Search results for: Polar solvent.

Authors: Ekin Kıpçak, Yağmur Karakuş, Mesut Akgün

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Hydrogen is an important chemical in many industries and it is expected to become one of the major fuels for energy generation in the future. Unfortunately, hydrogen does not exist in its elemental form in nature and therefore has to be produced from hydrocarbons, hydrogen-containing compounds or water.

Above its critical point (374.8^oC and 22.1MPa), water has lower density and viscosity, and a higher heat capacity than those of ambient water. Mass transfer in supercritical water (SCW) is enhanced due to its increased diffusivity and transport ability. The reduced dielectric constant makes supercritical water a better solvent for organic compounds and gases. Hence, due to the aforementioned desirable properties, there is a growing interest toward studies regarding the gasification of organic matter containing biomass or model biomass solutions in supercritical water.

In this study, hydrogen and biofuel production by the catalytic gasification of 2-Propanol in supercritical conditions of water was investigated. Ru/Al₂O₃ was the catalyst used in the gasification reactions. All of the experiments were performed under a constant pressure of 25 MPa. The effects of five reaction temperatures (400, 450, 500, 550 and 600^oC) and five reaction times (10, 15, 20, 25 and 30 s) on the gasification yield and flammable component content were investigated.

Keywords: 2-Propanol, Gasification, Ru/Al2O3, Supercritical water.

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Authors: M. E. Abalaka, S. Y. Daniyan, S. O. Adeyemo, D. Damisa

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Gold nanoparticles (AuNPs) have gained increasing interest in recent times. This is greatly due to their special features, which include unusual optical and electronic properties, high stability and biological compatibility, controllable morphology and size dispersion, and easy surface functionalization. In typical synthesis, AuNPs were produced by reduction of gold salt AuCl4 in an appropriate solvent. A stabilizing agent was added to prevent the particles from aggregating. The antibacterial activity of different sizes of gold nanoparticles was investigated against Staphylococcus aureus, Salmonella typhi and Pseudomonas pneumonia using the disk diffusion method in a Müeller–Hinton Agar. The Au-NPs were effective against all bacteria tested. That the Au-NPs were successfully synthesized in suspension and were used to study the antibacterial activity of the two medicinal plants against some bacterial pathogens suggests that Au-NPs can be employed as an effective bacteria inhibitor and may be an effective tool in medical field. The study clearly showed that the Au-NPs exhibiting inhibition towards the tested pathogenic bacteria in vitro could have the same effects in vivo and thus may be useful in the medical field if well researched into.

Keywords: Gold Nanoparticles, Gomphrena celesioides, Prunus amygdalus, Pathogens.

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Authors: Eka Maulana, Sholeh Hadi Pramono, Dody Fanditya, M. Julius

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In this paper, extract of papaya leaves are used as a natural dye and combined by variations of solvent concentration applied on DSSC (Dye-Sensitized Solar Cell). Indonesian geographic located on the equator line occasions the magnitude of the potential to develop organic solar cells made from extracts of chlorophyll as a substitute for inorganic materials or synthetic dye on DSSC material. Dye serves as absorbing photons which are then converted into electrical energy. A conductive coated glass layer called TCO (Transparent Conductive Oxide) is used as a substrate of electrode. TiO2 nanoparticles as binding dye molecules, redox couple iodide/ tri-iodide as the electrolyte and carbon as the counter electrode in the DSSC are used. TiO2 nanoparticles, organic dyes, electrolytes, and counter electrode are arranged and combined with the layered structure of the photo-catalyst absorption layer. Dye absorption measurements using a spectrophotometer at 400-800 nm light spectrum produces a total amount of chlorophyll 80.076 mg/l. The test cell at 7 watt LED light with 5000 lux luminescence was obtained Voc and Isc of 235.5 mV and 14 μA, respectively.

Keywords: DSSC (Dye-Sensitized Solar Cell), natural dye, chlorophyll, absorption.

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Authors: Beena Sethi

Abstract:

This work involves the degradation of plastic waste in the presence of three different nanocatalysts. A thin film of LLDPE was formed with all three nanocatalysts separately in the solvent. Thermo Gravimetric Analysis (TGA) and Differential Scanning Calorimetric (DSC) analysis of polymers suggest that the presence of these catalysts lowers the degradation temperature and the change mechanism of degradation. Gas chromatographic analysis was carried out for two films. In gas chromatography (GC) analysis, it was found that degradation of pure polymer produces only 32% C3/C4 hydrocarbons and 67.6% C5/C9 hydrocarbons. In the presence of these catalysts, more than 80% of polymer by weight was converted into either liquid or gaseous hydrocarbons. Change in the mechanism of degradation of polymer was observed therefore more C3/C4 hydrocarbons along with valuable feedstock are produced. Adjustment of dose of nanocatalyst, use of nano-admixtures and recycling of catalyst can make this catalytic feedstock recycling method a good tool to get sustainable environment. The obtained products can be utilized as fuel or can be transformed into other useful products. In accordance with the principles of sustainable development, chemical recycling i.e. tertiary recycling of polymers along with the reuse (zero order recycling) of plastics can be the most appropriate and promising method in this direction. The tertiary recycling is attracting much attention from the viewpoint of the energy resource.

Keywords: Degradation, differential scanning calorimetry, feedstock recycling, gas chromatography, thermogravimetric analysis. DSC.

