Search results for: solvent extraction in Ionic liquid

Authors: Netsanet Kebede Hundessa

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Substrate modification of thin film composite (TFC) membranes with various crosslinkers is typically necessary for organic solvent nanofiltration (OSN) applications. This modification is aimed at enhancing membrane stability and solvent resistance, but it often results in a decline in permeance. This study introduces a distinct approach by developing a coordination-crosslinked polyimide substrate, which differs from the covalently-crosslinked substrates traditionally used. This developed substrate achieves enhanced solvent resistance, improved hydrophilicity, and optimized porous microstructure simultaneously. The study investigates the effects of an alkaline coagulation bath, subsequent ion exchange, and further solvent activation. The resulting TFC membrane successfully overcomes the typical permeability-selectivity trade-off of OSN membranes. It demonstrates significantly improved solvent permeance (1.5–2 times higher than previously reported data) with values of 65.2 LMH/bar for methanol, 33.1 LMH/bar for ethanol, and 59.1 LMH/bar for acetone while maintaining competitive solute rejection (>98% for Rose Bengal). This research is expected to provide a new direction for developing high-performance OSN composite membranes and other separation applications.

Keywords: metal coordinatiom, thin film composite membrane, organic solvent nanofiltration, solvent activation

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Authors: Marina Stramarkou, Sofia Papadaki, Konstantina Kyriakopoulou, Magdalini Krokida

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Nowadays, microalgae represent the diverse branch of microorganism that is used not only in fish farming, but also in food, cosmetics, pharmaceuticals and biofuel production as they can produce a wide range of unique functional ingredients. In the present work, a remarkable microalga Chlorella vulgaris (CV) was selected as a raw material for the recovery of multifunctional extracts. First of all, the drying of raw biomass was examined with freeze-drying showing the best behavior. Ultrasonic-assisted extraction (UAE) using different solvents was applied under the specific optimized conditions. In case of raw biomass, ethanol was the suitable solvent, whereas on dried samples water performed better. The total carotenoid, β-carotene, chlorophyll and protein content in the raw materials, extracts and extraction residues was determined using UV-Vis spectrometry. The microalgae biomass and the extracts were evaluated regarding their antiradical activity using the DPPH method.

Keywords: antioxidant activity, pigments, proteins, ultrasound assisted extraction

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Authors: Adetokunbo Ademola Falade, Oluwatoyin Olakunle Akinsete, Hussein Omeiza Aliu

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Solvent-aided dilution processes are often employed to recover bitumen by reducing its viscosity. In this study, methanol, toluene, and xylene were investigated as potential hydrocarbon solvents for solvent-aided hydrocarbon recovery of Agbabu bitumen. Solubility, Viscosity, and Saturate, Aromatic, Resin and Asphaltene (SARA) Analysis tests were carried out to determine the solubility of the bitumen in the solvents, the viscosity, and the SARA fraction of the natural bitumen and bitumen-solvent mixtures. Agbabu bitumen was found to have a high content of saturates and aromatics. Viscosity decreases as pressure increases, while solubility reduces as temperature increases. The experimental diffusivity of the sample decreases with temperature and increases with pressure, indicating that the presence of additional solvent molecules in the oil phase facilitates diffusion. Agbabu bitumen was found to be most soluble in toluene, and its viscosity was reduced most in it. Xylene exhibited a similar effect as toluene on the sample, though lesser but better than methanol. Methanol reduced the saturated content and significantly raised the asphaltene content, keeping the mixture viscosity high, a condition that, in turn, favors its colloidal stability. The colloidal instability index (CII) values, which account for the asphaltene stability of the mixture, show that the bitumen-methanol system with a CII of 0.874 will have mild asphaltene deposit issues while others are unstable. This approach of combining multiple tests with the CII can accurately predict the behavior of Agbabu bitumen in solvents and enhance the decision on the choice of bitumen recovery technology.

Keywords: asphaltene, bitumen, diffusivity, hydrocarbon solvent, SARA

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Authors: Kolela J Nyembwe, Darlington C. Ashiegbu, Herman J. Potgieter

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Over the past few decades, the demand for metals has increased significantly. This has led to a decrease and decline of high-grade ore over time and an increase in mineral complexity and matrix heterogeneity. In addition to that, there are rising concerns about greener processes and a sustainable environment. Due to these challenges, the mining and metal industry has been forced to develop new technologies that are able to economically process and recover metallic values from low-grade ores, materials having a metal content locked up in industrially processed residues (tailings and slag), and complex matrix mineral deposits. Several methods to address these issues have been developed, among which are ionic liquids (IL), heap leaching, and bioleaching. Recently, the gas phase extraction technique has been gaining interest because it eliminates many of the problems encountered in conventional mineral processing methods. The technique relies on the formation of volatile metal complexes, which can be removed from the residual solids by a carrier gas. The complexes can then be reduced using the appropriate method to obtain the metal and regenerate-recover the organic extractant. Laboratory work on the gas phase have been conducted for the extraction and recovery of aluminium (Al), iron (Fe), copper (Cu), chrome (Cr), nickel (Ni), lead (Pb), and vanadium V. In all cases the extraction revealed to depend of temperature and mineral surface area. The process technology appears very promising, offers the feasibility of recirculation, organic reagent regeneration, and has the potential to deliver on all promises of a “greener” process.

