (0.9) respectively, it has a bland odour, a reddish brown colour and a mild taste. The values obtained for watermelon seed oil are saponification value (83.3mgKOH/g), free fatty acid (6.58mg/KOH/g), iodine value (122.6g/100), peroxide value (5.3meq/kg), acid value (3.74mgKOH/g), pH value (6.3), refractive index (1.47), and specific gravity (0.9) respectively, it has a nutty flavour, a golden yellow colour and a mild taste. From the result obtained, it shows that cottonseed oil has high acid value which shows the stability of the oil and its stability to rancidity. Consequently, watermelon seed oil is order wise.

Keywords: extraction, solvent, cotton seeds, watermelon seeds

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Authors: Kun Liang Ang, Eng Toon Saw, Wei He, Xuecheng Dong, Seeram Ramakrishna

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Ester solvents are widely used in pharmaceutical, printing and flavor industry due to their good miscibility, low toxicity, and high volatility. Through pervaporation, these ester solvents can be recovered from industrial wastewater. While metal-doped silicalite 1 zeolite membranes are commonly used in organic solvent recovery in the pervaporation process, these ceramic membranes suffer from low membrane permeation flux, mainly due to the high thickness of the metal-doped zeolite membrane. Herein, a simple method of fabricating an ultrathin tin-silicalite 1 membrane supported on alumina tube is reported. This ultrathin membrane is able to achieve high permeation flux and separation factor for an ester in a diluted aqueous solution. Nanosized tin-Silicalite 1 seeds which are smaller than 500nm has been formed through hydrothermal synthesis. The sn-Silicalite 1 seeds were then seeded onto alumina tube through dip coating, and the tin-Silicalite 1 membrane was then formed by hydrothermal synthesis in an autoclave through secondary growth method. Multiple membrane synthesis factors such as seed size, ceramic substrate surface pore size selection, and secondary growth conditions were studied for their effects on zeolite membrane growth. The microstructure, morphology and the membrane thickness of tin-Silicalite 1 zeolite membrane were examined. The membrane separation performance and stability will also be reported.

Keywords: ceramic membrane, pervaporation, solvent recovery, Sn-MFI zeolite

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Authors: Aarti Singh, Anees Ahmad

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Essential oil was extracted from lemon grass (Cymbopogon martini) with supercritical carbondioxide (SC-CO2) at pressure of 140 bar and temperature of 55 °C and CO2 flow rate of 8 gmin-1, and its composition and yield were compared with other conventional extraction methods of oil, HD (Hydrodistillation), SE (Solvent Extraction), UAE (Ultrasound Assisted Extraction). SC-CO2 extraction is a green and sustainable extraction technique. Each oil was analysed by GC-MS, the major constituents were neral (44%), Z-citral (43%), geranial (27%), caryophyllene (4.6%) and linalool (1%). The essential oil of lemon grass is valued for its neral and citral concentration. The oil obtained by supercritical carbon-dioxide extraction contained maximum concentration of neral (55.05%) whereas ultrasonication extracted oil contained minimum content (5.24%) and it was absent in solvent extracted oil. The antioxidant properties have been assessed by DPPH and superoxide scavenging methods.

Keywords: cymbopogon martini, essential oil, FT-IR, GC-MS, HPTLC, SC-CO2

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Authors: Dewi Selvia Fardhyanti, Astrilia Damayanti

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Coal tar is a liquid by-product of the process of coal gasification and carbonation, also in some industries such as steel, power plant, cement, and others. This liquid oil mixture contains various kinds of useful compounds such as aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. This research investigates thermodynamic modelling of liquid-liquid equilibria (LLE) in solvent extraction of o-Cresol from the coal tar. The equilibria are modeled by ternary components of Wohl, Van Laar, and Three-Suffix Margules models. The values of the parameters involved are obtained by curve-fitting to the experimental data. Based on the comparison between calculated and experimental data, it turns out that among the three models studied, the Three-Suffix Margules seems to be the best to predict the LLE of o-Cresol for those system.

Keywords: coal tar, o-Cresol, Wohl, Van Laar, three-suffix margules

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Authors: A. Zonouzi, M. Auli, M. Javanmard Dakheli, M. A. Hejazi