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Authors: Esther Lorrayne M. Pereira, Adriana Souza M. Batista, Fabíola A. S. Ribeiro, Adelina P. Santos, Clascídia A. Furtado, Luiz O. Faria

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The combination of multi–walled carbon nanotubes (MWCNTs) with polymers offers an attractive route to reinforce the macromolecular compounds as well as the introduction of new properties based on morphological modifications or electronic interactions between the two constituents. As they are only a few nanometers in dimension, it offers ultra-large interfacial area per volume between the nano-element and polymer matrix. Nevertheless, the use of MWCNTs as a rough material in different applications has been largely limited by their poor processability, insolubility, and infusibility. Studies concerning the nanofiller reinforced polymer composites are justified in an attempt to overcome these limitations. This work presents one preliminary study of MWCNTs dispersion into the PVDF homopolymer. For preparation, the composite components were diluted in n,n-dimethylacetamide (DMAc) with mechanical agitation assistance. After complete dilution, followed by slow evaporation of the solvent at 60°C, the samples were dried. Films of about 80 μm were obtained. FTIR and UV-Vis spectroscopic techniques were used to characterize the nanocomposites. The appearance of absorption bands in the FTIR spectra of nanofilled samples, when compared to the spectrum of pristine PVDF samples, are discussed and compared with the UV-Vis measurements.

Keywords: Composites materials, FTIR, MWNTs, PVDF, UVVis.

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Authors: Martin Klaumünzer, Jakob Hübner, Denis Spitzer

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Within this paper, latest results on processing of energetic nanomaterials by means of the Spray Flash Evaporation technique are presented. This technology constitutes a highly effective and continuous way to prepare fascinating materials on the nano- and micro-scale. Within the process, a solution is set under high pressure and sprayed into an evacuated atomization chamber. Subsequent ultrafast evaporation of the solvent leads to an aerosol stream, which is separated by cyclones or filters. No drying gas is required, so the present technique should not be confused with spray dying. Resulting nanothermites, insensitive explosives or propellants and compositions are foreseen to replace toxic (according to REACH) and very sensitive matter in military and civil applications. Diverse examples are given in detail: nano-RDX (n-Cyclotrimethylentrinitramin) and nano-aluminum based systems, mixtures (n-RDX/n-TNT - trinitrotoluene) or even cocrystalline matter like n-CL-20/HMX (Hexanitrohexaazaisowurtzitane/ Cyclotetra-methylentetranitramin). These nanomaterials show reduced sensitivity by trend without losing effectiveness and performance. An analytical study for material characterization was performed by using Atomic Force Microscopy, X-Ray Diffraction, and combined techniques as well as spectroscopic methods. As a matter of course, sensitivity tests regarding electrostatic discharge, impact, and friction are provided.

Keywords: Continuous synthesis, energetic material, nanoscale, nanothermite, nanoexplosive.

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Authors: Nuridayanti Che Khalib, Kaliyaperumal Thanigaimani, Suhana Arshad, Ibrahim Abdul Razak

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The 1:1 cocrystal of 2-amino-4-chloro-6- methylpyrimidine (2A4C6MP) with 4-methylbenzoic acid (4MBA) (I) has been prepared by slow evaporation method in methanol, which was crystallized in monoclinic C2/c space group, Z = 8, and a = 28.431 (2) Å, b = 7.3098 (5) Å, c = 14.2622 (10) Å and β = 109.618 (3)°. The presence of unionized –COOH functional group in cocrystal I was identified both by spectral methods (1H and 13C NMR, FTIR) and X-ray diffraction structural analysis. The 2A4C6MP molecule interact with the carboxylic group of the respective 4MBA molecule through N—H⋯O and O—H⋯N hydrogen bonds, forming a cyclic hydrogen–bonded motif R2 2(8). The crystal structure was stabilized by Npyrimidine—H⋯O=C and C=O—H⋯Npyrimidine types hydrogen bonding interactions. Theoretical investigations have been computed by HF and density function (B3LYP) method with 6–311+G (d,p)basis set. The vibrational frequencies together with 1H and 13C NMR chemical shifts have been calculated on the fully optimized geometry of cocrystal I. Theoretical calculations are in good agreement with the experimental results. Solvent–free formation of this cocrystal I is confirmed by powder X-ray diffraction analysis.

Keywords: Supramolecular Cocrystal, 2-amino-4-chloro-6- methylpyrimidine, Hartree-Fock and DFT Studies, Spectroscopic Analysis.

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Authors: P. Rahnemoon, M. Sarabi Jamab, M. Javanmard Dakheli, A. Bostan

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In recent years, tendency to use of natural antimicrobial agents in food industry has increased. Pomegranate peels containing phenolic compounds and anti-microbial agents, are counted as valuable source for extraction of these compounds. In this study, the extraction of pomegranate peel extract was carried out at different ethanol/water ratios (40:60, 60:40, and 80:20), temperatures (25, 40, and 55 ˚C), and time durations (20, 24, and 28 h). The extraction yield, phenolic compounds, flavonoids, and anthocyanins were measured. ‎Antimicrobial activity of pomegranate peel extracts were determined against some food-borne ‎microorganisms such as Salmonella enteritidis, Escherichia coli, Listeria monocytogenes, ‎‎Staphylococcus aureus, Aspergillus niger, and Saccharomyces cerevisiae by agar diffusion and MIC methods. Results showed that at ethanol/water ratio 60:40, 25 ˚C and 24 h maximum amount of phenolic compounds ‎‏(‎‏‎349.518‎‏ ‏mg gallic acid‏/‏g dried extract), ‎flavonoids (250.124 mg rutin‏/‏g dried extract), anthocyanins (252.047 ‎‏‏mg ‎cyanidin‏‎3‎‏glucoside‏/‏‎100 g dried extract), and the strongest antimicrobial activity were obtained. ‎All extracts’ antimicrobial activities were demonstrated against every tested ‎‎microorganisms‏.‎‏ Staphylococcus aureus showed the highest sensitivity among the tested ‎‎‎microorganisms.

Keywords: Antimicrobial agents, phenolic compounds, pomegranate peel, solvent extraction.