Keywords: gas-phase extraction, hydrometallurgy, low-grade ore, sustainable environment

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Authors: J. Švarc-Gajić, A. Cvetanović

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Apigenin is a flavone synthetized by many plants and quite abundant in chamomile (Matricaria recutita) in its free form and in the form of its glucoside and different acylated forms. Many beneficial health effects have been attributed to apigenin, such as chemo-preventive, anxiolytic, anti-inflammatory, antioxidant and antispasmodic. It is reported that free apigenin is much more bioactive in comparison to its bound forms. Subcritical water offers numerous advantages in comparison to conventional extraction techniques, such as good selectivity, low price and safety. Superheated water exhibits high hydrolytical potential which must be carefully balanced when using this solvent for the extraction of bioactive molecules. Moderate hydrolytical potential can be exploited to liberate apigenin from its bound forms, thus increasing biological potential of obtained extracts. The polarity of pressurized water and its hydrolytical potential are highly dependent on the temperature. In this research chamomile ligulate flowers were extracted by pressurized hot water in home-made subcritical water extractor in conditions of convective mass transfer. The influence of the extraction temperature was investigated at 30 bars. Extraction yields of total phenols, total flavonoids and apigenin depending on the operational temperature were calculated based on spectrometric assays. Optimal extraction temperature for maximum yields of total phenols and flavonoids showed to be 160°C, whereas apigenin yield was the highest at 120°C.

Keywords: superheated water, temperature, chamomile, apigenin

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Authors: Vijayalakshmi Marella, NageswaraRaoPilli

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This paper describes a simple, rapid and sensitive liquid chromatography / tandem mass spectrometry assay for the determination of montelukast in human plasma using montelukast d6 as an internal standard. Analyte and the internal standard were extracted from 50 µL of human plasma via solid phase extraction technique without evaporation, drying and reconstitution steps. The chromatographic separation was achieved on a C18 column by using a mixture of methanol and 5mM ammonium acetate (80:20, v/v) as the mobile phase at a flow rate of 0.8 mL/min. Good linearity results were obtained during the entire course of validation. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more number of samples in short time, thus increasing the productivity. The proposed method was found to be applicable to clinical studies.

Keywords: Montelukast, tandem mass spectrometry, montelukast d6, FDA guidelines

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Authors: Othman Saoudi

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In this work, we have interested in the investigation of the chemical denaturants and synthesized ionic liquids effects on the fluorescence properties of the laccase from Trametes versicolor. The fluorescence properties of the laccase result from the presence of Tryptophan, which has an aromatic core responsible for the absorption in ultra violet domain and the emission of the photons of fluorescence. The effect Pyrrolidinuim Formate ([pyrr][F]) and Morpholinium Formate ([morph][F]) ionic liquids on the laccase behavior for various volumetric fractions are studied. We have shown that the fluorescence spectrum relative to the [pyrr][F] presents a single band with a maximum around 340 nm and a secondary peak at 361 nm for a volumetric fraction of 20% v/v. For concentration superiors to 40%, the fluorescence intensity decreases and a displacement of the peaks toward higher wavelengths has occurred. For the [morph][F], the fluorescence spectrum showed a single band around 340 nm. The intensity of the principal peak decreases for concentration superiors to 20% v/v. From the plot representing the variation of the λₘₐₓ versus the volumetric concentration, we have determined the concentration of the half-transitions C1/2. These concentrations are equal to 42.62% and 40.91% v/v in the presence of [pyrr][F] and [morph][F] respectively. For the chemical denaturation, we have shown that the fluorescence intensity decreases with increasing denaturant concentrations where the maximum of the wavelength of emission shifts toward the higher wavelengths. We have also determined from the spectrum relative to the urea and GdmCl, the unfolding energy, ∆GD. The results show that the variation of the unfolding energy as a function of the denaturant concentrations varies according to the linear regression model. We have demonstrated also that the half-transitions C1/2 have occurred for urea and GdmCl denaturants concentrations around 3.06 and 3.17 M respectively.

Keywords: laccase, fluorescence, ionic liquids, chemical denaturants

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Authors: Marta Paszkiewicz, Justyna Łuczak, Martyna Marchelek, Adriana Zaleska-Medynska

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In recent years, photocatalytical processes have been intensively investigated for destruction of pollutants, hydrogen evolution, disinfection of water, air and surfaces, for the construction of self-cleaning materials (tiles, glass, fibres, etc.). Titanium dioxide (TiO2) is the most popular material used in heterogeneous photocatalysis due to its excellent properties, such as high stability, chemical inertness, non-toxicity and low cost. It is well known that morphology and microstructure of TiO2 significantly influence the photocatalytic activity. This characteristics as well as other physical and structural properties of photocatalysts, i.e., specific surface area or density of crystalline defects, could be controlled by preparation route. In this regard, TiO2 particles can be obtained by sol-gel, hydrothermal, sonochemical methods, chemical vapour deposition and alternatively, by ionothermal synthesis using ionic liquids (ILs). In the TiO2 particles synthesis ILs may play a role of a solvent, soft template, reagent, agent promoting reduction of the precursor or particles stabilizer during synthesis of inorganic materials. In this work, the effect of the ILs anion type on morphology and photoactivity of TiO2 is presented. The preparation of TiO2 microparticles with spherical structure was successfully achieved by solvothermal method, using tetra-tert-butyl orthotitatane (TBOT) as the precursor. The reaction process was assisted by an ionic liquids 1-butyl-3-methylimidazolium bromide [BMIM][Br], 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF4] and 1-butyl-3-methylimidazolium haxafluorophosphate [BMIM][PF6]. Various molar ratios of all ILs to TBOT (IL:TBOT) were chosen. For comparison, reference TiO2 was prepared using the same method without IL addition. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Brenauer-Emmett-Teller surface area (BET), NCHS analysis, and FTIR spectroscopy were used to characterize the surface properties of the samples. The photocatalytic activity was investigated by means of phenol photodegradation in the aqueous phase as a model pollutant, as well as formation of hydroxyl radicals based on detection of fluorescent product of coumarine hydroxylation. The analysis results showed that the TiO2 microspheres had spherical structure with the diameters ranging from 1 to 6 µm. The TEM micrographs gave a bright observation of the samples in which the particles were comprised of inter-aggregated crystals. It could be also observed that the IL-assisted TiO2 microspheres are not hollow, which provides additional information about possible formation mechanism. Application of the ILs results in rise of the photocatalytic activity as well as BET surface area of TiO2 as compared to pure TiO2. The results of the formation of 7-hydroxycoumarin indicated that the increased amount of ·OH produced at the surface of excited TiO2 for samples TiO2_ILs well correlated with more efficient degradation of phenol. NCHS analysis showed that ionic liquids remained on the TiO2 surface confirming structure directing role of that compounds.

