Search results for: ultrasonic solvent extraction (USE)

Authors: Alafara A. Baba, Kuranga I. Ayinla, Folahan A. Adekola, Rafiu B. Bale

Abstract:

Due to increasing demands and diverse applications of copper oxide as pigment in ceramics, cuprammonium hydroxide solution for rayon, p-type semi-conductor, dry cell batteries production and as safety disposal of hazardous materials, a study on the hydrometallurgical operations involving leaching, solvent extraction and precipitation for the recovery of copper for producing high grade copper oxide from a Nigerian chalcopyrite ore in chloride media has been examined. At a particular set of experimental parameter with respect to acid concentration, reaction temperature and particle size, the leaching investigation showed that the ore dissolution increases with increasing acid concentration, temperature and decreasing particle diameter at a moderate stirring. The kinetics data has been analyzed and was found to follow diffusion control mechanism. At optimal conditions, the extent of ore dissolution reached 94.3%. The recovery of the total copper from the hydrochloric acid-leached chalcopyrite ore was undertaken by solvent extraction and precipitation techniques, prior to the beneficiation of the purified solution as copper oxide. The purification of the leach liquor was firstly done by precipitation of total iron and manganese using Ca(OH)2 and H2O2 as oxidizer at pH 3.5 and 4.25, respectively. An extraction efficiency of 97.3% total copper was obtained by 0.2 mol/L Dithizone in kerosene at 25±2ºC within 40 minutes, from which ≈98% Cu from loaded organic phase was successfully stripped by 0.1 mol/L HCl solution. The beneficiation of the recovered pure copper solution was carried out by crystallization through alkali addition followed by calcination at 600ºC to obtain high grade copper oxide (Tenorite, CuO: 05-0661). Finally, a simple hydrometallurgical scheme for the operational extraction procedure amenable for industrial utilization and economic sustainability was provided.

Keywords: chalcopyrite ore, Nigeria, copper, copper oxide, solvent extraction

Procedia PDF Downloads 388

Authors: Muhammad Naeem, Abdulrahman A. Al-Rabiah

Abstract:

Technical mixture of C4 containing 1-butene and n-butane are very close to each other with respect to their boiling points i.e. -6.3°C for 1-butene and -1°C for n-butane. Extractive distillation process is used for the separation of 1-butene from the existing mixture of C4. The solvent is the essential of extractive distillation, and an appropriate solvent shows an important role in the process economy of extractive distillation. Aspen Plus has been applied for the separation of these hydrocarbons as a simulator; moreover NRTL activity coefficient model was used in the simulation. This model indicated that the material balances in this separation process were accurate for several solvent flow rates. Mixture of acetonitrile and water used as a solvent and 99 % pure 1-butene was separated. This simulation proposed the ratio of the feed to solvent as 1 : 7.9 and 15 plates for the solvent recovery column, previously feed to solvent ratio was more than this and the proposed plates were 30, which can economize the separation process.

Keywords: extractive distillation, 1-butene, Aspen Plus, ACN solvent

Procedia PDF Downloads 442

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

Procedia PDF Downloads 356

Authors: P. Kiran Kumar, S. Vijaya Krishna, Kavita Verma1, V. Himabindu

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Concern about global warming and energy security has led to increased biomass utilization as an alternative feedstock to fossil fuels. Biomass is a promising feedstock since it is abundant and cheap and can be transformed into fuels and chemical products. Microalgae biofuels are likely to have a much lower impact on the environment. Microalgae cultivation using sewage with industrial flue gases is a promising concept for integrated biodiesel production, CO₂ sequestration, and nutrients recovery. Autotrophic, Mixotrophic, and Heterotrophic are the three modes of cultivation for microalgae biomass. Several mechanical and chemical processes are available for the extraction of lipids/oily components from microalgae biomass. In organic solvent extraction methods, a prior drying of biomass and recovery of the solvent is required, which are energy-intensive. Thus, the hydrothermal process overcomes the drawbacks of conventional solvent extraction methods. In the hydrothermal process, the biomass is converted into oily components by processing in a hot, pressurized water environment. In this process, in addition to the lipid fraction of microalgae, other value-added products such as proteins, carbohydrates, and nutrients can also be recovered. In the present study was (Scenedesmus quadricauda) was isolated and cultivated in autotrophic, heterotrophic, and mixotrophically using sewage wastewater and industrial flue gas in batch and continuous mode. The harvested algae biomass from S. quadricauda was used for the recovery of lipids and bio-oil. The lipids were extracted from the algal biomass using sonication as a cell disruption method followed by solvent (Hexane) extraction, and the lipid yield obtained was 8.3 wt% with Palmitic acid, Oleic acid, and Octadeonoic acid as fatty acids. The hydrothermal process was also carried out for extraction of bio-oil, and the yield obtained was 18wt%. The bio-oil compounds such as nitrogenous compounds, organic acids, and esters, phenolics, hydrocarbons, and alkanes were obtained by the hydrothermal process of algal biomass. Nutrients such as NO₃⁻ (68%) and PO₄⁻ (15%) were also recovered along with bio-oil in the hydrothermal process.