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Authors: N. Outili, A-H. Meniai

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Modeling transfer phenomena in several chemical engineering operations leads to the resolution of partial differential equations systems. According to the complexity of the operations mechanisms, the equations present a nonlinear form and analytical solution became difficult, we have then to use numerical methods which are based on approximations in order to transform a differential system to an algebraic one.Finite element method is one of numerical methods which can be used to obtain an accurate solution in many complex cases of chemical engineering.The packed columns find a large application like contactor for liquid-liquid systems such solvent extraction. In the literature, the modeling of this type of equipment received less attention in comparison with the plate columns.A mathematical bidimensionnal model with radial and axial dispersion, simulating packed tower extraction behavior was developed and a partial differential equation was solved using the finite element method by adopting the Galerkine model. We developed a Mathcad program, which can be used for a similar equations and concentration profiles are obtained along the column. The influence of radial dispersion was prooved and it can-t be neglected, the results were compared with experimental concentration at the top of the column in the extraction system: acetone/toluene/water.

Keywords: finite element method, Galerkine method, liquidliquid extraction modelling, packed column simulation, two dimensional model

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Authors: Maíra O. Palm, Cintia Marangoni, Ozair Souza, Noeli Sellin

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Wastes from a vegetal extracts industry (cocoa, oak, Guarana and mate) were characterized by particle size, proximate and ultimate analysis, lignocellulosic fractions, high heating value, thermal analysis (Thermogravimetric analysis – TGA, and Differential thermal analysis - DTA) and energy density to evaluate their potential as biomass in the form of briquettes for power generation. All wastes presented adequate particle sizes to briquettes production. The wastes showed high moisture content, requiring previous drying for use as briquettes. Cocoa and oak wastes had the highest volatile matter contents with maximum mass loss at 310 ºC and 450 ºC, respectively. The solvents used in the aroma extraction process influenced in the moisture content of the wastes, which was higher for mate due to water has been used as solvent. All wastes showed an insignificant loss mass after 565 °C, hence resulting in low ash content. High carbon and hydrogen contents and low sulfur and nitrogen contents were observed ensuring a low generation of sulfur and nitrous oxides. Mate and cocoa exhibited the highest carbon and lignin content, and high heating value. The dried wastes had high heating value, from 17.1 MJ/kg to 20.8 MJ/kg. The results indicate the energy potential of wastes for use as fuel in power generation.

Keywords: Agro-industrial waste, biomass, briquettes, combustion.

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Authors: Sarun Keithmaleesatti, Pakorn Varanusupakul, Wattasit Siriwong, Kumthorn Thirakhupt, Mark Robson, Noppadon Kitana

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Organochlorine pesticides (OCPs) are known to be persistent and bioaccumulative toxicants that may cause reproductive impairments in wildlife as well as human. The current study uses the snail-eating turtle Malayemys macrocephala, a long-lived animal commonly distribute in rice field habitat in central part of Thailand, as a sentinel to monitor OCP contamination in environment. The nest soil, complete clutch of eggs, and blood of the turtle were collected from agricultural areas in the Chao Phraya River Basin, Thailand during the nesting season of 2007-2008. The novel methods for tissue extraction by an accelerated solvent extractor (ASE, for egg) and liquid-liquid extraction (for blood) have been developed. The nineteen OCP residues were analyzed by gas chromatography with micro-electron captured detector (GC-μECD). The validated methods have met requirements of the AOAC standard. The results indicated that significant amounts of OCPs are still contaminated in nest soil and eggs of the turtle even though the OCPs had been banned in this area for many years. This suggested the potential risk to health of wildlife as well as human in the area.

Keywords: Gas chromatography, persistent organic pollutants, rice field, sentinel species.

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Authors: Edison Muzenda

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The aim of this study was to compare the solubility of selected volatile organic compounds in water and silicon oil using the simple static headspace method. The experimental design allowed equilibrium achievement within 30 – 60 minutes. Infinite dilution activity coefficients and Henry-s law constants for various organics representing esters, ketones, alkanes, aromatics, cycloalkanes and amines were measured at 303K. The measurements were reproducible with a relative standard deviation and coefficient of variation of 1.3x10-3 and 1.3 respectively. The static determined activity coefficients using shaker flasks were reasonably comparable to those obtained using the gas liquid - chromatographic technique and those predicted using the group contribution methods mainly the UNIFAC. Silicon oil chemically known as polydimethysiloxane was found to be better absorbent for VOCs than water which quickly becomes saturated. For example the infinite dilution mole fraction based activity coefficients of hexane is 0.503 and 277 000 in silicon oil and water respectively. Thus silicon oil gives a superior factor of 550 696. Henry-s law constants and activity coefficients at infinite dilution play a significant role in the design of scrubbers for abatement of volatile organic compounds from contaminated air streams. This paper presents the phase equilibrium of volatile organic compounds in very dilute aqueous and polymeric solutions indicating the movement and fate of chemical in air and solvent. The successful comparison of the results obtained here and those obtained using other methods by the same authors and in literature, means that the results obtained here are reliable.

Keywords: Abatement, absorbent, activity coefficients, equilibrium, Henry's law constant.

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Authors: Wai Keng Teng, Gek Cheng Ngoh, Rozita Yusoff, Mohamed Kheireddine Aroua, Joe Shen Heng

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As a by-product of the biodiesel industries, glycerol has been vastly generated which surpasses the market demand. It is imperative to develop an efficient glycerol valorization processes in minimizing the net energy requirement and intensifying the biodiesel production. In this study, base-catalyzed transesterification of glycerol with dimethyl carbonate using microwave irradiation as heating method to produce glycerol carbonate was conducted by varying grades of glycerol, i.e. 70%, 86% and 99% purity, that is obtained from biodiesel plant. Metal oxide catalysts were used with varying operating parameters including reaction time, DMC/glycerol molar ratio, catalyst weight %, temperature and stirring speed. From the study on the effect of different operating parameters it was found that the type of catalyst used has the most significant effect on the transesterification reaction. Amidst the metal oxide catalysts examined, CaO gave the best performance. This study indicates the feasibility of producing glycerol carbonate using different grade of glycerol in both conventional thermal activation and microwave irradiation with CaO as catalyst. Microwave assisted transesterification (MAT) of glycerol into glycerol carbonate has demonstrated itself as an energy efficient route by achieving 94.2% yield of GC at 65°C, 5 minutes reaction time, 1 wt% CaO and DMC/glycerol molar ratio of 2. The advantages of MAT transesterification route has made the direct utilization of bioglycerol from biodiesel production without the need of purification. This has marked a more economical and less-energy intensive glycerol carbonate synthesis route.

