Search results for: acetic acid extraction

Authors: Wehandaka Pancapalaga

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This study aimed to analyze the water content, yield, fat content, protein content, viscosity, gel strength, pH, melting and organoleptic rabbit skin gelatin with acetic acid extraction levels are different. The materials used in this study were Rex rabbit skin male. Treatments that P1 = the extraction of acetic acid 2% (v / v); P2 = the extraction of acetic acid 3% (v / v); P3 = the extraction of acetic acid 4 % (v / v). P5 = the extraction of acetic acid 5% (v / v). The results showed that the greater the concentration of acetic acid as the extraction of rabbit skin can reduce the water content and fat content of rabbit skin gelatin but increase the protein content, viscosity, pH, gel strength, yield and melting point rabbit skin gelatin. texture, color and smell of gelatin rabbits there were no differences with cow skin gelatin. The results showed that the quality of rabbit skin gelatin accordance Indonesian National Standard (SNI). Conclusion 5% acetic acid extraction produces the best quality gelatin.

Keywords: gelatin, skin rabbit, acetic acid extraction, quality

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Authors: Mingchuan Zhou, Haitao Zhang, Hongfang Ma, Weiyong Ying

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Alumina supported platinum and tin catalysts with different loadings of Pt and Sn were prepared and characterized by low temperature N₂ adsorption/desorption, H₂-temperature programed reduction and CO pulse chemisorption. Pt and Sn below 1% loading were suitable for acetic acid hydrogenation. The best performance over 0.75Pt1Sn/Al₂O₃ can reach 87.55% conversion of acetic acid and 47.39% selectivity of ethanol. The operating conditions of acetic acid hydrogenation over 1Pt1Sn/Al₂O₃ were investigated. High reaction temperature can enhance the conversion of acetic acid, but it decreased total selectivity of ethanol and acetyl acetate. High pressure and low weight hourly space velocity were beneficial to both conversion of acetic acid and selectivity to ethanol.

Keywords: acetic acid, hydrogenation, operating condition, PtSn

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Authors: Ng Mei Han, Nu'man Abdul Hadi

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Extraction of ferulic acid from palm pressed fiber using deep eutectic solvent (DES) of choline chloride-acetic acid (ChCl-AA) and choline chloride-citric acid (ChCl-CA) are reported. Influence of water content in DES on the extraction efficiency was investigated. ChCl-AA and ChCl-CA experienced a drop in viscosity from 9.678 to 1.429 and 22.658 ± 1.655 mm2/s, respectively as the water content in the DES increased from 0 to 50 wt% which contributed to higher extraction efficiency for the ferulic acid. Between 41,155 ± 940 mg/kg ferulic acid was obtained after 6 h reflux when ChCl-AA with 30 wt% water was used for the extraction compared to 30,940 ± 621 mg/kg when neat ChCl-AA was used. Although viscosity of the DES could be improved with the addition of water, there is a threshold where the DES could tolerate the presence of water without changing its solvent behavior. The optimum condition for extraction of ferulic acid from palm pressed fiber was heating for 6 h with DES containing 30 wt% water.

Keywords: deep eutectic solvent, extraction, ferulic acid, palm fibre

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Authors: Kyung-Soon Choi, Ji-Young Hwang, Young-Hee Pyo

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Vinegars have been used as an alternative remedy for treating gout, but the scientific basis remains to be elucidated. In this study, acetic acid fermentation was applied for the first time to Monascus-fermented soybeans to examine its effect on the bioactive components together with the xanthine oxidase inhibitory (XOI) activity of the soy vinegar. The content of total phenols (0.47~0.97 mg gallic acid equivalents/mL) and flavonoids (0.18~0.39 mg quercetin equivallents/mL) were spectrophotometrically determined, and the content of organic acid (10.22~59.76 mg/mL) and isoflavones (6.79~7.46 mg/mL) were determined using HPLC-UV. The analytical method for ubiquinones (0.079~0.276 μg/mL) employed saponification before solvent extraction and quantification using LC-MS. Soy vinegar also showed significant XOI (95.3%) after 20 days of acetic acid fermentation at 30 °C. The results suggest that soy vinegar has potential as a novel medicinal food.