Keywords: heterogeneous photocatalysis, IL-assisted synthesis, ionic liquids, TiO2

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Authors: Boor Singh Lalia, Yarjan Abdul Samad, Raed Hashaikeh

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Three different kinds of solid polymer electrolytes were prepared using polyethylene oxide (PEO) as a base polymer, networked cellulose (NC) as a physical support and LiClO4 as a conductive salt for the electrolytes. Networked cellulose, a modified form of cellulose, is a biodegradable and environmentally friendly additive which provides a strong fibrous networked support for structural stability of the electrolytes. Although the PEO/NC/LiClO4 electrolyte retains its structural integrity and mechanical properties at 100oC as compared to pristine PEO-based polymer electrolytes, it suffers from poor ionic conductivity. To improve the room temperature conductivity of the electrolyte, PEO is replaced by the polyethylene glycol (PEG) which is a liquid phase that provides high mobility for Li+ ions transport in the electrolyte. PEG/NC/LiClO4 shows improvement in ionic conductivity compared to PEO/NC/LiClO4 at room temperature, but it is brittle and tends to form cracks during processing. An advanced solid polymer electrolyte with optimum ionic conductivity and mechanical properties is developed by using a ternary system: TEGDME/PEO/NC+LiClO4. At room temperature, this electrolyte exhibits an ionic conductivity to the order of 10-5 S/cm, which is very high compared to that of the PEO/LiClO4 electrolyte. Pristine PEO electrolytes start melting at 65 °C and completely lose its mechanical strength. Dynamic mechanical analysis of TEGDME: PEO: NC (70:20:10 wt%) showed an improvement of storage modulus as compared to the pristine PEO in the 60–120 °C temperature range. Also, with an addition of NC, the electrolyte retains its mechanical integrity at 100 oC which is beneficial for Li-ion battery operation at high temperatures. Differential scanning calorimetry (DSC) and thermal gravimetry analysis (TGA) studies revealed that the ternary polymer electrolyte is thermally stable in the lithium ion battery operational temperature range. As-prepared polymer electrolyte was used to assemble LiFePO4/ TEGDME/PEO/NC+LiClO4/Li half cells and their electrochemical performance was studied via cyclic voltammetry and charge-discharge cycling.

Keywords: solid polymer electrolyte, ionic conductivity, mechanical properties, lithium ion batteries, cyclic voltammetry

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

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Solvent recovery process is receiving utmost attention in recent year due to the scarcity of natural resource and consciousness of circular economy in chemical and pharmaceutical manufacturing process. Solvent dehydration process is one of the important process to recover and to purify the solvent for reuse. Due to the complexity of solvent waste or wastewater effluent produced in pharmaceutical industry resulting the wastewater treatment process become complicated, thus an alternative solution is to recover the valuable solvent in solvent waste. To treat solvent waste and to upgrade solvent purity, membrane pervaporation process is shown to be a promising technology due to the energy intensive and low footprint advantages. Ceramic membrane is adopted as solvent dehydration membrane owing to the chemical and thermal stability properties as compared to polymeric membrane. NaA zeolite membrane is generally used as solvent dehydration process because of its narrow and distinct pore size and high hydrophilicity. NaA zeolite membrane has been mainly applied in alcohol dehydration in fermentation process. At this stage, the membrane performance exhibits high separation factor with low flux using tubular ceramic membrane. Thus, defect free and ultrathin NaA membrane should be developed to increase water flux. Herein, we report a simple preparation protocol to prepare ultrathin NaA zeolite membrane supported on tubular ceramic membrane by controlling the seed size synthesis, seeding methods and conditions, ceramic substrate surface pore size selection and secondary growth conditions. The microstructure and morphology of NaA zeolite membrane will be examined and reported. Moreover, the membrane separation performance and stability will also be reported in isopropanol dehydration, ketone dehydration and ester dehydration particularly for the application in pharmaceutical industry.

Keywords: ceramic membrane, NaA zeolite, pharmaceutical industry, solvent recovery

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Authors: Rafiuddin

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Composite solid electrolyte of the salt and oxide type is an effective approach to improve the ionic conductivity in low and intermediate temperature regions. The conductivity enhancement in the composites occurs via interfaces. Because of their high ionic conduction, composite electrolytes have wide applications in different electrochemical devices such as solid-state batteries, solid oxide fuel cells, and electrochemical cells. In this work, a series of novel (1‒x) (CdI2‒Ag2CrO4)‒xAl2O3 composite solid electrolytes has been synthesized. The prepared materials were characterized by X‒ray diffraction, differential thermal analysis, and AC impedance spectroscopy. The impedance spectra show single semicircle representing the simultaneous contribution of grain and grain boundary. The conductivity increased with the increase of Al2O3 content and shows the maximum conductivity (σ= 0.0012 S cm‒1) for 30% of Al2O3 content at 30 ℃.