Keywords: Biodiesel, glycerol, glycerol carbonate, microwave irradiation.

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Authors: Ghulam Murshid

Abstract:

Carbon dioxide is one of the major greenhouse gas (GHG) contributors. It is an obligation of the industry to reduce the amount of carbon dioxide emission to the acceptable limits. Tremendous research and studies are reported in the past and still the quest to find the suitable and economical solution of this problem needed to be explored in order to develop the most plausible absorber for carbon dioxide removal. Amino acids can be potential alternate solvents for carbon dioxide capture from gaseous streams. This is due to its ability to resist oxidative degradation, low volatility and its ionic structure. In addition, the introduction of promoter-like piperazine to amino acid helps to further enhance the solubility. In this work, the effect of piperazine on thermo physical properties and solubility of β-Alanine aqueous solutions were studied for various concentrations. The measured physicochemical properties data was correlated as a function of temperature using least-squares method and the correlation parameters are reported together with it respective standard deviations. The effect of activator piperazine on the CO2 loading performance of selected amino acid under high-pressure conditions (1bar to 10bar) at temperature range of (30 to 60)oC was also studied. Solubility of CO2 decreases with increasing temperature and increases with increasing pressure. Quadratic representation of solubility using Response Surface Methodology (RSM) shows that the most important parameter to optimize solubility is system pressure. The addition of promoter increases the solubility effect of the solvent.

Keywords: Amino acids, CO2, Global warming, Solubility.

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Authors: T. C. Machaba, S. M. Mahlo

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The current study investigates the antifungal properties of crude plant extracts from selected medicinal plant species. Eight plant species used by the traditional healers and local people to treat fungal infections were selected for further phytochemical analysis and biological assay. The selected plant species were extracted with solvent of various polarities such as acetone, methanol, ethanol, hexane, dichloromethane, ethyl acetate and water. Leaf, roots and bark extracts of Maerua juncea Pax, Albuca seineri (Engl & K. Krause) J.C Manning & Goldblatt, Senna italica Mill., Elephantorrhiza elephantina (Burch.) Skeels, Indigofera circinata Benth., Schinus molle L., Asparagus buchananii Bak., were screened for antifungal activity against three animal fungal pathogens (Candida albicans, Aspergillus fumigatus and Cryptococcus neoformans). All plant extracts were active against the tested microorganisms. Acetone, dichloromethane, hexane and ethanol extracts of Senna italica and Elephantorrhiza elephantine had excellent activity against Candida albicans and A. fumigatus with the lowest MIC value of 0.02 mg/ml. Bioautography assay was used to determine the number of antifungal compounds presence in the plant extracts. No active compounds were observed in plant extracts of Indigofera circinnata, Schinus molle and Pentarrhinum insipidum with good antifungal activity against C. albicans and A. fumigatus indicating possible synergism between separated metabolites.

Keywords: Antifungal activity, minimum inhibitory concentration, bioautography.

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Authors: R. Ibrahim, M. Azmirruddin, M. Jabir, N. Johari, M. Muhamad, A. R. A. Talib

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Inconel718 has been widely used as a super alloy in aerospace application due to the high strength at elevated temperatures, satisfactory oxidation resistance and heat corrosion resistance. In this study, the Inconel718 has been fabricated using high technology of Metal Injection Molding (MIM) process due to the cost effective technique for producing small, complex and precision parts in high volume compared with conventional method through machining. Through MIM, the binder system is one of the most important criteria in order to successfully fabricate the Inconel718. Even though, the binder system is a temporary, but failure in the selection and removal of the binder system will affect on the final properties of the sintered parts. Therefore, the binder system based on palm oil derivative which is palm stearin has been formulated and developed to replace the conventional binder system. The rheological studies of the mixture between the powder and binders system have been determined properly in order to be successful during injection into injection molding machine. After molding, the binder holds the particles in place. The binder system has to be removed completely through debinding step. During debinding step, solvent debinding and thermal pyrolysis has been used to remove completely of the binder system. The debound part is then sintered to give the required physical and mechanical properties. The results show that the properties of the final sintered parts fulfill the Standard Metal Powder Industries Federation (MPIF) 35 for MIM parts.

Keywords: Binder system, rheological study, metal injection molding, debinding and sintered parts.

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Authors: Is Fatimah, Winda Novita, Yopi Andika, Imam Sahroni, Basitoh Djaelani, Yuyun Yunani N.

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Contamination of aromatic compounds in water can cause severe long-lasting effects not only for biotic organism but also on human health. Several alternative technologies for remediation of polluted water have been attempted. One of these is adsorption process of aromatic compounds by using organic modified clay mineral. Porous structure of clay is potential properties for molecular adsorptivity and it can be increased by immobilizing hydrophobic structure to attract organic compounds. In this work natural montmorillonite were modified with cetyltrimethylammonium (CTMA+) and was evaluated for use as adsorbents of aromatic compounds: benzene, toluene, and 2-chloro phenol in its single and multicomponent solution by ethanol:water solvent. Preparation of CTMA-montmorillonite was conducted by simple ion exchange procedure and characterization was conducted by using x-day diffraction (XRD), Fourier-transform infra red (FTIR) and gas sorption analysis. The influence of structural modification of montmorillonite on its adsorption capacity and adsorption affinity of organic compound were studied. It was shown that adsorptivity of montmorillonite was increased by modification associated with arrangements of CTMA+ in the structure even the specific surface area of modified montmorillonite was lower than raw montmorillonite. Adsorption rate indicated that material has affinity to adsorb compound by following order: benzene> toluene > 2-chloro phenol. The adsorption isotherms of benzene and toluene showed 1st order adsorption kinetic indicating a partition phenomenon of compounds between the aqueous and organophilic CTMAmontmorillonite.