Keywords: flue gas, hydrothermal process, microalgae, sewage wastewater, sonication

Procedia PDF Downloads 136

Authors: Dewi Selvia Fardhyanti, Astrilia Damayanti

Abstract:

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: Norsyamimi Hassim, Masturah Markom

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Supercritical fluid extraction (SFE) has been known as a sustainable and safe extraction technique for plant extraction due to the minimal usage of organic solvent. In this study, a scale-up process for the selected herbal plant (Phyllanthus niruri) was investigated by using supercritical carbon dioxide (SC-CO2) with food-grade (ethanol-water) cosolvent. The quantification of excess ethanol content in the final dry extracts was conducted to determine the safety of enriched extracts. The extraction yields obtained by scale-up SFE unit were not much different compared to the predicted extraction yields with an error of 2.92%. For component contents, the scale-up extracts showed comparable quality with laboratory-scale experiments. The final dry extract showed that the excess ethanol content was 1.56% g/g extract. The fish embryo toxicity test (FETT) on the zebrafish embryos showed no toxicity effects by the extract, where the LD50 value was found to be 505.71 µg/mL. Thus, it has been proven that SFE with food-grade cosolvent is a safe extraction technique for the production of bioactive compounds from P. niruri.

Keywords: scale-up, supercritical fluid extraction, enriched extract, toxicity, ethanol content

Procedia PDF Downloads 130

Authors: Reihaneh Ahmadzadeh Ghavidel

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Free radicals such as reactive oxygen species (ROS) have detrimental effects on human health through several mechanisms. On the other hand, antioxidant molecules reduce free radical generation in biologic systems. Synthetic antioxidants, which are used in food industry, have also negative impact on human health. Therefore recognition of natural antioxidants such as anthocyanins can solve these problems simultaneously. Coleus (Solenostemon scutellarioides) with red leaves is a rich source of anthocyanins compounds. In this study we evaluated the effect of time (10, 20 and 30 min) and temperature (40, 50 and 60° C) on optimization of anthocyanin extraction using surface response method. In addition, the study was aimed to determine maximum extraction for anthocyanin from coleus plant using ultrasound method. The results indicated that the optimum conditions for extraction were 39.84 min at 69.25° C. At this point, total compounds were achieved 3.7451 mg 100 ml⁻¹. Furthermore, under optimum conditions, anthocyanin concentration, extraction efficiency, ferric reducing ability, total phenolic compounds and EC50 were registered 3.221931, 6.692765, 223.062, 3355.605 and 2.614045, respectively.

Keywords: anthocyanin, antioxidant, coleus, extraction, sonication

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Authors: N. R. Putra, A. H. Abdul Aziz, A. S. Zaini, Z. Idham, F. Idrus, M. Z. Bin Zullyadini, M. A. Che Yunus

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The content of omega-3 in soybean oil is important in the development of infants and is an alternative for the omega-3 in fish oils. The investigation of extraction of soybean oil is needed to obtain the bioactive compound in the extract. Supercritical carbon dioxide extraction is modern and green technology to extract herbs and plants to obtain high quality extract due to high diffusivity and solubility of the solvent. The aim of this study was to obtain the optimum condition of soybean oil extraction by modified supercritical carbon dioxide. The soybean oil was extracted by using modified supercritical carbon dioxide (SC-CO₂) under the temperatures of 40, 60, 80 °C, pressures of 150, 250, 350 Bar, and constant flow-rate of 10 g/min as the parameters of extraction processes. An experimental design was performed in order to optimize three important parameters of SC-CO₂ extraction which are pressure (X₁), temperature (X₂) to achieve optimum yields of soybean oil. Box Behnken Design was applied for experimental design. From the optimization process, the optimum condition of extraction of soybean oil was obtained at pressure 338 Bar and temperature 80 °C with oil yield of 2.713 g. Effect of pressure is significant on the extraction of soybean oil by modified supercritical carbon dioxide. Increasing of pressure will increase the oil yield of soybean oil.

Keywords: soybean oil, SC-CO₂ extraction, yield, optimization

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Authors: N. Bourayou, A. -H. Meniai, A. Gouaoura

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The presence of salt can either raise or lower the distribution coefficient of a solute acetic acid in liquid- liquid equilibria. The coefficient of solute is defined as the ratio of the composition of solute in solvent rich phase to the composition of solute in diluents (water) rich phase. The phenomena are known as salting–out or salting-in, respectively. The effect of monovalent salt, sodium chloride and the bivalent salt, sodium sulfate on the distribution of acetic acid between 1-butanol and water at 298.15K were experimentally shown to be effective in modifying the liquid-liquid equilibrium of water/acetic acid/1-butanol system in favour of the solvent extraction of acetic acid from an aqueous solution with 1-butanol, particularly at high salt concentrations of both salts. All the two salts studied are found to have to salt out effect for acetic acid in varying degrees. The experimentally measured data were well correlated by Eisen-Joffe equation. NRTL model for solvent mixtures containing salts was able to provide good correlation of the present liquid-liquid equilibrium data. Using the regressed salt concentration coefficients for the salt-solvent interaction parameters and the solvent-solvent interaction parameters obtained from the same system without salt. The calculated phase equilibrium was in a quite good agreement with the experimental data, showing the ability of NRTL model to correlate salt effect on the liquid-liquid equilibrium.

