Solvent Extraction and Spectrophotometric Determination of Palladium(II) Using P-Methylphenyl Thiourea as a Complexing Agent

A precise, sensitive, rapid and selective method for the solvent extraction, spectrophotometric determination of palladium(II) using para-methylphenyl thiourea (PMPT) as an extractant is developed. Palladium(II) forms yellow colored complex with PMPT which shows an absorption maximum at 300 nm. The colored complex obeys Beer’s law up to 7.0 µg ml-1 of palladium. The molar absorptivity and Sandell’s sensitivity were found to be 8.486 x 103 l mol-1cm-1 and 0.0125 μg cm-2 respectively. The optimum conditions for the extraction and determination of palladium have been established by monitoring the various experimental parameters. The precision of the method has been evaluated and the relative standard deviation has been found to be less than 0.53%. The proposed method is free from interference from large number of foreign ions. The method has been successfully applied for the determination of palladium from alloy, synthetic mixtures corresponding to alloy samples.

The Mechanism Study of Degradative Solvent Extraction of Biomass by Liquid Membrane-Fourier Transform Infrared Spectroscopy

Degradative solvent extraction is the method developed for biomass upgrading by dewatering and fractionation of biomass under the mild condition. However, the conversion mechanism of the degradative solvent extraction method has not been fully understood so far. The rice straw was treated in 1-methylnaphthalene (1-MN) at a different solvent-treatment temperature varied from 250 to 350 oC with the residence time for 60 min. The liquid membrane-Fourier Transform Infrared Spectroscopy (FTIR) technique is applied to study the processing mechanism in-depth without separation of the solvent. It has been found that the strength of the oxygen-hydrogen stretching  (3600-3100 cm-1) decreased slightly with increasing temperature in the range of 300-350 oC. The decrease of the hydroxyl group in the solvent soluble suggested dehydration reaction taking place between 300 and 350 oC. FTIR spectra in the carbonyl stretching region (1800-1600 cm-1) revealed the presence of esters groups, carboxylic acid and ketonic groups in the solvent-soluble of biomass. The carboxylic acid increased in the range of 200 to 250 oC and then decreased. The prevailing of aromatic groups showed that the aromatization took place during extraction at above 250 oC. From 300 to 350 oC, the carbonyl functional groups in the solvent-soluble noticeably decreased. The removal of the carboxylic acid and the decrease of esters into the form of carbon dioxide indicated that the decarboxylation reaction occurred during the extraction process.

Nanofluid-Based Emulsion Liquid Membrane for Selective Extraction and Separation of Dysprosium

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

Optimization of Samarium Extraction via Nanofluid-Based Emulsion Liquid Membrane Using Cyanex 272 as Mobile Carrier

Samarium as a rare-earth element is playing a growing important role in high technology. Traditional methods for extraction of rare earth metals such as ion exchange and solvent extraction have disadvantages of high investment and high energy consumption. Emulsion liquid membrane (ELM) as an improved solvent extraction technique is an effective transport method for separation of various compounds from aqueous solutions. In this work, the extraction of samarium from aqueous solutions by ELM was investigated using response surface methodology (RSM). The organic membrane phase of the ELM was a nanofluid consisted of multiwalled carbon nanotubes (MWCNT), Span80 as surfactant, Cyanex 272 as mobile carrier, and kerosene as base fluid. 1 M nitric acid solution was used as internal aqueous phase. The effects of the important process parameters on samarium extraction were investigated, and the values of these parameters were optimized using the Central Composition Design (CCD) of RSM. These parameters were the concentration of MWCNT in nanofluid, the carrier concentration, and the volume ratio of organic membrane phase to internal phase (Roi). The three-dimensional (3D) response surfaces of samarium extraction efficiency were obtained to visualize the individual and interactive effects of the process variables. A regression model for % extraction was developed, and its adequacy was evaluated. The result shows that % extraction improves by using MWCNT nanofluid in organic membrane phase and extraction efficiency of 98.92% can be achieved under the optimum conditions. In addition, demulsification was successfully performed and the recycled membrane phase was proved to be effective in the optimum condition.

Performance Study of Neodymium Extraction by Carbon Nanotubes Assisted Emulsion Liquid Membrane Using Response Surface Methodology