Keywords: Adsorption, Desorption, Montmorillonite, Organoclay, Surfactant.

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Authors: S. Demiray, M. E. Pintado, P. M. L. Castro

Abstract:

There is a growing interest in the food industry and in preventive health care for the development and evaluation of natural antioxidants from medicinal plant materials. In the present work, extracts of three medicinal plants (Tilia argentea, Crataegi folium leaves and Polygonum bistorta roots) used in Turkish phytotheraphy were screened for their phenolic profiles and antioxidant properties. Crude extracts were obtained from different parts of plants, by solidliquid extraction with pure water, 70% acetone and 70% methanol aqueous solvents. The antioxidant activity of the extracts was determined by ABTS.+ radical cation scavenging activity. The Folin Ciocalteu procedure was used to assess the total phenolic concentrations of the extracts as gallic acid equivalents. A modified liquid chromatography-electro spray ionization-mass spectrometry (LC-ESI-MS) was used to obtain chromatographic profiles of the phenolic compounds in the medicinal plants. The predominant phenolic compounds detected in different extracts of the plants were catechin, protocatechuic and chlorogenic acids. The highest phenolic contents were obtained by using 70% acetone as aqueous solvent, whereas the lowest phenolic contents were obtained by water extraction due to Folin Ciocalteu results. The results indicate that acetone extracts of Tilia argentea had the highest antioxidant capacity as free ABTS radical scavengers. The lowest phenolic contents and antioxidant capacities were obtained from Polygonum bistorta root extracts.

Keywords: Medicinal plants, antioxidant activity, totalphenolics, LC-ESI-MS.

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Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

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The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe₃O₄/Al₂O₃ NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe₃O₄/Al₂O₃ NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL⁻¹, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL^-1 Fe²⁺ was 2.3%.

Keywords: Alumina-coated magnetite nanoparticles, magnetic mixed hemimicell solid-phase extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample.

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Authors: Maliheh Raji, Hossein Abolghasemi, Jaber Safdari, Ali Kargari

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Dysprosium is a rare earth element which is essential for many growing high-technology applications. Dysprosium along with neodymium plays a significant role in different applications such as metal halide lamps, permanent magnets, and nuclear reactor control rods preparation. The purification and separation of rare earth elements are challenging because of their similar chemical and physical properties. Among the various methods, membrane processes provide many advantages over the conventional separation processes such as ion exchange and solvent extraction. In this work, selective extraction and separation of dysprosium from aqueous solutions containing an equimolar mixture of dysprosium and neodymium by emulsion liquid membrane (ELM) was investigated. The organic membrane phase of the ELM was a nanofluid consisting of multiwalled carbon nanotubes (MWCNT), Span80 as surfactant, Cyanex 272 as carrier, kerosene as base fluid, and nitric acid solution as internal aqueous phase. Factors affecting separation of dysprosium such as carrier concentration, MWCNT concentration, feed phase pH and stripping phase concentration were analyzed using Taguchi method. Optimal experimental condition was obtained using analysis of variance (ANOVA) after 10 min extraction. Based on the results, using MWCNT nanofluid in ELM process leads to increase the extraction due to higher stability of membrane and mass transfer enhancement and separation factor of 6 for dysprosium over neodymium can be achieved under the optimum conditions. Additionally, demulsification process was successfully performed and the membrane phase reused effectively in the optimum condition.

Keywords: Emulsion liquid membrane, MWCNT nanofluid, separation, Taguchi Method.

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Authors: Marinos Xagoraris, Iliada K. Lappa, Charalambos Kanakis, Dimitra Daferera, Christina Papadopoulou, Georgios Sourounis, Charilaos Giotis, Pavlos Bouchagier, Christos S. Pappas, Petros A. Tarantilis, Efstathia Skotti

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The aim of this work was to recover phenolic compounds from grape skins produced in Greek varieties of the Ionian Islands in order to form the basis of calculations for their further utilization in the context of the circular economy. Isolation and further utilization of phenolic compounds is an important issue in winery by-products. For this purpose, 37 samples were collected, extracted, and analyzed in an attempt to provide the appropriate basis for their sustainable exploitation. Extraction of the bioactive compounds was held using an eco-friendly, non-toxic, and highly effective water-glycerol solvent system. Then, extracts were analyzed using UV-Vis, liquid chromatography-mass spectrometry (LC-MS), FTIR, and Raman spectroscopy. Also, total phenolic content and antioxidant activity were measured. LC-MS chromatography showed qualitative differences between different varieties. Peaks were attributed to monomeric 3-flavanols as well as monomeric, dimeric, and trimeric proanthocyanidins. The FT-IR and Raman spectra agreed with the chromatographic data and contributed to identifying phenolic compounds. Grape skins exhibited high total phenolic content (TPC), and it was proved that during vinification, a large number of polyphenols remained in the pomace. This study confirmed that grape skins from Ionian Islands are a promising source of bioactive compounds, suggesting their utilization under a bio-economic and environmental strategic framework.

Keywords: Antioxidant activity, grape skin, phenolic compounds, waste recovery.