Keywords: activity coefficient, Eisen-Joffe, NRTL model, sodium chloride

Procedia PDF Downloads 276

Authors: Michele C. Mesomo, Madeline de Souza Correa, Roberta L. Kruger, Luis R. S. Kanda, Marcos L. Corazza

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Natural extracts of plants have been used for many years for different purposes and recently they have been screened for their potential use as alternative remedies and food preservatives. Inflorescences of M. paradisiaca L., also known as the heart of the banana, have great economic interest due to its fruit. All parts of the banana are used for many different purposes, including use in folk medicine. The use of extraction via supercritical technology has grown in recent years, though it is still necessary to obtain experimental information for the construction of industrial plants. This work reports the extraction of Musa paradisiaca L. using compressed propane as solvent. The effects of the supercritical extraction conditions, pressure and temperature on the yield were evaluated. The raw material, inflorescences banana, was dried at 313.15 K and milled. The particle size used for the packaging of the extraction cell was 12 mesh (23.5%), 16 mesh (23.5%), 32 mesh (34.5%), 48 mesh (18.5%). The extractions were performed in a laboratory scale unit at pressures of 3.0 MPa, 6.5 MPa and 10.0 MPa and at 308.15 K, 323.15 K and 338.15 K. The operating conditions tested achieved a maximum yield of 2.94 wt% for the CO2 extraction at 10.0 MPa and 338.15 K, higher pressure and temperature. The lower yield, 2.29 wt%, was obtained in the condition of lower pressure and higher temperature. Temperature presented significant and positive effect on the extraction yield with supercritical CO2, while pressure had no effect on the yield. The overall extraction curves showed typical behavior obtained for the supercritical extraction procedure and and reached a constant extraction rate of about 80 to 100 min. The largest amount of extract was obtained at the beginning of the process, within 10 to 60 min.

Keywords: banana, natural products, supercritical extraction, temperature

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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

Procedia PDF Downloads 67

Authors: Muhammad Naeem, Abdulrahman A. Al-Rabiah, Wasif Mughees

Abstract:

Technical mixture of C4 containing 1-butene and n-butane are very close to each other with regard to their boiling points i.e. -6.3°C for 1-butene and -1°C for n-butane. Extractive distillation process is used for the separation of 1-butene from the existing mixture of C4. The solvent is the essential of extractive distillation, and an appropriate solvent plays an important role in the process economy of extractive distillation. Aspen Plus has been applied for the separation of these hydrocarbons as a simulator. Moreover, NRTL activity coefficient model was used in the simulation. This model indicated that the material balances in this separation process were accurate for several solvent flow rates. Mixture of acetonitrile and water used as a solvent and 99% pure 1-butene was separated. This simulation proposed the ratio of the feed to solvent as 1: 7.9 and 15 plates for the solvent recovery column. Previously feed to solvent ratio was more than this and the number of proposed plates were 30, which shows that the separation process can be economized.

Keywords: extractive distillation, 1-butene, aspen plus, ACN solvent

Procedia PDF Downloads 533

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 253

Authors: Elham Mahdian, Reza Karazhian, Rahele Dehghan Tanha

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Pepper (Capsicum annum L.) which belong to the family Solananceae, are known for their versatility as a vegetable crop and are consumed both as fresh vegetables or dehydrated for spices. Pepper is considered an excellent source of bioactive nutrients. Ascorbic acid, carotenoids and phenolic compounds are its main antioxidant constituents. Ultrasound assisted extraction is an inexpensive, simple and efficient alternative to conventional extraction techniques. The mechanism of action for ultrasound-assisted extraction are attributed to cavitations, mechanical forces and thermal impact, which result in disruption of cells walls, reduce particle size, and enhance mass transfer across cell membranes. In this study, response surface methodology was used to optimize experimental conditions for ultrasonic assisted extraction of carotenoid compounds from Chili peppers. Variables were included extraction temperatures at 3 levels (30, 40 and 50 °C), extraction times at 3 levels (10, 25 and 40 minutes) and power at 3 levels (30, 60 and 90 %). It was observed that ultrasound waves applied at temperature of 49°C, time of 10 minutes and power 89 % resulted to the highest carotenoids contents (lycopene and β-carotene), while the lowest value was recorded in the control. Thus, results showed that ultrasound waves have strong impact on extraction of carotenoids from pepper.