The high purity rare earth elements (REEs) have been vastly used in the field of chemical engineering, metallurgy, nuclear energy, optical, magnetic, luminescence and laser materials, superconductors, ceramics, alloys, catalysts, and etc. Neodymium is one of the most abundant rare earths. By development of a neodymium–iron–boron (Nd–Fe–B) permanent magnet, the importance of neodymium has dramatically increased. Solvent extraction processes have many operational limitations such as large inventory of extractants, loss of solvent due to the organic solubility in aqueous solutions, volatilization of diluents, etc. One of the promising methods of liquid membrane processes is emulsion liquid membrane (ELM) which offers an alternative method to the solvent extraction processes. In this work, a study on Nd extraction through multi-walled carbon nanotubes (MWCNTs) assisted ELM using response surface methodology (RSM) has been performed. The ELM composed of diisooctylphosphinic acid (CYANEX 272) as carrier, MWCNTs as nanoparticles, Span-85 (sorbitan triooleate) as surfactant, kerosene as organic diluent and nitric acid as internal phase. The effects of important operating variables namely, surfactant concentration, MWCNTs concentration, and treatment ratio were investigated. Results were optimized using a central composite design (CCD) and a regression model for extraction percentage was developed. The 3D response surfaces of Nd(III) extraction efficiency were achieved and significance of three important variables and their interactions on the Nd extraction efficiency were found out. Results indicated that introducing the MWCNTs to the ELM process led to increasing the Nd extraction due to higher stability of membrane and mass transfer enhancement. MWCNTs concentration of 407 ppm, Span-85 concentration of 2.1 (%v/v) and treatment ratio of 10 were achieved as the optimum conditions. At the optimum condition, the extraction of Nd(III) reached the maximum of 99.03%.

Optimization of Process Parameters using Response Surface Methodology for the Removal of Zinc(II) by Solvent Extraction

A factorial design of experiments and a response surface methodology were implemented to investigate the liquid-liquid extraction process of zinc (II) from acetate medium using the 1-Butyl-imidazolium di(2-ethylhexyl) phosphate [BIm+][D2EHP-]. The optimization process of extraction parameters such as the initial pH effect (2.5, 4.5, and 6.6), ionic liquid concentration (1, 5.5, and 10 mM) and salt effect (0.01, 5, and 10 mM) was carried out using a three-level full factorial design (33). The results of the factorial design demonstrate that all these factors are statistically significant, including the square effects of pH and ionic liquid concentration. The results showed that the order of significance: IL concentration > salt effect > initial pH. Analysis of variance (ANOVA) showing high coefficient of determination (R2 = 0.91) and low probability values (P < 0.05) signifies the validity of the predicted second-order quadratic model for Zn (II) extraction. The optimum conditions for the extraction of zinc (II) at the constant temperature (20 °C), initial Zn (II) concentration (1mM) and A/O ratio of unity were: initial pH (4.8), extractant concentration (9.9 mM), and NaCl concentration (8.2 mM). At the optimized condition, the metal ion could be quantitatively extracted.

Distribution of Phospholipids, Cholesterol and Carotenoids in Two-Solvent System during Egg Yolk Oil Solvent Extraction

Egg yolk oil is a concentrated source of egg bioactive compounds, such as fat-soluble vitamins, phospholipids, cholesterol, carotenoids and others. To extract lipids and other fat-soluble nutrients from liquid egg yolk, a two-step extraction process involving polar (ethanol) and non-polar (hexane) solvents were used. This extraction technique was based on egg yolk bioactive compounds polarities, where non-polar compound was extracted into non-polar hexane, but polar in to polar alcohol/water phase. But many egg yolk bioactive compounds are not strongly polar or non-polar. Egg yolk phospholipids, cholesterol and pigments are amphipatic (have both polar and non-polar regions) and their behavior in ethanol/hexane solvent system is not clear. The aim of this study was to clarify the behavior of phospholipids, cholesterol and carotenoids during extraction of egg yolk oil with ethanol and hexane and determine the loss of these compounds in egg yolk oil. Egg yolks and egg yolk oil were analyzed for phospholipids (phosphatidylcholine (PC) and phosphatidylethanolamine (PE)), cholesterol and carotenoids (lutein, zeaxanthin, canthaxanthin and β-carotene) content using GC-FID and HPLC methods. PC and PE are polar lipids and were extracted into polar ethanol phase. Concentration of PC in ethanol was 97.89% and PE 99.81% from total egg yolk phospholipids. Due to cholesterol’s partial extraction into ethanol, cholesterol content in egg yolk oil was reduced in comparison to its total content presented in egg yolk lipids. The highest amount of lutein and zeaxanthin was concentrated in ethanol extract. The opposite situation was observed with canthaxanthin and β-carotene, which became the main pigments of egg yolk oil.