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Authors: Syarifah Abd Rahim, Fatinah Ab Rahman, Engku N. E. M. Nasir, Noor A. Ramle

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Co-crystal is believed to improve the solubility and dissolution rates and thus, enhanced the bioavailability of poor water soluble drugs particularly during the oral route of administration. With the existing of poorly soluble drugs in pharmaceutical industry, the screening of co-crystal formation using carbamazepine (CBZ) as a model drug compound with dicarboxylic acids co-crystal formers (CCF) namely fumaric (FA) and succinic (SA) acids in ethanol has been studied. The co-crystal formations were studied by varying the mol ratio values of CCF to CBZ to access the effect of CCF concentration on the formation of the co-crystal. Solvent evaporation, slurry and cooling crystallization which representing the solution based method co-crystal screening were used. Based on the differential scanning calorimetry (DSC) analysis, the melting point of CBZ-SA in different ratio was in the range between 188oC-189oC. For CBZ-FA form A and CBZ-FA form B the melting point in different ratio were in the range of 174oC-175oC and 185oC-186oC respectively. The product crystal from the screening was also characterized using X-ray powder diffraction (XRPD). The XRPD pattern profile analysis has shown that the CBZ co-crystals with FA and SA were successfully formed for all ratios studied. The findings revealed that CBZ-FA co-crystal were formed in two different polymorphs. It was found that CBZ-FA form A and form B were formed from evaporation and slurry crystallization methods respectively. On the other hand, in cooling crystallization method, CBZ-FA form A was formed at lower mol ratio of CCF to CBZ and vice versa. This study disclosed that different methods and mol ratios during the co-crystal screening can affect the outcome of co-crystal produced such as polymorphic forms of co-crystal and thereof. Thus, it was suggested that careful attentions is needed during the screening since the co-crystal formation is currently one of the promising approach to be considered in research and development for pharmaceutical industry to improve the poorly soluble drugs.

Keywords: Carbamazepine, co-crystal, co-crystal former, dicarboxylic acid.

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Authors: Pascal Mwenge, Tumisang Seodigeng

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The combination of world population and the third industrial revolution led to high demand for fuels. On the other hand, the decrease of global fossil 8fuels deposits and the environmental air pollution caused by these fuels has compounded the challenges the world faces due to its need for energy. Therefore, new forms of environmentally friendly and renewable fuels such as biodiesel are needed. The primary analytical techniques for methanolysis yield monitoring have been chromatography and spectroscopy, these methods have been proven reliable but are more demanding, costly and do not provide real-time monitoring. In this work, the in situ monitoring of biodiesel from sunflower oil using FTIR (Fourier Transform Infrared) has been studied; the study was performed using EasyMax Mettler Toledo reactor equipped with a DiComp (Diamond) probe. The quantitative monitoring of methanolysis was performed by building a quantitative model with multivariate calibration using iC Quant module from iC IR 7.0 software. 15 samples of known concentrations were used for the modelling which were taken in duplicate for model calibration and cross-validation, data were pre-processed using mean centering and variance scale, spectrum math square root and solvent subtraction. These pre-processing methods improved the performance indexes from 7.98 to 0.0096, 11.2 to 3.41, 6.32 to 2.72, 0.9416 to 0.9999, RMSEC, RMSECV, RMSEP and R2Cum, respectively. The R² value of 1 (training), 0.9918 (test), 0.9946 (cross-validation) indicated the fitness of the model built. The model was tested against univariate model; small discrepancies were observed at low concentration due to unmodelled intermediates but were quite close at concentrations above 18%. The software eliminated the complexity of the Partial Least Square (PLS) chemometrics. It was concluded that the model obtained could be used to monitor methanol of sunflower oil at industrial and lab scale.

Keywords: Biodiesel, calibration, chemometrics, FTIR, methanolysis, multivariate analysis, transesterification.

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Authors: R. D. Kulkarni, Mayur Chaudhari, S. Mishra

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Curing of paints by exposure to UV radiations is emerging as one of the best film forming technique as an alternative to traditional solvent borne oxidative and thermal curing coatings. The composition and chemistry of UV curable coatings and role of multifunctional and monofunctional monomers, oligomers, and photoinitiators have been discussed. The limitations imposed by thermodynamic equilibrium and tendency for acrylic double bond polymerizations during synthesis of multifunctional acrylates have been presented. Aim of present investigation was thus to explore the reaction variables associated with synthesis of multifunctional acrylates. Zirconium oxychloride was evaluated as catalyst against regular acid functional catalyst. The catalyzed synthesis of glyceryl acrylate and neopentyl glycol acrylate was conducted by variation of following reaction parameters: two different reactant molar ratios- 1:4 and 1:6; catalyst usage in % by moles on polyol- 2.5, 5.0 and 7.5 and two different reaction temperatures- 45 and 75 0C. The reaction was monitored by determination of acid value and hydroxy value at regular intervals, besides TLC, HPLC, and FTIR analysis of intermediates and products. On the basis of determination of reaction progress over 1-60 hrs, the esterification reaction was observed to follow 2nd order kinetics with rate constant varying from 1*10-4 to 7*10-4. The thermal and catalytic components of second order rate constant and energy of activation were also determined. Uses of these kinetic and thermodynamic parameters in design of reactor for manufacture of multifunctional acrylate ester have been presented. The synthesized multifunctional acrylates were used to formulate and apply UV curable clear coat followed by determination of curing characteristics and mechanical properties of cured film. The overall curing rates less than 05 min. were easily attained indicating economical viability of radiation curable system due to faster production schedules

Keywords: glyceryl acrylate, neopentyl glycol acrylate, kinetic modeling, zirconium oxychloride.