Keywords: composite solid electrolyte, X-ray diffraction, Impedance spectroscopy, ionic conductivity

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Authors: Najwa Othman, Norhidayah Suleiman, Gun Hean Chong

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

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

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Authors: Asep Sukohar, Ramadhan Triyandi, Muhammad Iqbal, Sahidin, Suharyani

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Introduction: Resveratrol is a class of bioactive chemicals found in melinjo, which has a wide range of biological actions. The purpose of this study is to determine the linarin content of the melinjo fraksi by using preparative-high-performance liquid chromatography (prep-HPLC). Method: Extraction used the soxhletation method with 96% ethanol solvent. Fractionation used ethyl acetate and ethanol in a ratio of 1:1. Tracing of linarin compound used prep-HPLC with a mobile phase ratio of distilled water: methanol (55: 45, v/v). The presence of linarin was detected using a wavelength of 215 nm. Fourier Transform Infrared (FTIR) was used to identify the functional groups of compound. Result: The retention time required to elute the ethyl acetate fraction was 2.601 minutes. Compound separation identification using Fourier Transform Infrared Spectroscopy - Quest Attenuated Total Reflectance (FTIR - QATR) has a similarity value range with standards from 0 to 1000. The elution results of the ethyl acetate fraction have similar values with the standard compounds linarin (668), resveratrol (578), and catechin (455). Conclusion: Tracing for active compound in the ethyl acetate fraction of Gnetum Gnemon L. using prep-HPLC showed a strong suspicion of the presence of linarin compound.

Keywords: Gnetum gnemon L., linarin, prep-HPLC, fraction ethyl acetate

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Authors: Fangyan Li, Lin Min Lee, Hui Zhu Peh, Shoet Harn Chan

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Advantame, a derivative of aspartame, is the latest addition to a family of low caloric and high potent dipeptide sweeteners which include aspartame, neotame and alitame. The use of advantame as a high-intensity sweetener in food was first accepted by Food Standards Australia New Zealand in 2011 and subsequently by US and EU food authorities in 2014, with the results from toxicity and exposure studies showing advantame poses no safety concern to the public at regulated levels. To our knowledge, currently there is barely any detailed information on the analytical method of advantame in food matrix, except for one report published in Japanese, stating a high performance liquid chromatography (HPLC) and liquid chromatography/ mass spectrometry (LC-MS) method with a detection limit at ppm level. However, the use of acid in sample preparation and instrumental analysis in the report raised doubt over the reliability of the method, as there is indication that stability of advantame is compromised under acidic conditions. Besides, the method may not be suitable for analyzing food matrices containing advantame at low ppm or sub-ppm level. In this presentation, a simple, specific and sensitive method for the determination of advantame in food is described. The method involved extraction with water and clean-up via solid phase extraction (SPE) followed by detection using liquid chromatography tandem mass spectrometry (LC-MS/MS) in negative electrospray ionization mode. No acid was used in the entire procedure. Single laboratory validation of the method was performed in terms of linearity, precision and accuracy. A low detection limit at ppb level was achieved. Satisfactory recoveries were obtained using spiked samples at three different concentration levels. This validated method could be used in the routine inspection of the advantame level in food.

Keywords: advantame, food, LC-MS/MS, sweetener

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Authors: Malek Miladi, Miguel Vegara, Maria Perez-Infantes, Khaled Mohamed Ramadan, Antonio Ruiz-Canales, Damaris Nunez-Gomez

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Coffee is the second consumed commodity worldwide, yet it also generates colossal waste. Proper management of coffee waste is proposed by converting them into products with higher added value to achieve sustainability of the economic and ecological footprint and protect the environment. Based on this, a study looking at the recovery of coffee waste is becoming more relevant in recent decades. Spent coffee grounds (SCG's) resulted from brewing coffee represents the major waste produced among all coffee industry. The fact that SCGs has no economic value be abundant in nature and industry, do not compete with agriculture and especially its high oil content (between 7-15% from its total dry matter weight depending on the coffee varieties, Arabica or Robusta), encourages its use as a sustainable feedstock for bio-oil production. The bio-oil extraction is a crucial step towards biodiesel production by the transesterification process. However, conventional methods used for oil extraction are not recommended due to their high consumption of energy, time, and generation of toxic volatile organic solvents. Thus, finding a sustainable, economical, and efficient extraction technique is crucial to scale up the process and to ensure more environment-friendly production. Under this perspective, the aim of this work was the statistical study to know an efficient strategy for oil extraction by n-hexane using indirect sonication. The coffee waste mixed Arabica and Robusta, which was used in this work. The temperature effect, sonication time, and solvent-to-solid ratio on the oil yield were statistically investigated as dependent variables by Central Composite Rotatable Design (CCRD) 23. The results were analyzed using STATISTICA 7 StatSoft software. The CCRD showed the significance of all the variables tested (P < 0.05) on the process output. The validation of the model by analysis of variance (ANOVA) showed good adjustment for the results obtained for a 95% confidence interval, and also, the predicted values graph vs. experimental values confirmed the satisfactory correlation between the model results. Besides, the identification of the optimum experimental conditions was based on the study of the surface response graphs (2-D and 3-D) and the critical statistical values. Based on the CCDR results, 29 ºC, 56.6 min, and solvent-to-solid ratio 16 were the better experimental conditions defined statistically for coffee waste oil extraction using n-hexane as solvent. In these conditions, the oil yield was >9% in all cases. The results confirmed the efficiency of using an ultrasound bath in extracting oil as a more economical, green, and efficient way when compared to the Soxhlet method.