Keywords: carotenoids, optimization, pepper, response surface methodology

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Authors: Ali Naeemy, Mir Ghasem Hoseini

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In this study, for the first time, an analytical method developed and validated by combining electrochemical impedance spectroscopy and electromembrane extraction (EIS-EME) by Vulcan/poly pyrrole nanocomposite modified screen-printed electrode (PPY–VU/SPE) for accurately quantifying zolpidem. EME parameters optimized, including solvent composition, voltage, pH adjustments and extraction time. Zolpidem was transferred from a donor solution (pH 5) to an acceptor solution (pH 13) using a hollow fiber in 1-octanol as a membrane, driven by a 60 V voltage for 25 minutes, ensuring precise and selective extraction. In comparison with SPE, VU/SPE and PPY/SPE, the PPY–VU/SPE was much more efficient for ZP oxidation. Calibration curves with good linearity were obtained in the concentration range of 2-75 µmol L-1 using the EIS-EME with the detection limit of 0.5 µmol L-1 . Finally, the EIS-EME by using the PPY– VU/SPE was successfully used to determine ZP in tablet dosage form, urine and plasma samples. Keywords: Electrochemical impedance spectroscopy, Electromembrane extraction, Zolpidem, Vulcan, poly pyrrole, Screen printed electrode

Keywords: electrochemical impedance spectroscopy, electromembrane extraction, screen printed electrode, zolpidem

Procedia PDF Downloads 34

Authors: Birute Bugelyte, Ingrida Jurkute, Vida Vickackaite

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The most complicated step of the determination of volatile compounds in complex matrices is the separation of analytes from the matrix. Traditional analyte separation methods (liquid extraction, Soxhlet extraction) require a lot of time and labour; moreover, there is a risk to lose the volatile analytes. In recent years, headspace gas chromatography has been used to determine volatile compounds. To date, traditional extraction solvents have been used in headspace gas chromatography. As a rule, such solvents are rather volatile; therefore, a large amount of solvent vapour enters into the headspace together with the analyte. Because of that, the determination sensitivity of the analyte is reduced, a huge solvent peak in the chromatogram can overlap with the peaks of the analyts. The sensitivity is also limited by the fact that the sample can’t be heated at a higher temperature than the solvent boiling point. In 2018 it was suggested to replace traditional headspace gas chromatographic solvents with non-volatile, eco-friendly, biodegradable, inexpensive, and easy to prepare deep eutectic solvents (DESs). Generally, deep eutectic solvents have low vapour pressure, a relatively wide liquid range, much lower melting point than that of any of their individual components. Those features make DESs very attractive as matrix media for application in headspace gas chromatography. Also, DESs are polar compounds, so they can be applied for microwave assisted extraction. The aim of this work was to investigate the possibility of applying deep eutectic solvents for microwave assisted extraction and headspace gas chromatographic determination of hexanal in fat-rich food. Hexanal is considered one of the most suitable indicators of lipid oxidation degree as it is the main secondary oxidation product of linoleic acid, which is one of the principal fatty acids of many edible oils. Eight hydrophilic and hydrophobic deep eutectic solvents have been synthesized, and the influence of the temperature and microwaves on their headspace gas chromatographic behaviour has been investigated. Using the most suitable DES, microwave assisted extraction conditions and headspace gas chromatographic conditions have been optimized for the determination of hexanal in potato chips. Under optimized conditions, the quality parameters of the prepared technique have been determined. The suggested technique was applied for the determination of hexanal in potato chips and other fat-rich food.

Keywords: deep eutectic solvents, headspace gas chromatography, hexanal, microwave assisted extraction

Procedia PDF Downloads 188

Authors: Seunghee Park, Junkyeong Kim, Eun-Seok Shin, Sang-Hun Han

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In this study, two kinds of nondestructive evaluation (NDE) techniques (rebound hardness and ultrasonic pulse velocity methods) are investigated for the effective maintenance of underwater concrete structures. A new methodology to estimate the underwater concrete strengths more effectively, named “artificial neural network (ANN) – based concrete strength estimation with the combination of rebound hardness and ultrasonic pulse velocity methods” is proposed and verified throughout a series of experimental works.

Keywords: underwater concrete, rebound hardness, Schmidt hammer, ultrasonic pulse velocity, ultrasonic sensor, artificial neural networks, ANN

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Authors: Majid Zargar, Frank Bullen, Ron Ayers

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One of the important factors in the design of asphalt concrete mixes is the accurate measurement of air voids and their variable distribution. Both can have significant impact on long and short term fatigue and creep behaviour under traffic. While some simple methods exist for overall evaluation of air voids, measuring air void distribution in asphalt concrete is very complex, involving expensive techniques such as X-ray methodologies. The research reported in the paper investigated the use of non-destructive ultrasonic techniques as an alternative to estimate the amount of air voids and their distribution within asphalt samples. Seventy-four Standard AC–14 asphalt samples made with three types of bitumen; Multigrade, PMB and C320 were analysed using ultrasonic techniques. The results have illustrated that ultrasonic testing has the potential of being a rapid, accurate and cost-effective method of estimating air void distribution in asphalt.