Keywords: acetic acid fermentation, bioactive component, soy vinegar, xanthine oxidase inhibitory activity

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Authors: Aidaoui Ahleme, Hasseine Abdelmalek

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Acetic acid is one of the simplest and most widely used carboxylic acids having many important chemical and industrial applications. Total worldwide production of acetic acid is about 6.5 million tonnes per year. A great deal of efforts has been made in developing feasible and economic method for recovery of carboxylic acids. Among them, Liquid-liquid extraction using aqueous two-phase systems (ATPS) has been demonstrated to be a highly efficient separation technique. The study of efficiently separating and recovering Acetic acid from aqueous solutions is an important significance on industry and environmentally sustainable development. Many research groups in different countries are working in this field and some methods are proposed in the literature. In this work, effect of sodium chloride with different content (5%, 10% and 20%) on the liquid-liquid equilibrium data of (water+ acetic acid+ DCM) system is investigated. The addition of the salt in an aqueous solution introduces ionic forces which affect liquid-liquid equilibrium and which influence directly the distribution coefficient of the solute. From the experimental results, it can be concluded that when the percentage of salt increases in the aqueous solution, the equilibrium between phases is modified in favor of the extracted phase.

Keywords: acetic acid recovery, aqueous solution, salting-effect, sodium chloride

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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

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Authors: Mingchuan Zhou, Haitao Zhang, Hongfang Ma, Weiyong Ying

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Alumina supported PtSn catalysts with cylindrical particles were prepared and characterized by using low temperature N2 adsorption/desorption and X-ray diffraction. Low temperature N2 adsorption/desorption demonstrate that the tableting changed the texture properties of catalysts. XRD pattern indicate that the crystal structure of supports had no change after reaction. The performances over particles of PtSn/Al2O3 catalysts were investigated with regards to reaction temperature, pressure, and H2/AcOH mole ratio. After tableting, the conversion of acetic acid and selectivity of ethanol and acetyl acetate decreased. High reaction temperature and pressure can improve conversion of acetic acid. H2/AcOH mole ratio of 9.36 showed the best performance on acetic acid hydrogenation. High pressure had benefits for the selectivity of ethanol and other two parameters had no obvious effect on selectivity.  

Keywords: acetic acid hydrogenation, cylindrical particles, ethanol, PtSn

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Authors: Fatih Özogul, Sezen Özçeli̇k, Yesim Özogul

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Lactic, acetic, succinic, propionic, formic and butyric acid production by lactic acid bacteria (LAB) were monitored in M17 broth (the control) and some fish (squid, shrimp, octopus, and eel) infusion broth by using HPLC method. There were significant differences in terms of lactic, acetic, succinic, propionic, formic and butyric acid production (p < 0.005) among bacterial strains. Acetic acid production was the lowest by LAB while succinic acid followed by propionic acid was synthesized at the highest levels. Lactic acid production ranged from 0 to 938 mg/L by all LAB strains in different infusion broth. The highest acetic acid production was found by Lb. acidophilus and Lb. delbrueckii subsp. lactic in octopus and shrimp infusion broth, with values of 872 and 674 mg/L, respectively while formic acid formation ranged from 1747 mg/L by Lb. acidophilus in octopus infusion broth to 69 mg/L by Lb. delbrueckii subsp. lactis in shrimp infusion broth. Propionic acid and butyric acid productions by St. thermophilus were 9852 and 3999 mg/L in shrimp infusion broth while Leu. mes. subsp. cremoris synthesized 312 and 9 mg/L of those organic acid in European squid infusion broth, respectively. Apparently, LAB strains had a great capability to generate succinic acid followed by propionic and butyric acid. In addition, other organic acid production differed significantly depending on bacterial strains and growth medium.

Keywords: Lactic acid bacteria , organic acid, HPLC analysis, growth medium

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Authors: Ghazi Faisal Najmuldeen, Rosli Mohd Yunus, Nurfarahin Bt Harun, Mardhiana Binti Ismail

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The microwave extraction has attracted great interest among the researchers. The main virtue of the microwave technique is cost-effective, time saving and simple handling procedure. Castor beans was chosen because of its high content in fatty acid, especially ricinoleic acid. The purpose of this research is to extract the castor oil by using the microwave assisted extraction (MAE) using ethanol as solvent and to investigate the influence of extraction time on castor oil yield and to characterize the main composition of the produced castor oil by using the GC-MS. It was found that there is a direct dependence between the oil yield and the time of extraction as it increases from 45% to 58% as the time increase from 10 min to 60 min. The major components of castor oil detected by GC-MS were ricinoleic acid, linoleic acid and oleic acid.