Phenolic Compounds and Antimicrobial Properties of Pomegranate (Punica granatum) Peel Extracts

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

Oil Extraction from Microalgae Dunalliela sp. by Polar and Non-Polar Solvents

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

Selective Solvent Extraction of Calcium and Magnesium from Concentrate Nickel Solutions Using Mixtures of Cyanex 272 and D2EHPA

The performance of organophosphorus extractants Cyanex 272 and D2EHPA on the purification of concentrate nickel sulfate solutions was evaluated. Batch scale tests were carried out at pH range of 2 to 7 using a laboratory solution simulating concentrate nickel liquors as those typically obtained when sulfate intermediates from nickel laterite are re-leached and treated for the selective removal of cobalt, zinc, manganese and copper with Cyanex 272 ([Ca] = 0.57 g/L, [Mg] = 3.2 g/L, and [Ni] = 88 g/L). The increase on the concentration of D2EHPA favored the calcium extraction. The extraction of magnesium is dependent on the pH and of ratio of extractants D2EHPA and Cyanex 272 in the organic phase. The composition of the investigated organic phase did not affect nickel extraction. The number of stages is dependent on the magnesium extraction. The most favorable operating condition to selectively remove calcium and magnesium was determined.

Role of Selenite and Selenate Uptake by Maize Plants in Chlorophyll A and B Content

Extracting and determining chlorophyll pigments (chlorophyll a and b) in green leaves are the procedures based on the solvent extraction of pigments in samples using N,Ndimethylformamide as the extractant. In this study, two species of soluble inorganic selenium forms, selenite (SeIV) and selenate (SeVI) at different concentrations were investigated on maize plants that were growing in nutrient solutions during 2 weeks and at the end of the experiment, amounts of chlorophyll a and b for first and second leaves of maize were measured. In accordance with the results we observed that our regarded Se concentrations in both forms of SeIV and SeVI were not effective on maize plants’ chlorophyll a and b significantly although high level of 3 mg.kg-1 SeIV had negative affect on growth of the samples that had been treated by it but about SeVI samples we did not observe this state and our different considered SeVI concentrations were not toxic for maize plants.

Production and Extraction of Quercetin and (+)-Catechin from Phyllanthus niruri Callus Culture

Quercetin and (+)-catechin are metabolites present in Phyllanthus niruri plant, have potential in medicinal uses as anticancer and antioxidant agents. Studies on production of quercetin and (+)-catechin from P. niruri callus culture via in vitro technique were carried out and the results were compared to the intact plant. P. niruri explants were cultured on Murashige and Skoog (MS) solidified media supplemented with several phytohormone combinations for one month. The metabolites were extracted from P. niruri callus and intact plant by using carbon dioxide supercritical fluid extraction (SFE) with ethanol as modifier and solvent extraction techniques. The extracts were analyzed by means of HPLC method. Results showed that P. niruri callus culture was successfully established. The highest content of quercetin (1.72%) was found from P. niruri callus grown in media supplemented with 0.8mg/L kinetin and 0.2mg/L 2,4-dicholophenoxyacetic acid (2,4-D), which was 1.2 fold higher than intact plant. Meanwhile, the highest amounts of (+)-catechin (0.63%) was found from P. niruri callus grown in media with addition of 0.2mg/L 1-naphthalene acetic acid (NAA) and 0.8mg/L 2,4-D. The SFE condition in this study showed better extraction efficiency when higher contents of selected metabolites were found in all SFE extracts compared to the common solvent extracts.

Separation of Manganese and Cadmium from Cobalt Electrolyte Solution by Solvent Extraction

Impurity metals such as manganese and cadmium from high-tenor cobalt electrolyte solution were selectively removed by solvent extraction method using Co-D2EHPA after converting the functional group of D2EHPA with Co2+ ions. The process parameters such as pH, organic concentration, O/A ratio, kinetics etc. were investigated and the experiments were conducted by batch tests in the laboratory bench scale. Results showed that a significant amount of manganese and cadmium can be extracted using Co-D2EHPA for the optimum processing of cobalt electrolyte solution at equilibrium pH about 3.5. The McCabe-Thiele diagram, constructed from the extraction studies showed that 100% impurities can be extracted through four stages for manganese and three stages for cadmium using O/A ratio of 0.65 and 1.0, respectively. From the stripping study, it was found that 100% manganese and cadmium can be stripped from the loaded organic using 0.4 M H2SO4 in a single contact. The loading capacity of Co-D2EHPA by manganese and cadmium were also investigated with different O/A ratio as well as with number of stages of contact of aqueous and organic phases. Valuable information was obtained for the designing of an impurities removal process for the production of pure cobalt with less trouble in the electrowinning circuit.

Extraction of Phenol, o-Cresol, and p-Cresol from Coal Tar: Effect of Temperature and Mixing

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 phenol, o-cresol, and p-cresol. These compounds are widely used as raw material for insecticides, dyes, medicines, perfumes, coloring matters, and many others. This research needed to be done that given the optimum conditions for the separation of phenol, o-cresol, and p-cresol from the coal tar by solvent extraction process. The aim of the present work was to study the effect of two kinds of aqueous were used as solvents: methanol and acetone solutions, the effect of temperature (298, 306, and 313K) and mixing (30, 35, and 40rpm) for the separation of phenol, o-cresol, and p-cresol from coal tar by solvent extraction. Results indicated that phenol, o-cresol, and p-cresol in coal tar were selectivity extracted into the solvent phase and these components could be separated by solvent extraction. The aqueous solution of methanol, mass ratio of solvent to feed, Eo/Ro=1, extraction temperature 306K and mixing 35 rpm were the most efficient for extraction of phenol, o-cresol, and p-cresol from coal tar.