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Authors: Md. Z. Alam, Amal A. Elgharbawy, Muhammad Moniruzzaman, Nassereldeen A. Kabbashi, Parveen Jamal

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The enzymatic hydrolysis of lignocellulosic biomass is one of the obstacles in the process of sugar production, due to the presence of lignin that protects the cellulose molecules against cellulases. Although the pretreatment of lignocellulose in ionic liquid (IL) system has been receiving a lot of interest; however, it requires IL removal with an anti-solvent in order to proceed with the enzymatic hydrolysis. At this point, introducing a compatible cellulase enzyme seems more efficient in this process. A cellulase enzyme that was produced by Trichoderma reesei on palm kernel cake (PKC) exhibited a promising stability in several ILs. The enzyme called PKC-Cel was tested for its optimum pH and temperature as well as its molecular weight. One among evaluated ILs, 1,3-diethylimidazolium dimethyl phosphate [DEMIM] DMP was applied in this study. Evaluation of six factors was executed in Stat-Ease Design Expert V.9, definitive screening design, which are IL/ buffer ratio, temperature, hydrolysis retention time, biomass loading, cellulase loading and empty fruit bunches (EFB) particle size. According to the obtained data, IL-enzyme system shows the highest sugar concentration at 70 °C, 27 hours, 10% IL-buffer, 35% biomass loading, 60 Units/g cellulase and 200 μm particle size. As concluded from the obtained data, not only the PKC-Cel was stable in the presence of the IL, also it was actually stable at a higher temperature than its optimum one. The reducing sugar obtained was 53.468±4.58 g/L which was equivalent to 0.3055 g reducing sugar/g EFB. This approach opens an insight for more studies in order to understand the actual effect of ILs on cellulases and their interactions in the aqueous system. It could also benefit in an efficient production of bioethanol from lignocellulosic biomass.

Keywords: Cellulase, hydrolysis, lignocellulose, pretreatment, stability.

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Authors: J. R. Büttler, T. Pham

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Basic understanding of interfacial mechanisms is of importance for the development of polymer composites. For this purpose, we need techniques to analyze the quality of interphases, their chemical and physical interactions and their strength and fracture resistance. In order to investigate the interfacial phenomena in detail, advanced characterization techniques are favorable. Dynamic mechanical thermal analysis (DMTA) using a rheological system is a sensitive tool. T-peel tests were performed with this system, to investigate the temperature-dependent peel behavior of woven textile composites. A model system was made of polyamide (PA) woven fabric laminated with films of polypropylene (PP) or PP modified by grafting with maleic anhydride (PP-g-MAH). Firstly, control measurements were performed with solely PP matrixes. Polymer melt investigations, as well as the extensional stress, extensional viscosity and extensional relaxation modulus at -10°C, 100 °C and 170 °C, demonstrate similar viscoelastic behavior for films made of PP-g-MAH and its non-modified PP-control. Frequency sweeps have shown that PP-g-MAH has a zero phase viscosity of around 1600 Pa·s and PP-control has a similar zero phase viscosity of 1345 Pa·s. Also, the gelation points are similar at 2.42*104 Pa (118 rad/s) and 2.81*104 Pa (161 rad/s) for PP-control and PP-g-MAH, respectively. Secondly, the textile composite was analyzed. The extensional stress of PA66 fabric laminated with either PP-control or PP-g-MAH at -10 °C, 25 °C and 170 °C for strain rates of 0.001 – 1 s^-1 was investigated. The laminates containing the modified PP need more stress for T-peeling. However, the strengthening effect due to the modification decreases by increasing temperature and at 170 °C, just above the melting temperature of the matrix, the difference disappears. Independent of the matrix used in the textile composite, there is a decrease of extensional stress by increasing temperature. It appears that the more viscous is the matrix, the weaker the laminar adhesion. Possibly, the measurement is influenced by the fact that the laminate becomes stiffer at lower temperatures. Adhesive lap-shear testing at room temperature supports the findings obtained with the T-peel test. Additional analysis of the textile composite at the microscopic level ensures that the fibers are well embedded in the matrix. Atomic force microscopy (AFM) imaging of a cross section of the composite shows no gaps between the fibers and matrix. Measurements of the water contact angle show that the MAH grafted PP is more polar than the virgin-PP, and that suggests a more favorable chemical interaction of PP-g-MAH with PA, compared to the non-modified PP. In fact, this study indicates that T-peel testing by DMTA is a technique to achieve more insights into polymeric textile composites.

Keywords: Dynamic mechanical thermal analysis, interphase, polyamide, polypropylene, textile composite, T-peel test.

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Authors: Abubakar Rashid, Muhammad Saad, Faheem Ahmed

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This paper provides a comprehensive study pertaining to diagnosis of intermittent high vibrations on an industrial gas turbine using detailed vibrations analysis, followed by its rectification. Engro Polymer & Chemicals Limited, a Chlor-Vinyl complex located in Pakistan has a captive combined cycle power plant having two 28 MW gas turbines (make Hitachi) & one 15 MW steam turbine. In 2018, the organization faced an issue of high vibrations on one of the gas turbines. These high vibration peaks appeared intermittently on both compressor’s drive end (DE) & turbine’s non-drive end (NDE) bearing. The amplitude of high vibration peaks was between 150-170% on the DE bearing & 200-300% on the NDE bearing from baseline values. In one of these episodes, the gas turbine got tripped on “High Vibrations Trip” logic actuated at 155µm. Limited instrumentation is available on the machine, which is monitored with GE Bently Nevada 3300 system having two proximity probes installed at Turbine NDE, Compressor DE &at Generator DE & NDE bearings. Machine’s transient ramp-up & steady state data was collected using ADRE SXP & DSPI 408. Since only 01 key phasor is installed at Turbine high speed shaft, a derived drive key phasor was configured in ADRE to obtain low speed shaft rpm required for data analysis. By analyzing the Bode plots, Shaft center line plot, Polar plot & orbit plots; rubbing was evident on Turbine’s NDE along with increased bearing clearance of Turbine’s NDE radial bearing. The subject bearing was then inspected & heavy deposition of carbonized coke was found on the labyrinth seals of bearing housing with clear rubbing marks on shaft & housing covering at 20-25 degrees on the inner radius of labyrinth seals. The collected coke sample was tested in laboratory & found to be the residue of lube oil in the bearing housing. After detailed inspection & cleaning of shaft journal area & bearing housing, new radial bearing was installed. Before assembling the bearing housing, cleaning of bearing cooling & sealing air lines was also carried out as inadequate flow of cooling & sealing air can accelerate coke formation in bearing housing. The machine was then taken back online & data was collected again using ADRE SXP & DSPI 408 for health analysis. The vibrations were found in acceptable zone as per ISO standard 7919-3 while all other parameters were also within vendor defined range. As a learning from subject case, revised operating & maintenance regime has also been proposed to enhance machine’s reliability.