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Microalgae are tiny photosynthetic plants. Nowadays, microalgae are being used as nutrient-dense foods and sources of fine chemicals. They have significant amounts of lipid, carotenoids, vitamins, protein, minerals, chlorophyll, and pigments. Oil extraction from algae is a hotly debated topic currently because introducing an efficient method could decrease the process cost. This can determine the sustainability of algae-based foods. Scientific research works show that solvent extraction using chloroform/methanol (2:1) mixture is one of the efficient methods for oil extraction from algal cells, but both methanol and chloroform are toxic solvents, and therefore, the extracted oil will not be suitable for food application. In this paper, the effect of two food grade solvents (hexane and hexane/ isopropanol) on oil extraction yield from microalgae Dunaliella sp. was investigated and the results were compared with chloroform/methanol (2:1) extraction yield. It was observed that the oil extraction yield using hexane, hexane/isopropanol (3:2) and chloroform/methanol (2:1) mixture were 5.4, 13.93, and 17.5 (% w/w, dry basis), respectively. The fatty acid profile derived from GC illustrated that the palmitic (36.62%), oleic (18.62%), and stearic acids (19.08%) form the main portion of fatty acid composition of microalgae Dunalliela sp. oil. It was concluded that, the addition of isopropanol as polar solvent could increase the extraction yield significantly. Isopropanol solves cell wall phospholipids and enhances the release of intercellular lipids, which improves accessing of hexane to fatty acids.

Keywords: fatty acid profile‎, microalgae‎, oil extraction‎, polar solvent‎

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Authors: Tamer El-Messery, Teresa Sanchez-Moya, Ruben Lopez-Nicolas, Gaspar Ros, Esmat Aly

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Olive leaves (OLs), the main by-product of the olive oil industry, have a considerable amount of phenolic compounds. The exploitation of these compounds represents the current trend in food processing. In this study, OLs polyphenols were microencapsulated with polycaprolactone (PCL) and utilized in formulating novel functional yoghurt. PCL-microcapsules were characterized by scanning electron microscopy, and Fourier transform infrared spectrometry analysis. Their total phenolic (TPC), total flavonoid (TFC) contents, and antioxidant activities (DPPH, FRAP, ABTS), and polyphenols bioaccessibility were measured after oral, gastric, and intestinal steps of in vitro digestion. The four yoghurt formulations (containing 0, 25, 50, and 75 mg of PCL-microsphere/100g yoghurt) were evaluated for their pH, acidity, syneresis viscosity, and color during storage. In vitro digestion significantly affected the phenolic composition in non-encapsulated extract while had a lower impact on encapsulated phenolics. Higher protection was provided for encapsulated OLs extract, and their higher release was observed at the intestinal phase. Yoghurt with PCL-microsphere had lower viscosity, syneresis, and color parameters, as compared to control yoghurt. Thus, OLs represent a valuable and cheap source of polyphenols which can be successfully applied, in microencapsulated form, to formulate functional yoghurt.

Keywords: yoghurt quality attributes, olive leaves, phenolic and flavonoids compounds, antioxidant activity, polycaprolactone as microencapsulant

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Authors: Kanika Kalra, Harmeet Kaur, Dinesh Goyal

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Total phenolics were extracted from waste orange peels by solvent extraction and alkali hydrolysis method. The most efficient solvents for extracting phenolic compounds from waste biomass were methanol (60%) > dimethyl sulfoxide > ethanol (60%) > distilled water. The extraction yields were significantly impacted by solvents (ethanol, methanol, and dimethyl sulfoxide) due to varying polarity and concentrations. Extraction of phenolics using 60% methanol yielded the highest phenolics (in terms of gallic acid equivalent (GAE) per gram of biomass) in orange peels. Alkali hydrolyzed extract from orange peels contained 7.58±0.33 mg GAE g⁻¹. By using the solvent extraction technique, it was observed that 60% methanol is comparatively the best-suited solvent for extracting polyphenolic compounds and gave the maximum yield of 4.68 ± 0.47 mg GAE g⁻¹ in orange peel extracts. DPPH radical scavenging activity and reducing the power of orange peel extract were checked, where 60% methanolic extract showed the highest antioxidant activity, 85.50±0.009% for DPPH, and dimethyl sulfoxide (DMSO) extract gave the highest yield of 1.75±0.01% for reducing power ability of the orange peels extract. Characterization of the polyphenolic compounds was done by using Fourier transformation infrared (FTIR) spectroscopy. Solvent and alkali hydrolysed extracts were evaluated for antibacterial activity using the agar well diffusion method against Gram-positive Bacillus subtilis MTCC441 and Gram-negative Escherichia coli MTCC729. Methanolic extract at 300µl concentration showed an inhibition zone of around 16.33±0.47 mm against Bacillus subtilis, whereas, for Escherichia coli, it was comparatively less. Broth-based turbidimetric assay revealed the antibacterial effect of different volumes of orange peel extracts against both organisms.