Keywords: coffee waste, optimization, oil yield, statistical planning

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Authors: X. Han, S. Duan, C. Liu, C. Zhou, W. Zhu, L. Kong

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The ionic imprinting technique refers to the three-dimensional rigid structure with the fixed pore sizes, which was formed by the binding interactions of ions and functional monomers and used ions as the template, it has a high level of recognition to the ionic template. The preparation of monolithic column by the in-situ polymerization need to put the compound of template, functional monomers, cross-linking agent and initiating agent into the solution, dissolve it and inject to the column tube, and then the compound will have a polymerization reaction at a certain temperature, after the synthetic reaction, we washed out the unread template and solution. The monolithic columns are easy to prepare, low consumption and cost-effective with fast mass transfer, besides, they have many chemical functions. But the monolithic columns have some problems in the practical application, such as low-efficiency, quantitative analysis cannot be performed accurately because of the peak shape is wide and has tailing phenomena; the choice of polymerization systems is limited and the lack of theoretical foundations. Thus the optimization of components and preparation methods is an important research direction. During the preparation of ionic imprinted monolithic columns, pore-forming agent can make the polymer generate the porous structure, which can influence the physical properties of polymer, what’ s more, it can directly decide the stability and selectivity of polymerization reaction. The compounds generated in the pre-polymerization reaction could directly decide the identification and screening capabilities of imprinted polymer; thus the choice of pore-forming agent is quite critical in the preparation of imprinted monolithic columns. This article mainly focuses on the research that when using different pore-forming agents, the impact of zinc ion imprinted monolithic column on the enrichment performance of zinc ion.

Keywords: high performance liquid chromatography (HPLC), ionic imprinting, monolithic column, pore-forming agent

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Authors: Chris Miskelly, Eoin Cunningham, Beatrice Smyth, John. D. Holbrey, Gosia Swadzba-Kwasny, Emily L. Byrne, Yoan Delavoux, Mantian Li.

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Recently, the use of ionic liquids (ILs) for the preparation of lignocellulose derived cellulosic materials as alternatives to petrochemical feedstocks has been the focus of considerable research interest. While the technical viability of IL-based lignocellulose treatment methodologies has been well established, the high cost of reagents inhibits commercial feasibility. This work aimed to assess the technoeconomic viability of the preparation of cellulose rich materials (CRMs) using protic ionic liquids (PILs) synthesized from low cost alkylamines and sulphuric acid. For this purpose, the tertiary alkylamines, triethylamine, and dimethylbutylamine were selected. Bulk scale production cost of the synthesized PILs, triethylammonium hydrogen sulphate and dimetheylbutylammonium hydrogen sulphate, was reported as $0.78 kg-1 to $1.24 kg-1. CRMs were prepared through the treatment of common wheat (Triticum aestivum) straw with these PILs. By controlling treatment parameters, CRMs with a cellulose content of ≥ 80 wt% were prepared. This was achieved using a T. aestivum straw to PIL loading ratio of 1:15 w/w, a treatment duration of 180 minutes, and ethanol as a cellulose antisolvent. Infrared spectra data and decreased onset degradation temperature of CRMs (ΔTONSET ~ 70 °C) suggested the formation of cellulose sulphate esters during treatment. Chemical derivatisation can aid the dispersion of prepared CRMs in non-polar polymer/ composite matrices, but act as a barrier to thermal processing at temperatures above 150 °C. It was also shown that treatment increased the crystallinity of CRMs (ΔCrI ~ 40 %) without altering the native crystalline structure or crystallite size (~ 2.6 nm) of cellulose; peaks associated with the cellulose I crystalline planes (110), (200), and (004) were observed at Bragg angles 16.0 °, 22.5 ° and 35.0 ° respectively. This highlighted the inability of assessed PILs to dissolve crystalline cellulose and was attributed to the high acidity (pKa ~ - 1.92 to - 6.42) of sulphuric acid derived anions. Electron micrographs revealed that the stratified multilayer tissue structure of untreated T. aestivum straw was significantly modified during treatment. T. aestivum straw particles were disassembled during treatment, with prepared CRMs adopting a golden-brown film-like appearance. This work demonstrated the degradation of non-cellulosic fractions of lignocellulose without dissolution of cellulose. It is the first to report on the derivatisation of cellulose during treatment with protic hydrogen sulphate ionic liquids, and the potential implications of this with reference to biopolymer feedstock preparation.

Keywords: cellulose, extraction, protic ionic liquids, esterification, thermal stability, waste valorisation, biopolymer feedstock

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Authors: Seyedeh Bahar Hashemi, Alireza Rahimi, Mehdi Arjmand

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Food is the source of energy and growth through the breakdown of its vital components and plays a vital role in human health and nutrition. Many natural compounds found in plant and animal materials play a special role in biological systems and the origin of many such compounds directly or indirectly is algae. Algae is an enormous source of polysaccharides and have gained much interest in human flourishing. In this study, algae biomass extraction is conducted using deep eutectic-based solvents (NADES) and Ultrasound-assisted extraction (UAE). The aim of this research is to extract bioactive compounds including total carotenoid, antioxidant activity, and polyphenolic contents. For this purpose, the influence of three important extraction parameters namely, biomass-to-solvent ratio, temperature, and time are studied with respect to their impact on the recovery of carotenoids, and phenolics, and on the extracts’ antioxidant activity. Here we employ the Response Surface Methodology for the process optimization. The influence of the independent parameters on each dependent is determined through Analysis of Variance. Our results show that Ultrasound-assisted extraction (UAE) for 50 min is the best extraction condition, and proline:lactic acid (1:1) and choline chloride:urea (1:2) extracts show the highest total phenolic contents (50.00 ± 0.70 mgGAE/gdw) and antioxidant activity [60.00 ± 1.70 mgTE/gdw, 70.00 ± 0.90 mgTE/gdw in 2.2-diphenyl-1-picrylhydrazyl (DPPH), and 2.2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS)]. Our results confirm that the combination of UAE and NADES provides an excellent alternative to organic solvents for sustainable and green extraction and has huge potential for use in industrial applications involving the extraction of bioactive compounds from algae. This study is among the first attempts to optimize the effects of ultrasonic-assisted extraction, ultrasonic devices, and deep natural eutectic point and investigate their application in bioactive compounds extraction from algae. We also study the future perspective of ultrasound technology which helps to understand the complex mechanism of ultrasonic-assisted extraction and further guide its application in algae.