Keywords: asphalt concrete, air voids, ultrasonic, mechanical behaviour

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Authors: Seyda Donmez, Oya Aydin Urucu, Ece Kok Yetimoglu

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Solidified floating organic drop microextraction was used for a preconcentration method of trace amount of lead. The analyte was complexed with 1-(2-pyridylazo)-2-naphtol and 1-undecanol, acetonitrile was added as an extraction and dispersive solvent respectively. The influences of some analytical parameters pH, volumes of extraction and disperser solvent, concentration of chelating agent, and concentration of salt were optimized. Under the optimum conditions the detection limits of Pb (II) was determined. The procedure was validated for the analysis of NCS DC 73347a hair standard reference material with satisfactory result. The developed procedure was successfully applied to food and water samples for detection of Pb (II) ions.

Keywords: analytical methods, graphite furnace atomic absorption spectrometry, heavy metals, solidified floating organic drop microextraction

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Authors: J. W. Choi, S. Y. Cho, H. J. Lee, W. Z. Oh, S. J. Choi

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Ionic liquids (ILs), which is alternative to conventional organic solvent, were used for extraction of Cs ions. ILs, as useful environment friendly green solvents, have been recently applied as replacement for traditional volatile organic compounds (VOCs) in liquid/liquid extraction of heavy metal ions as well as organic and inorganic species and pollutants. Thus, Ionic liquids were used for extraction of Cs ions from the liquid radioactive waste. In most cases, Cs ions present in radioactive wastes in very low concentration, approximately less than 1ppm. Therefore, unlike established extraction system the required amount of ILs as extractant is comparatively very small. This extraction method involves cation exchange mechanism in which Cs ion transfers to the organic phase and binds to one crown ether by chelation in exchange of single ILs cation, IL_cation+, transfer to the aqueous phase. In this extraction system showed solid-liquid separation in which the Ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonly)imide (C2mimTf2N) and the crown ether Dicyclohexano-18-crown-6 (DCH18C6) both were used here in very little amount as solvent and as extractant, respectively. 30 mM of CsNO3 was used as simulated waste solution cesium ions. Generally, in liquid-liquid extraction, the molar ratio of CE:Cs+:ILs was 1:5~10:>100, while our applied molar ratio of CE:Cs+:ILs was 1:2:1~10. The quantity of CE and Cs ions were fixed to 0.6 and 1.2 mmol, respectively. The phenomenon of precipitation showed two kinds of separation: solid-liquid separation in the ratio of 1:2:1 and 1:2:2; solid-liquid-liquid separation (3 phase) in the ratio of 1:2:5 and 1:2:10. In the last system, 3 phases were precipitate-ionic liquids-aqueous. The precipitate was verified to consist of Cs+, DCH18C6, Tf2N- based on the cation exchange mechanism. We analyzed precipitate using scanning electron microscopy with X-ray microanalysis (SEM-EDS), an elemental analyser, Fourier transform infrared spectroscopy (FT-IR) and differential scanning calorimetry (DSC). The experimental results showed an easy extraction method and confirmed the composition of solid precipitate. We also obtained information that complex formation ratio of Cs+ to DCH18C6 is 0.88:1 regardless of C2mimTf2N quantities.

Keywords: extraction, precipitation, solid-liquid seperation, ionic liquid, precipitate

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Authors: Margarita Belousova

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The ultrasonic densitometry (RU patent № 2541038) was used to assess the density of the bone tissue in the jaws of patients after orthodontic treatment. In addition, by ultrasonic densitometry assessed the state of the bone tissue in the region III phalanges of middle fingers in above mentioned patients. A comparative study was carried out in healthy volunteers of same age. It was established a significant decrease of the ultrasound wave speed and bone mineral density after active period of orthodontic treatment. Statistically, significant differences in bone mineral density of the fingers by ultrasonic densitometry in both groups of patients were not detected.

Keywords: intraoral ultrasonic densitometry, bone tissue density of jaws, bone tissue density of phalanges of fingers, orthodontic treatment

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Authors: M. Dehghan, R. Al-Mahaidi, I. Sbarski

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An industrial epoxy adhesive used in Carbon Fiber Reinforced Polymer (CFRP)-strengthening systems was modified by dispersing multi-walled carbon nanotubes (MWCNTs). Nanocomposites were fabricated using solvent-assisted dispersion method and ultrasonic mixing. Thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA) and tensile tests were conducted to study the effect of nanotubes dispersion on the thermal and mechanical properties of the epoxy composite. Experimental results showed a substantial enhancement in the decomposition temperature and tensile properties of epoxy composite, while, the glass transition temperature (Tg) was slightly reduced due to the solvent effect. The morphology of the epoxy nanocomposites was investigated by SEM. It was proved that using solvent improves the nanotubes dispersion. However, at contents higher than 2 wt. %, nanotubes started to re-bundle in the epoxy matrix which negatively affected the final properties of epoxy composite.