Keywords: ADRE, bearing, gas turbine, GE Bently Nevada, Hitachi, vibration.

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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In this paper, a simple chemical precipitation route for the preparation of titanium dioxide nanoparticles, synthesized by using titanium tetra isopropoxide as a precursor and polyvinyl pyrrolidone (PVP) as a capping agent, is reported. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) of the samples were recorded and the phase transformation temperature of titanium hydroxide, Ti(OH)₄ to titanium oxide, TiO₂ was investigated. The as-prepared Ti(OH)₄ precipitate was annealed at 800°C to obtain TiO₂ nanoparticles. The thermal, structural, morphological and textural characterizations of the TiO₂ nanoparticle samples were carried out by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM) techniques. The as-prepared precipitate was characterized using DSC-TGA and confirmed the mass loss of around 30%. XRD results exhibited no diffraction peaks attributable to anatase phase, for the reaction products, after the solvent removal. The results indicate that the product is purely rutile. The vibrational frequencies of two main absorption bands of prepared samples are discussed from the results of the FTIR analysis. The formation of nanosphere of diameter of the order of 10 nm, has been confirmed by FESEM. The optical band gap was found by using UV-Visible spectrum. From photoluminescence spectra, a strong emission was observed. The obtained results suggest that this method provides a simple, efficient and versatile technique for preparing TiO₂ nanoparticles and it has the potential to be applied to other systems for photocatalytic activity.

Keywords: TiO2 nanoparticles, chemical precipitation route, phase transition, Fourier Transform Infra-Red spectroscopy, micro Raman spectroscopy, UV-Visible absorption spectroscopy, Photoluminescence spectroscopy, Field Effect Scanning Electron Microscopy.

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Authors: Mário Silva, Filipa Gomes, Filipa Oliveira, Simone Morais, Cristina Delerue-Matos

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Brown seaweeds are abundant in Portuguese coastline and represent an almost unexploited marine economic resource. One of the most common species, easily available for harvesting in the northwest coast, is Saccorhiza polyschides grows in the lowest shore and costal rocky reefs. It is almost exclusively used by local farmers as natural fertilizer, but contains a substantial amount of valuable compounds, particularly alginates, natural biopolymers of high interest for many industrial applications. Alginates are natural polysaccharides present in cell walls of brown seaweed, highly biocompatible, with particular properties that make them of high interest for the food, biotechnology, cosmetics and pharmaceutical industries. Conventional extraction processes are based on thermal treatment. They are lengthy and consume high amounts of energy and solvents. In recent years, microwave-assisted extraction (MAE) has shown enormous potential to overcome major drawbacks that outcome from conventional plant material extraction (thermal and/or solvent based) techniques, being also successfully applied to the extraction of agar, fucoidans and alginates. In the present study, acid pretreatment of brown seaweed Saccorhiza polyschides for subsequent microwave-assisted extraction (MAE) of alginate was optimized. Seaweeds were collected in Northwest Portuguese coastal waters of the Atlantic Ocean between May and August, 2014. Experimental design was used to assess the effect of temperature and acid pretreatment time in alginate extraction. Response surface methodology allowed the determination of the optimum MAE conditions: 40 mL of HCl 0.1 M per g of dried seaweed with constant stirring at 20ºC during 14h. Optimal acid pretreatment conditions have enhanced significantly MAE of alginates from Saccorhiza polyschides, thus contributing for the development of a viable, more environmental friendly alternative to conventional processes.

Keywords: Acid pretreatment, Alginate, Brown seaweed, Microwave-assisted extraction, Response surface methodology.

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Authors: Abdullah Faqihi, John Hedley

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Biosensors play a significant role in the healthcare sectors, scientific and technological progress. Developing electrodes that are easy to manufacture and deliver better electrochemical performance is advantageous for diagnostics and biosensing. They can be implemented extensively in various analytical tasks such as drug discovery, food safety, medical diagnostics, process controls, security and defence, in addition to environmental monitoring. Development of biosensors aims to create high-performance electrochemical electrodes for diagnostics and biosensing. A biosensor is a device that inspects the biological and chemical reactions generated by the biological sample. A biosensor carries out biological detection via a linked transducer and transmits the biological response into an electrical signal; stability, selectivity, and sensitivity are the dynamic and static characteristics that affect and dictate the quality and performance of biosensors. In this research, a developed experimental study for laser scribing technique for graphene oxide inside a vacuum chamber for processing of graphene oxide is presented. The processing of graphene oxide (GO) was achieved using the laser scribing technique. The effect of the laser scribing on the reduction of GO was investigated under two conditions: atmosphere and vacuum. GO solvent was coated onto a LightScribe DVD. The laser scribing technique was applied to reduce GO layers to generate rGO. The micro-details for the morphological structures of rGO and GO were visualised using scanning electron microscopy (SEM) and Raman spectroscopy so that they could be examined. The first electrode was a traditional graphene-based electrode model, made under normal atmospheric conditions, whereas the second model was a developed graphene electrode fabricated under a vacuum state using a vacuum chamber. The purpose was to control the vacuum conditions, such as the air pressure and the temperature during the fabrication process. The parameters to be assessed include the layer thickness and the continuous environment. Results presented show high accuracy and repeatability achieving low cost productivity.

Keywords: Laser scribing, LightScribe DVD, graphene oxide, scanning electron microscopy.

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