Keywords: orange peels, total phenolic content, antioxidant, antibacterial

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Authors: Pratap K. Chhotaray, Jitendriya Swain, Ashok Mishra, Ramesh L. Gardas

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Ionic liquids (ILs) are molten salts, consist predominantly of ions and found to be liquid below 100°C. The unparalleled growing interest in ILs is based upon their never ending design flexibility. The use of ILs as a co-solvent in binary as well as a ternary mixture with molecular solvents multifold it’s utility. Since polarity is one of the most widely applied solvent concepts which represents simple and straightforward means for characterizing and ranking the solvent media, its study for a binary mixture of ILs is crucial for its widespread application and development. The primary approach to the assessment of solution phase intermolecular interactions, which generally occurs on the picosecond to nanosecond time scales, is to exploit the optical response of photophysical probe. Pyrene butyric acid (PBA) is used as fluorescence probe due to its high quantum yield, longer lifetime and high solvent polarity dependence of fluorescence spectra. Propylammonium formate (PAF) is the IL used for this study. Both the UV-absorbance spectra and steady state fluorescence intensity study of PBA in different concentration of aqueous PAF, reveals that with an increase in PAF concentration, both the absorbance and fluorescence intensity increases which indicate the progressive solubilisation of PBA. Whereas, near about 50% of IL concentration, all of the PBA molecules get solubilised as there are no changes in the absorbance and fluorescence intensity. Furthermore, the ratio II/IV, where the band II corresponds to the transition from S1 (ν = 0) to S0 (ν = 0), and the band IV corresponds to transition from S1 (ν = 0) to S0 (ν = 2) of PBA, indicates that the addition of water into PAF increases the polarity of the medium. Time domain lifetime study shows an increase in lifetime of PBA towards the higher concentration of PAF. It can be attributed to the decrease in non-radiative rate constant at higher PAF concentration as the viscosity is higher. The monoexponential decay suggests that homogeneity of solvation environment whereas the uneven width at full width at half maximum (FWHM) indicates there might exist some heterogeneity around the fluorophores even in the water-IL mixed solvents.

Keywords: fluorescence, ionic liquid, lifetime, polarity, pyrene butyric acid

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Authors: D. S. Fardhyanti, Megawati, W. B. Sediawan

Abstract:

Coal tar is a liquid by-product of the process of coal gasification and carbonation. This liquid oil mixture contains various kinds of useful compounds such as aromatic compounds and phenolic compounds. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. This research investigates thermodynamic modelling of liquid-liquid equilibria (LLE) in the separation of phenol from the coal tar by solvent extraction. The equilibria are modeled by ternary components of Wohl, Van Laar, and Three-Suffix Margules models. The values of the parameters involved are obtained by curve-fitting to the experimental data. Based on the comparison between calculated and experimental data, it turns out that among the three models studied, the Three-Suffix Margules seems to be the best to predict the LLE of p-Cresol mixtures for those system.

Keywords: coal tar, phenol, Wohl, Van Laar, Three-Suffix Margules

Procedia PDF Downloads 225

Authors: Hassiba Benguergoura, Kamal Chanane, Sâad Moulay

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Pervaporation (PV), a membrane-based separation technology, has gained much attention because of its energy saving capability and low-cost, especially for separation of azeotropic or close-boiling liquid mixtures. There are two crucial issues for industrial application of pervaporation process. The first is developing membrane material and tailoring membrane structure to obtain high pervaporation performances. The second is modeling pervaporation transport to better understand of the above-mentioned structure–pervaporation relationship. Many models were proposed to predict the mass transfer process, among them, solution-diffusion model is most widely used in describing pervaporation transport including preferential sorption, diffusion and evaporation steps. For modeling pervaporation transport, the permeation flux, which depends on the solubility and diffusivity of components in the membrane, should be obtained first. Traditionally, the solubility was calculated according to the Flory–Huggins theory. Separation of the benzene (Bz)/cyclohexane (Cx) mixture is industrially significant. Numerous papers have been focused on the Bz/Cx system to assess the PV properties of membrane materials. Membranes with both high permeability and selectivity are desirable for practical application. Several new polymers have been prepared to get both high permeability and selectivity. Styrene-butadiene rubbers (SBR), dense membranes cross-linked by chloromethylation were used in the separation of benzene/cyclohexane mixtures. The impact of chloromethylation reaction as a new method of cross-linking SBR on the pervaporation performance have been reported. In contrast to the vulcanization with sulfur, the cross-linking takes places on styrene units of polymeric chains via a methylene bridge. The partial pervaporative (PV) fluxes of benzene/cyclohexane mixtures in styrene-butadiene rubber (SBR) were predicted using Fick's first law. The predicted partial fluxes and the PV separation factor agreed well with the experimental data by integrating Fick's law over the benzene concentration. The effects of feed concentration and operating temperature on the predicted permeation flux by this proposed model are investigated. The predicted permeation fluxes are in good agreement with experimental data at lower benzene concentration in feed, but at higher benzene concentration, the model overestimated permeation flux. The predicted and experimental permeation fluxes all increase with operating temperature increasing. Solvent sorption levels for benzene/ cyclohexane mixtures in a SBR membrane were determined experimentally. The results showed that the solvent sorption levels were strongly affected by the feed composition. The Flory- Huggins equation generates higher R-square coefficient for the sorption selectivity.