Keywords: natural deep eutectic solvents, ultrasound-assisted extraction, algae, antioxidant activity, phenolic compounds, carotenoids

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Authors: S. A. A. Nabeela Nasreen, S. Sundarrajan, S. A. Syed Nizar, Seeram Ramakrishna

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Metal-organic frameworks (MOFs) have attracted considerable interest due to its diverse pore size tunability, fascinating topologies and extensive uses in fields such as catalysis, membrane separation, chemical sensing, etc. Zeolitic imidazolate frameworks (ZIFs) are a class of MOF with porous crystals containing extended three-dimensional structures of tetrahedral metal ions (e.g., Zn) bridged by Imidazolate (Im). Selected ZIFs are used to separate solvent/solvent mixtures. A layer by layer formation of the nanocomposite of Zinc oxide (ZnO) and ZIF on a ceramic support using a solvothermal method was engaged and tested for target solvent/solvent separation. Metal oxide layer was characterized by XRD, SEM, and TEM to confirm the smooth and continuous coating for the separation process. The chemical composition of ZIF films was studied by using X-Ray absorption near-edge structure (XANES) spectroscopy. The obtained ceramic tube with metal oxide and ZIF layer coating were tested for its packing density, thickness, distribution of seed layers and variation of permeation rate of solvent mixture (isopropyl alcohol (IPA)/methyl isobutyl ketone (MIBK). Pervaporation technique was used for the separation to achieve a high permeation rate with separation ratio of > 99.5% of the solvent mixture.

Keywords: metal oxide, membrane, pervaporation, solvothermal, ZIF

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Authors: Maxim S. Botalov, Svetlana М. Titova, Denis V. Smyshlyaev, Grigory M. Bunkov, Evgeny V. Kirillov, Sergey V. Kirillov, Maxim A. Mashkovtsev, Vladimir N. Rychkov

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In uranium production, in-situ leaching (ISL) with its relatively low cost has become an important technology. As the orebody containing uranium most often contains a considerable value of other metals, particularly rare earth metals it has rendered feasible to recover the REM from the barren ISL solutions, from which the major uranium content has been removed. Ural Federal University (UrFU, Ekaterinburg, Russia) have performed joint research on the development of industrial technologies for the extraction of REM and Scandium compounds from Uranium ISL solutions. Leaching experiments at UrFU have been supported with multicomponent solution model. The experimental work combines solvent extraction with advanced ion exchange methodology in a pilot facility capable of treating 500 kg/hr of solids. The pilot allows for the recovery of a 99% concentrate of scandium oxide and collective concentrate with over 50 % REM content, with further recovery of heavy and light REM concentrates (99%).

Keywords: extraction, ion exchange, rare earth elements, scandium

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Authors: Cesar Torres, Robert Briber, Nam Sun Wang

Abstract:

Eye drops are the most commonly used treatment for short-term and long-term ophthalmic diseases. However, eye drops could deliver only about 5% of the functional ingredients contained in a burst dosage. To address the limitations of eye drops, the use of therapeutic contact lenses has been introduced. Drug-loaded contact lenses provide drugs a longer residence time in the tear film and hence, decrease the potential risk of side effects. Nevertheless, a major limitation of contact lenses as drug delivery devices is that most of the drug absorbed is released within the first few hours. This fact limits their use for extended release. The present study demonstrates the application of long-alkyl chain ionic surfactants on extending drug release kinetics from commercially available silicone hydrogel contact lenses. In vitro release experiments were carried by immersing drug-containing contact lenses in phosphate buffer saline at physiological pH. The drug concentration as a function of time was monitored using ultraviolet-visible spectroscopy. The results of the study demonstrate that release kinetics is dependent on the ionic surfactant weight percent in the contact lenses, and on the length of the hydrophobic alkyl chain of the ionic surfactants. The use of ionic surfactants in contact lenses can extend the delivery of drugs from a few hours to a few weeks, depending on the physicochemical properties of the drugs. Contact lenses embedded with ionic surfactants could be potential biomaterials to be used for extended drug delivery and in the treatment of ophthalmic diseases. However, ocular irritation and toxicity studies would be needed to evaluate the safety of the approach.

Keywords: contact lenses, drug delivery, controlled release, ionic surfactant

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Authors: Alexandra C. Blaga, Dan Caşcaval, Alexandra Tucaliuc, Madalina Poştaru, Anca I. Galaction

Abstract:

Amino acids are valuable chemical products used in in human foods, in animal feed additives and in the pharmaceutical field. Recently, there has been a noticeable rise of amino acids utilization throughout the world to include their use as raw materials in the production of various industrial chemicals: oil gelating agents (amino acid-based surfactants) to recover effluent oil in seas and rivers and poly(amino acids), which are attracting attention for biodegradable plastics manufacture. The amino acids can be obtained by biosynthesis or from protein hydrolysis, but their separation from the obtained mixtures can be challenging. In the last decades there has been a continuous interest in developing processes that will improve the selectivity and yield of downstream processing steps. The liquid-liquid extraction of amino acids (dissociated at any pH-value of the aqueous solutions) is possible only by using the reactive extraction technique, mainly with extractants of organophosphoric acid derivatives, high molecular weight amines and crown-ethers. The purpose of this study was to analyse the separation of nine amino acids of acidic character (l-aspartic acid, l-glutamic acid), basic character (l-histidine, l-lysine, l-arginine) and neutral character (l-glycine, l-tryptophan, l-cysteine, l-alanine) by reactive extraction with di-(2-ethylhexyl)phosphoric acid (D2EHPA) dissolved in butyl acetate. The results showed that the separation yield is controlled by the pH value of the aqueous phase: the reactive extraction of amino acids with D2EHPA is possible only if the amino acids exist in aqueous solution in their cationic forms (pH of aqueous phase below the isoeletric point). The studies for individual amino acids indicated the possibility of selectively separate different groups of amino acids with similar acidic properties as a function of aqueous solution pH-value: the maximum yields are reached for a pH domain of 2–3, then strongly decreasing with the pH increase. Thus, for acidic and neutral amino acids, the extraction becomes impossible at the isolelectric point (pHi) and for basic amino acids at a pH value lower than pHi, as a result of the carboxylic group dissociation. From the results obtained for the separation from the mixture of the nine amino acids, at different pH, it can be observed that all amino acids are extracted with different yields, for a pH domain of 1.5–3. Over this interval, the extract contains only the amino acids with neutral and basic character. For pH 5–6, only the neutral amino acids are extracted and for pH > 6 the extraction becomes impossible. Using this technique, the total separation of the following amino acids groups has been performed: neutral amino acids at pH 5–5.5, basic amino acids and l-cysteine at pH 4–4.5, l-histidine at pH 3–3.5 and acidic amino acids at pH 2–2.5.

Keywords: amino acids, di-(2-ethylhexyl) phosphoric acid, reactive extraction, selective extraction

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Authors: Shoji Mori, Kunito Okuyama

Abstract:

Annular two phase flow is encountered in many industrial equipments, including flow near nuclear fuel rods in boiling water reactor (BWR). Especially, disturbance waves play important roles in the pressure drop, the generation of entrainments, and the dryout of the liquid film. Therefore, it is important to clarify the behavior of disturbance waves and base film. However, most of the previous studies have been performed under atmospheric pressure conditions that provides the properties of liquid and gas which are significantly different from those of a BWR. Therefore, the effect of properties in gas and liquid on liquid film characteristics should be clarified. In this paper we focus on the effect of gas-liquid density ratio on liquid film thickness characteristics. The experiments have been conducted at four density ratio conditions (ρL/ρG =763, 451, 231, and 31). As a result, it is found that and interfacial shear stress collapse not only tF ave but also tF max and tF min successfully under the same liquid mass flow rate conditions irrespective of ρL/ρG, and moreover a non-dimensional parameter tends to collapse tF max，tF ave，and tF min in the wide range of experimental conditions (ρL/ρG：31～763，We：10～1800，ReL:500 ～ 2200).

Keywords: two phase flow, liquid film, annular flow, disturbance wave

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Authors: Wei Quan, Liu Chao, Mohammed N. Afsar

Abstract:

The dielectric properties and ionic conductivity of novel "ceramic state" polymer electrolytes for high capacity lithium battery are characterized by radio-frequency and Microwave methods in two broad frequency ranges from 50 Hz to 20 KHz and 4 GHz to 40 GHz. This innovative solid polymer electrolyte which is highly ionic conductive (10-3 S/cm at room temperature) from -40 oC to +150 oC and can be used in any battery application. Such polymer exhibits properties more like a ceramic rather than polymer. The various applied measurement methods produced accurate dielectric results for comprehensive analysis of electrochemical properties and ion transportation mechanism of this newly invented polymer electrolyte. Two techniques and instruments employing air gap measurement by capacitance bridge and inwave guide measurement by vector network analyzer are applied to measure the complex dielectric spectra. The complex dielectric spectra are used to determine the complex alternating current electrical conductivity and thus the ionic conductivity.

Keywords: polymer electrolyte, dielectric permittivity, lithium battery, ionic relaxation, microwave measurement

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Authors: Surya Chandra Tiwari, Kamal Kishore Pant, Sreedevi Upadhyayula

Abstract:

CO2 capture using benign cost-effective solvents is an essential unit operation not only in the process industry for CO2 separation and recovery from industrial off-gas streams but also for direct capture from air to clean the environment. Several solvents are identified, by researchers, with high CO2 capture efficiency due to their favorable chemical and physical properties, interaction mechanism with CO2, and low regeneration energy cost. However, N-Methyldiethanolamine (MDEA) is the most frequently used solvent for CO2 capture with promoters such as piperazine (Pz) and monoethanolamine (MEA). These promoters have several issues such as low thermal stability, heat-stable salt formation, and being highly degradable. Therefore, new class promoters need to be used to overcome these issues. Functionalized ionic liquids (FILs) have the potential to overcome these limitations. Hence, in this work, four different new class functionalized ionic liquids (FILs) were used as promoters and determined their effectivity toward enhancement of the CO2 absorption performance. The CO2 absorption is performed at different pressure (2 bar, 4.4 bar, and 7 bar) and different temperature (303, 313, and 323K). The results confirmed that CO2 loading increases around 18 to 22% after 5wt% FILs blended in the MDEA. It was noticed that the CO2 loading increases with increasing pressure and decreases with increasing temperature for all absorbents systems. Further, the absorption kinetics was determined, and results showed that all the FILs provide an excellent absorption rate enhancement. Additionally, for the interaction mechanism study, 13C NMR analysis was performed for the blend aqueous MDEA-CO2 system. The results suggested that the FILs blend MDEA system produced a high amount of carbamates and bicarbonates during CO2 absorption, which further decreases with increasing temperature. Eventually, regeneration energy was calculated, and results confirmed that the energy heat duty penalty was lower in the [TETAH][Im] blend MDEA system. Overall, [TETAH][Pz], [TETAH][Im], [DETAH][Im] and [DETAH][Tz] showed the promising ability as promoters to enhance CO2 capturing performance of MDEA.