Keywords: carbon fiber reinforced polymer, epoxy, multi-walled carbon nanotube, DMA, glass transition temperature

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Authors: Orose Rugchati, Khumthong Mahawongwiriya

Abstract:

Dendrobium hybrid cv. Ear-Sakul has become one of the important commercial commodities in Thailand agricultural industry worldwide, either as potted plants or as cut flowers due to the attractive color produced in flower petals. Anthocyanins are the main flower pigments and responsible for the natural attractive display of petal colors. These pigments play an important role in functionality, such as to attract animal pollinators, classification, and grading of these orchids. Dendrobium hybrid cv. Ear-Sakul has been collected from local area farm in different stage flowers (F1, F2-F5, and F6). Anthocyanins pigment were extracted from the fresh flower by solvent extraction (MeOH–TFA 99.5:0.5v/v at 4ºC) and purification with ethyl acetate. The main anthocyanins components are cyanidin, pelargonidin, and delphinidin. Pure anthocyanin contents were analysis by UV-Visible spectroscopy technique at λ max 535, 520 and 546 nm respectively. The anthocyanins contents were converted in term of monomeric anthocyanins pigment (mg/L). The anthocyanins contents of all sample were compared with standard pigments cyanidin, pelargonidin and delphinidin. From this experiment is a simple extraction and analysis anthocyanins content in different stage of flowers results shown that monomeric anthocyanins pigment contents of different stage flowers (F1, F2-F5 and F6 ): cyanidin – 3 – glucoside (mg/l) are 0.85+0.08, 24.22+0.12 and 62.12+0.6; Pelargonidin 3,5-di- glucoside(mg/l) 10.37+0.12, 31.06+0.8 and 81.58+ 0.5; Delphinidin (mg/l) 6.34+0.17, 18.98+0.56 and 49.87+0.7; and the appearance of extraction pure anthocyanins in L(a, b): 2.71(1.38, -0.48), 1.06(0.39,-0.66) and 2.64(2.71,-3.61) respectively. Dendrobium Hybrid cv. Ear-Sakul could be used as a source of anthocyanins by simple solvent extraction and stage of flowers as a guideline for the prediction amount of main anthocyanins components are cyanidin, pelargonidin, and delphinidin could be application and development in quantities, and qualities with the advantage for food pharmaceutical and cosmetic industries.

Keywords: analysis, anthocyanins contents, different stage flowers, Dendrobium Hybrid cv. Ear-Sakul

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Authors: Kuen Ming Shu, Ren Kai Ho

Abstract:

Ultrasonic horn has the functions of amplifying amplitude and reducing resonant impedance in ultrasonic system. Its primary function is to amplify deformation or velocity during vibration and focus ultrasonic energy on the small area. It is a crucial component in design of ultrasonic vibration system. There are five common design methods for ultrasonic horns: analytical method, equivalent circuit method, equal mechanical impedance, transfer matrix method, finite element method. In addition, the general optimization design process is to change the geometric parameters to improve a single performance. Therefore, in the general optimization design process, we couldn't find the relation of parameter and objective. However, a good optimization design must be able to establish the relationship between input parameters and output parameters so that the designer can choose between parameters according to different performance objectives and obtain the results of the optimization design. In this study, an ultrasonic horn provided by Maxwide Ultrasonic co., Ltd. was used as the contrast of optimized ultrasonic horn. The ANSYS finite element analysis (FEA) software was used to simulate the distribution of the horn amplitudes and the natural frequency value. The results showed that the frequency for the simulation values and actual measurement values were similar, verifying the accuracy of the simulation values. The ANSYS DesignXplorer was used to perform Response Surface optimization, which could shows the relation of parameter and objective. Therefore, this method can be used to substitute the traditional experience method or the trial-and-error method for design to reduce material costs and design cycles.

Keywords: horn, natural frequency, response surface optimization, ultrasonic vibration

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Authors: Lenuta Kloetzer, Alexandra C. Blaga, Dan Cascaval, Alexandra Tucaliuc, Anca I. Galaction