Keywords: benzene, cyclohexane, pervaporation, permeation, sorption modeling, SBR

Procedia PDF Downloads 294

Authors: Senthil Rajan Dharmalingam, Shamala Nadaraju, Srinivasan Ramamurthy

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Doxorubicin is the most widely used anticancer drugs in chemotherapy treatment. However, problems related to the development of multidrug resistance (MDR) and acute cardiotoxicity have led researchers to investigate alternative forms of administering doxorubicin for cancer therapy. Several methods have been attempted to overcome MDR, including the co-administration of a chemosensitizer inhibiting the efflux caused by ATP binding cassette transporters with anticancer drugs, and the bypass of the efflux mechanism. Co encapsulation of doxorubicin (Dox) and cyclosporine A (CSA) into poly (DL-lactide-co-glycolide) nanoparticles was emulsification-solvent evaporation method using polyvinyl alcohol as emulsion stabilizers. The Dox-CSA loaded nanoparticles were evaluated for particle size, zeta potential and PDI by light scattering analysis and thermal characterizations by differential scanning calorimetry (DSC). Loading efficiency (LE %) and in-vitro dissolution samples were evaluated by developed and validated HPLC method. The optimum particle size obtained is 298.6.8±39.4 nm and polydispersity index (PDI) is 0.098±0.092. Zeta potential is found to be -29.9±4.23. Optimum pH to increase Dox LE% was found 7.1 which gave 42.5% and 58.9% increase of LE% for pH 6.6 and pH 8.6 compared respectively. LE% achieved for Dox is 0.07±0.01 % and CSA is 0.09±0.03%. Increased volume of PVA and weight of PLGA shows increase in size of nanoparticles. DSC thermograms showed shift in the melting peak for the nanoparticles compared to Dox and CSA indicating encapsulation of drugs. In conclusion, these preliminary studies showed the feasibility of PLGA nanoparticles to entrap Dox and CSA and require future in-vivo studies to be performed to establish its potential.

Keywords: doxorubicin, cyclosporine, PLGA, nanoparticles

Procedia PDF Downloads 433

Authors: Shradha S. Binani, P. S. Bodke, R. V. Joat

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Recent decades have witnessed an exponential growth in the field of acoustical parameters and ultrasound on solid, liquid and gases. Ultrasonic propagation parameters yield valuable information regarding the behavior of liquid systems because intra and intermolecular association, dipolar interaction, complex formation and related structural changes affecting the compressibility of the system which in turn produces variations in the ultrasonic velocity. The acoustic and thermo dynamical parameters obtained in ultrasonic study show that ion-solvation is accompanied by the destruction or enhancement of the solvent structure. In the present paper the ultrasonic velocity (v), density (ρ), viscosity(η) have been measured for the pharmacological important compound 2-hydroxy substituted phenyl pyrimidine derivative (2-hydroxy-4-(4’-methoxy phenyl)-6-(2’-hydroxy-4’-methyl-5’-chlorophenyl)pyrimidine) in ethanol as a solvent by using different concentration at constant room temperature. These experimental data have been used to estimate physical parameter like adiabatic compressibility, intermolecular free length, relaxation time, free volume, specific acoustic impedance, relative association, Wada’s constant, Rao’s constant etc. The above parameters provide information in understanding the structural and molecular interaction between solute-solvent in the drug solution with respect to change in concentration.

Keywords: acoustical parameters, ultrasonic velocity, density, viscosity, 2-hydroxy substituted phenyl pyrimidine derivative

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Authors: F. Adjel, S. Almi, D. Barkat

Abstract:

The synergistic solvent extraction of cobalt (II) from 0.33 mol dm-3 Na2SO4 aqueous solutions with capric acid (HL) in the absence and presence of tri-n-octylphosphine oxide (TOPO) in chloroform at 25°C, has been studied. The extracted species when the capric acid compound was used alone, is CoL2(HL)2. In the presence of TOPO, a remarkable enhancement on the extraction of nickel (II) with 0.02 mol dm-3 capric acid was observed upon the addition of 0.0025 to 0.01 mol dm-3 TOPO in chloroform. From an synergistic extraction- equilibrium study, the synergistic enhancement was ascribed to the adduct formation CoL2(HL)2 n(TOPO). The TOPO-HL interaction strongly influences the synergistic extraction efficiency. The synergistic extraction stoichiometry of cobalt (II) with capric acid and TOPO is studied with the methods of slope analysis. The equilibrium constants were determined.

Keywords: solvent extraction, cobalt (II), capric acid, TOPO, synergism

Procedia PDF Downloads 497