Feasibility Study for a Castor oil Extraction Plant in South Africa

A feasibility study for the design and construction of a pilot plant for the extraction of castor oil in South Africa was conducted. The study emphasized the four critical aspects of project feasibility analysis, namely technical, financial, market and managerial aspects. The technical aspect involved research on existing oil extraction technologies, namely: mechanical pressing and solvent extraction, as well as assessment of the proposed production site for both short and long term viability of the project. The site is on the outskirts of Nkomazi village in the Mpumalanga province, where connections for water and electricity are currently underway, potential raw material supply proves to be reliable since the province is known for its commercial farming. The managerial aspect was evaluated based on the fact that the current producer of castor oil will be fully involved in the project while receiving training and technical assistance from Sasol Technology, the TSC and SEDA. Market and financial aspects were evaluated and the project was considered financially viable with a Net Present Value (NPV) of R2 731 687 and an Internal Rate of Return (IRR) of 18% at an annual interest rate of 10.5%. The payback time is 6years for analysis over the first 10 years with a net income of R1 971 000 in the first year. The project was thus found to be feasible with high chance of success while contributing to socio-economic development. It was recommended for lab tests to be conducted to establish process kinetics that would be used in the initial design of the plant.

Study on Extraction of Niobium Oxide from Columbite–Tantalite Concentrate

The principal objective of this study is to be able to extract niobium oxide from columbite-tantalite concentrate of Thayet Kon Area in Nay Phi Taw. It is recovered from columbite-tantalite concentrate which contains 19.29 % Nb2O5.The recovery of niobium oxide from columbite-tantalite concentrate can be divided into three main sections, namely, digestion of the concentrate, recovery from the leached solution and precipitation and calcinations. The concentrate was digested with hydrofluoric acid and sulfuric acid. Of the various parameters that effect acidity and time were studied. In the recovery section solvent extraction process using methyl isobutyl ketone was investigated. Ammonium hydroxide was used as a precipitating agent and the precipitate was later calcined. The percentage of niobium oxide is 74%.

Study on Extraction of Ceric Oxide from Monazite Concentrate

Cerium oxide is to be recovered from monazite, which contains about 27.35% CeO2. The principal objective of this study is to be able to extract cerium oxide from monazite of Moemeik Myitsone Area. The treatment of monazite in this study involves three main steps; extraction of cerium hydroxide from monazite, solvent extraction of cerium hydroxide, and precipitation with oxalic acid and calcination of cerium oxalate.

Synthesis of Unconventional Materials Using Chitosan and Crown Ether for Selective Removal of Precious Metal Ions

The polyfunctional and highly reactive bio-polymer, the chitosan was first regioselectively converted into dialkylated chitosan using dimsyl anionic solution(NaH in DMSO) and bromodecane after protecting amino groups by phthalic anhydride. The dibenzo-18-crown-6-ether, on the other hand, was converted into its carbonyl derivatives via Duff reaction prior to incorporate into chitosan by Schiff base formation. Thus formed diformylated dibenzo-18-crown-6-ether was condensed with lipophilic chitosan to prepare the novel solvent extraction reagent. The products were characterized mainly by IR and 1H-NMR. Hence, the multidentate crown ether-embedded polyfunctional bio-material was tested for extraction of Pd(II) and Pt(IV) in aqueous solution.

The Applications of Quantum Mechanics Simulation for Solvent Selection in Chemicals Separation

The quantum mechanics simulation was applied for calculating the interaction force between 2 molecules based on atomic level. For the simple extractive distillation system, it is ternary components consisting of 2 closed boiling point components (A,lower boiling point and B, higher boiling point) and solvent (S). The quantum mechanics simulation was used to calculate the intermolecular force (interaction force) between the closed boiling point components and solvents consisting of intermolecular between A-S and B-S. The requirement of the promising solvent for extractive distillation is that solvent (S) has to form stronger intermolecular force with only one component than the other component (A or B). In this study, the systems of aromatic-aromatic, aromatic-cycloparaffin, and paraffindiolefin systems were selected as the demonstration for solvent selection. This study defined new term using for screening the solvents called relative interaction force which is calculated from the quantum mechanics simulation. The results showed that relative interaction force gave the good agreement with the literature data (relative volatilities from the experiment). The reasons are discussed. Finally, this study suggests that quantum mechanics results can improve the relative volatility estimation for screening the solvents leading to reduce time and money consuming

Two Dimensionnal Model for Extraction Packed Column Simulation using Finite Element Method

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