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Rosmarinic acid, an ester of caffeic acid and 3-(3,4-dihydroxyphenyl) lactic acid, is considered a valuable compound for the pharmaceutical and cosmetic industries due to its antimicrobial, antioxidant, antiviral, anti-allergic, and anti-inflammatory effects. It can be obtained by extraction from vegetable or animal materials, by chemical synthesis and biosynthesis. Indifferent of the method used for rosmarinic acid production, the separation and purification process implies high amount of raw materials and laborious stages leading to high cost for and limitations of the separation technology. This study focused on separation of rosmarinic acid by synergic reactive extraction with a mixture of two extractants, one acidic (acid di-(2ethylhexyl) phosphoric acid, D2EHPA) and one with basic character (Amberlite LA-2). The studies were performed in experimental equipment consisting of an extraction column where the phases’ mixing was made by mean of a perforated disk with 45 mm diameter and 20% free section, maintained at the initial contact interface between the aqueous and organic phases. The vibrations had a frequency of 50 s⁻¹ and 5 mm amplitude. The extraction was carried out in two solvents with different dielectric constants (n-heptane and dichloromethane) in which the extractants mixture of varying concentration was dissolved. The pH-value of initial aqueous solution was varied between 1 and 7. The efficiency of the studied extraction systems was quantified by distribution and synergic coefficients. For calculating these parameters, the rosmarinic acid concentration in the initial aqueous solution and in the raffinate have been measured by HPLC. The influences of extractants concentrations and solvent polarity on the efficiency of rosmarinic acid separation by synergic extraction with a mixture of Amberlite LA-2 and D2EHPA have been analyzed. In the reactive extraction system with a constant concentration of Amberlite LA-2 in the organic phase, the increase of D2EHPA concentration leads to decrease of the synergic coefficient. This is because the increase of D2EHPA concentration prevents the formation of amine adducts and, consequently, affects the hydrophobicity of the interfacial complex with rosmarinic acid. For these reasons, the diminution of synergic coefficient is more important for dichloromethane. By maintaining a constant value of D2EHPA concentration and increasing the concentration of Amberlite LA-2, the synergic coefficient could become higher than 1, its highest values being reached for n-heptane. Depending on the solvent polarity and D2EHPA amount in the solvent phase, the synergic effect is observed for Amberlite LA-2 concentrations over 20 g/l dissolved in n-heptane. Thus, by increasing the concentration of D2EHPA from 5 to 40 g/l, the minimum concentration value of Amberlite LA-2 corresponding to synergism increases from 20 to 40 g/l for the solvent with lower polarity, namely, n-heptane, while there is no synergic effect recorded for dichloromethane. By analysing the influences of the main factors (organic phase polarity, extractant concentration in the mixture) on the efficiency of synergic extraction of rosmarinic acid, the most important synergic effect was found to correspond to the extractants mixture containing 5 g/l D2EHPA and 40 g/l Amberlite LA-2 dissolved in n-heptane.

Keywords: Amberlite LA-2, di(2-ethylhexyl) phosphoric acid, rosmarinic acid, synergic effect

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Authors: N. Prabavathy, R. Balasundaraprabhu, S. Shalini, Dhayalan Velauthapillai, S. Prasanna, N. Muthukumarasamy

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Dye sensitized solar cell (DSSC) has become a significant research area due to their fundamental and scientific importance in the area of energy conversion. Synthetic dyes as sensitizer in DSSC are efficient and durable but they are costlier, toxic and have the tendency to degrade. Natural sensitizers contain plant pigments such as anthocyanin, carotenoid, flavonoid, and chlorophyll which promote light absorption as well as injection of charges to the conduction band of TiO2 through the sensitizer. But, the efficiency of natural dyes is not up to the mark mainly due to instability of the pigment such as anthocyanin. The stability issues in vitro are mainly due to the effect of solvents on extraction of anthocyanins and their respective pH. Taking this factor into consideration, in the present work, the anthocyanins were extracted from the flower Caesalpinia pulcherrima (C. pulcherrimma) with various solvents and their respective stability and pH values are discussed. The usage of citric acid as solvent to extract anthocyanin has shown good stability than other solvents. It also helps in enhancing the sensitization properties of anthocyanins with Titanium dioxide (TiO2) nanorods. The IPCE spectra show higher photovoltaic performance for dye sensitized TiO2nanorods using citric acid as solvent. The natural DSSC using citric acid as solvent shows a higher efficiency compared to other solvents. Hence citric acid performs to be a safe solvent for natural DSSC in boosting the photovoltaic performance and maintaining the stability of anthocyanins.

Keywords: Caesalpinia pulcherrima, citric acid, dye sensitized solar cells, TiO₂ nanorods

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Authors: L. Cesari, L. Canabady-Rochelle, F. Mutelet

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The thermal conversion of lignin produces bio-oils that contain many compounds with high added-value such as phenolic compounds. In order to efficiently extract these compounds, the possible use of choline bis(trifluoromethylsulfonyl)imide [Choline][NTf2] ionic liquid was explored. To this end, a multistep approach was implemented. First, binary (phenolic compound and solvent) and ternary (phenolic compound and solvent and ionic liquid) solutions were investigated. Eight binary systems of phenolic compound and water were investigated at atmospheric pressure. These systems were quantified using the turbidity method and UV-spectroscopy. Ternary systems (phenolic compound and water and [Choline][NTf2]) were investigated at room temperature and atmospheric pressure. After stirring, the solutions were let to settle down, and a sample of each phase was collected. The analysis of the phases was performed using gas chromatography with an internal standard. These results were used to quantify the values of the interaction parameters of thermodynamic models. Then, extractions were performed on synthetic solutions to determine the influence of several operating conditions (temperature, kinetics, amount of [Choline][NTf2]). With this knowledge, it has been possible to design and simulate an extraction process composed of one extraction column and one flash. Finally, the extraction efficiency of [Choline][NTf2] was quantified with real bio-oils from lignin pyrolysis. Qualitative and quantitative analysis were performed using gas chromatographic connected to mass spectroscopy and flame ionization detector. The experimental measurements show that the extraction of phenolic compounds is efficient at room temperature, quick and does not require a high amount of [Choline][NTf2]. Moreover, the simulations of the extraction process demonstrate that [Choline][NTf2] process requires less energy than an organic one. Finally, the efficiency of [Choline][NTf2] was confirmed in real situations with the experiments on lignin pyrolysis bio-oils.