Keywords: CO2 capture, interaction mechanism, kinetics, Ionic liquids

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Authors: Yaseen Muhammad, Zhenxia Zhao, Zhangfa Tong

Abstract:

A key problem with hydrodesulfurization (HDS) process of fuel oils is the application of severe operating conditions. In this study, we proposed the catalytic HDS of dibenzothiophene (DBT) integrated with ionic liquids (ILs) application at mild temperature and pressure over low loaded (0.5 wt.%) Pd promoted Co-Mo@Al₂O₃ and Ni-Mo@Al₂O₃ catalysts. Among the thirteen ILs tested, [BMIM]BF₄, [(CH₃)₄N]Cl, [EMIM]AlCl₄, and [(C₈H₁₇)(C₃H₇)₃P]Br enhanced the catalytic HDS efficiency while the latest ranked the top of activity list as confirmed by DFT studies as well. Experimental results revealed that Pd incorporation greatly enhanced the HDS activity of classical Co or Ni based catalysts. At mild optimized experimental conditions of 1 MPa H₂ pressure, 120 oC, IL:oil ratio of 1:3 and 4 h reaction time, the % DBT conversion (21 %) by Ni-Mo@Al₂O₃ was enhanced to 69 % (over Pd-Ni-Mo@ Al₂O₃) using [(C₈H₁₇) (C₃H₇)₃P]Br. The fresh and spent catalysts were characterized for textural properties using XPS, SEM, EDX, XRD and BET surface area techniques. An overall catalytic HDS activity followed the order of: Pd-Ni-Mo@Al₂O₃ > Pd-Co-Mo@Al₂O₃ > Ni-Mo@Al₂O₃ > Co-Mo@Al₂O₃. [(C₈H₁₇) (C₃H₇)₃P]Br.could be recycled four times with minimal decrease in HDS activity. Reaction products were analyzed by GC-MS which helped in proposing reaction mechanism for the IL coupled HDS process. The present approach attributed to its cost-effective nature, ease of operation with less mechanical requirements in terms of mild operating conditions, and high efficiency could be deemed as an alternative approach for the HDS of DBT on industrial level applications.

Keywords: DFT simulation, GC-MS and reaction mechanism, Ionic liquid coupled HDS of DBT, low Pd loaded catalyst, mild operating condition

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

Abstract:

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: Deepak Kumar, Jahangeer, Brijesh Kumar Yadav, Shashi Mathur

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In-situ remediation is a technique which can remediate either surface or groundwater at the site of contamination. In the present study, simulation optimization approach has been used to develop management strategy for remediating LNAPL (Light Non-Aqueous Phase Liquid) contaminated aquifers. Benzene, toluene, ethyl benzene and xylene are the main component of LNAPL contaminant. Collectively, these contaminants are known as BTEX. In in-situ bioremediation process, a set of injection and extraction wells are installed. Injection wells supply oxygen and other nutrient which convert BTEX into carbon dioxide and water with the help of indigenous soil bacteria. On the other hand, extraction wells check the movement of plume along downstream. In this study, optimal design of the system has been done using PSO (Particle Swarm Optimization) algorithm. A comprehensive management strategy for pumping of injection and extraction wells has been done to attain a maximum allowable concentration of 5 ppm and 4.5 ppm. The management strategy comprises determination of pumping rates, the total pumping volume and the total running cost incurred for each potential injection and extraction well. The results indicate a high pumping rate for injection wells during the initial management period since it facilitates the availability of oxygen and other nutrients necessary for biodegradation, however it is low during the third year on account of sufficient oxygen availability. This is because the contaminant is assumed to have biodegraded by the end of the third year when the concentration drops to a permissible level.

Keywords: groundwater, in-situ bioremediation, light non-aqueous phase liquid, BTEX, particle swarm optimization

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Authors: A. B. Bazaralieva, A. A. Turgumbayeva

Abstract:

The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: Allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Velasco-Rendón María Del Carmen, Cuéllar-Bermúdez Sara Paulina, Parra-Saldívar Roberto

Abstract:

Phycocyanin is a blue pigment protein with fluorescent activity produced by cyanobacteria. It has been recently studied to determine its anticancer, antioxidant and antiinflamatory potential. Since 2014 it was approved as a Generally Recognized As Safe (GRAS) proteic pigment for the food industry. Therefore, phycocyanin shows potential for the food, nutraceutical, pharmaceutical and diagnostics industry. Conventional phycocyanin extraction includes buffer solutions and ammonium sulphate followed by chromatography or ATPS for protein separation. Therefore, further purification steps are time-requiring, energy intensive and not suitable for scale-up processing. This work presents an alternative to conventional methods that also allows large scale application with commercially available equipment. The extraction was performed by exposing the dry biomass to mechanical cavitation and salting out with NaCl to use an edible reagent. Also, isoelectric point precipitation was used by addition of HCl and neutralization with NaOH. The results were measured and compared in phycocyanin concentration, purity and extraction yield. Results showed that the best extraction condition was the extraction by salting out with 0.20 M NaCl after 30 minutes cavitation, with a concentration in the supernatant of 2.22 mg/ml, a purity of 3.28 and recovery from crude extract of 81.27%. Mechanical cavitation presumably increased the solvent-biomass contact, making the crude extract visibly dark blue after centrifugation. Compared to other systems, our process has less purification steps, similar concentrations in the phycocyanin-rich fraction and higher purity. The contaminants present in our process edible NaCl or low pHs that can be neutralized. It also can be adapted to a semi-continuous process with commercially available equipment. This characteristics make this process an appealing alternative for phycocyanin extraction as a pigment for the food industry.

Keywords: extraction, phycocyanin, precipitation, scale-up

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