Keywords: bio-oils, extraction, lignin, phenolic compounds

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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: Kyohei Yoshino, Masahiko Matsumiya, Yuji Sasaki

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Recently, studies have been conducted on Au(III) extraction using ionic liquids (ILs) as extractants or diluents. ILs such as piperidinium, pyrrolidinium, and pyridinium have been studied as extractants for noble metal extractions. Furthermore, the polarity, hydrophobicity, and solvent miscibility of these ILs can be adjusted depending on their intended use. Therefore, the unique properties of ILs make them functional extraction media. The extraction mechanism of Au(III) using phosphonium-based ILs and relevant thermodynamic studies are yet to be reported. In the present work, we focused on the mechanism of Au(III) extraction and related thermodynamic analyses using phosphonium-based ILs. Triethyl-n-pentyl, triethyl-n-octyl, and triethyl-n-dodecyl phosphonium bis(trifluoromethyl-sulfonyl)amide, [P₂₂₂ₓ][NTf₂], (X = 5, 8, and 12) were investigated for Au(III) extraction. The IL–Au complex was identified as [P₂₂₂₅][AuCl₄] using UV–Vis–NIR and Raman spectroscopic analyses. The extraction behavior of Au(III) was investigated with a change in the [P₂₂₂ₓ][NTf₂]IL concentration from 1.0 × 10–4 to 1.0 × 10–1 mol dm−3. The results indicate that Au(III) can be easily extracted by the anion-exchange reaction in the [P₂₂₂ₓ][NTf₂]IL. The slope range 0.96–1.01 on the plot of log D vs log[P₂₂₂ₓ][NTf2]IL indicates the association of one mole of IL with one mole of [AuCl4−] during extraction. Consequently, [P₂₂₂ₓ][NTf₂] is an anion-exchange extractant for the extraction of Au(III) in the form of anions from chloride media. Thus, this type of phosphonium-based IL proceeds via an anion exchange reaction with Au(III). In order to evaluate the thermodynamic parameters on the Au(III) extraction, the equilibrium constant (logKₑₓ’) was determined from the temperature dependence. The plot of the natural logarithm of Kₑₓ’ vs the inverse of the absolute temperature (T–1) yields a slope proportional to the enthalpy (ΔH). By plotting T–1 vs lnKₑₓ’, a line with a slope range 1.129–1.421 was obtained. Thus, the result indicated that the extraction reaction of Au(III) using the [P₂₂₂ₓ][NTf₂]IL (X=5, 8, and 12) was exothermic (ΔH=-9.39〜-11.81 kJ mol-1). The negative value of TΔS (-4.20〜-5.27 kJ mol-1) indicates that microscopic randomness is preferred in the [P₂₂₂₅][NTf₂]IL extraction system over [P₂₂₂₁₂][NTf₂]IL. The total negative alternation in Gibbs energy (-5.19〜-6.55 kJ mol-1) for the extraction reaction would thus be relatively influenced by the TΔS value on the number of carbon atoms in the alkyl side length, even if the efficiency of ΔH is significantly influenced by the total negative alternations in Gibbs energy. Electrochemical analysis revealed that extracted Au(III) can be reduced in two steps: (i) Au(III)/Au(I) and (ii) Au(I)/Au(0). The diffusion coefficients of the extracted Au(III) species in [P₂₂₂ₓ][NTf₂] (X = 5, 8, and 12) were evaluated from 323 to 373 K using semi-integral and semi-differential analyses. Because of the viscosity of the IL medium, the diffusion coefficient of the extracted Au(III) increases with increasing alkyl chain length. The 4f7/2 spectrum based on X-ray photoelectron spectroscopy revealed that the Au electrodeposits obtained after 10 cycles of continuous extraction and electrodeposition were in the metallic state.

Keywords: au(III), electrodeposition, phosphonium-based ionic liquids, solvent extraction

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Authors: Michał Maksimczuk, Łukasz Kaczmarek, Tomasz Wejrzanowski

Abstract:

This study concerns high-resolution X-ray computed microtomography (µCT) and ultrasonic pulse analysis of Cambrian sandstones from a borehole located in the Baltic Sea Coast of northern Poland. µCT and ultrasonic technique are non-destructive methods commonly used to determine the internal structure of reservoir rock sample. The spatial resolution of the µCT images obtained was 27 µm, which enabled the author to create accurate 3-D visualizations of structure geometry and to calculate the ratio of pores volume to the total sample volume. A copper X-ray source filter was used to reduce image artifacts. Furthermore, samples Young’s modulus and Poisson ratio were obtained with use of ultrasonic pulse technique. µCT and ultrasonic pulse technique provide complex information which can be used for explorations and characterization of reservoir rocks.

Keywords: elastic parameters, linear absorption coefficient, northern Poland, tight gas

Procedia PDF Downloads 246