Keywords: microwave assisted extraction (MAE), castor oil, ricinoleic acid, linoleic acid

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Authors: A. Bara, D. Barkat

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Liquid-liquid extraction is one of the most useful techniques for selective removal and recovery of metal ions from aqueous solutions, applied in purification processes in numerous chemical and metallurgical industries. In this work, The liquid-liquid extraction of cobalt (II) and copper (II) from aqueous solution by capric acid (HL) in chloroform at 25°C has been studied. Our interest in this paper is to study the effect of concentration of capric acid on the extraction of Co(II) and Cu(II) to see the complexes could be formed in the organic phase using various concentration of capric acid. The extraction of cobalt (II) and copper (II) is extracted as the complex CoL2 (HL )2, CuL2 (HL)2.

Keywords: capric acid, Cobalt(II), copper(II), liquid-liquid extraction

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Authors: Neil Jolly, Louisa Beukes, Santiago Benito-SaEz

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Kei-apple is a tree found on the African continent. Limited information exists on the effect of alcoholic and acetous fermentation on the phytochemicals. The fruit has increased L-malic, ascorbic, and phenolic acids. Juice was co-inoculated with Schizosaccharomyces pombe and Saccharomyces cerevisiae to induce alcoholic fermentation and acetous fermentation using acetic acid bacteria. Saccharomyces cerevisiae+S. pombe wines and vinegars had highest pH. Total acidity, soluble solids and L-malic acid decreased during alcoholic and acetous fermentation with highest in S. cerevisiae wines and vinegars. Volatile acidity was highest in S. pombe vinegars but not different from S. cerevisiae and S. cerevisiae+S. pombe. Gallic acid was highest in S. pombe wines and vinegars. Syringic acid was highest in S. cerevisiae wines and vinegars. S. cerevisiae+S. pombe wines were highest in caffeic, p-coumaric and protocatechuic acids. Schizosaccharomyces pombe vinegars were highest in caffeic and p-coumaric acids. Ferulic and sinapic acids were highest in S. pombe and S. cerevisiae wines, respectively. Chlorogenic acid was most abundant in both wines and vinegars. Saccharomyces cerevisiae+S. pombe and S. cerevisiae had a positive effect on most phenolic acids. Saccharomyces cerevisiae +acetic acid bacteria had an increased effect on syringic and chlorogenic acids. Schizosaccharomyces pombe+acetic acid bacteria resulted in an increase in gallic, caffeic and p-coumaric acids. Acetic acid bacteria had minimal performance with respect to volatile acidity production in comparison to commercial vinegars. Acetic acid bacteria selection should therefore be reconsidered and the decrease of certain phenolic acids during acetous fermentation needs to be investigated.

Keywords: acetic acid bacteria, liquid chromatography, phenolics, saccharomyces cerevisiae, schizosaccharomyces pombe

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

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

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

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Authors: Nidhi Nalin

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This study is theoretical modelling of the fermentation process of glucose in agricultural wastes like discarded peaches to produce hydrogen, acetic acid, and carbon dioxide using Thermotoga neopolitana bacteria. The hydrogen gas produced in this process can be used in hydrogen fuel cells to generate power, and the fermented broth with acetic acid and salts could be utilized as salty vinegar if enough acetic acid is produced. The theoretical modelling was done using SuperPro software, and the results indicated how much sugar (discarded peaches) is required to produce both hydrogen and vinegar for the process to be profitable.

Keywords: fermentation, thermotoga, hydrogen, vinegar, biofuel

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

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

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

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

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The synergistic solvent extraction of nickel ion from 0.33 mol dm^-3 Na2SO4 aqueous solutions with capric acid (HL) in the absence and presence of Tri-n-octylphosphine oxide (TOPO) in chloroform at 25°C, has been studied. The extracted species when the capric acid compound was used alone, is NiL2 and NiL2(HL). In the presence of TOPO, a remarkable enhancement on the extraction of nickel (II) with 0.02 mol dm^-3 capric acid was observed upon the addition of 0.00125 and 0.0025 mol dm^-3 TOPO in chloroform. From a synergistic extraction- equilibrium study, the synergistic enhancement was ascribed to the adduct formation NiL2(TOPO) and NiL2(HL)(TOPO). The TOPO-HL interaction strongly influences the synergistic extraction efficiency. The synergistic extraction stoichiometry of nickel (II) with capric acid and TOPO is studied with the methods of slope analysis. The equilibrium constants were determined.

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

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Authors: Panumard Kaewmora, Thirasak Rirksomboon, Vissanu Meeyoo

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Due to the globally growing demands of petroleum fuel and fossil fuels, the scarcity or even depletion of fossil fuel sources could be inevitable. Alternatively, the utilization of renewable sources, such as biomass, has become attractive to the community. Biomass can be converted into bio-oil by fast pyrolysis. In water phase of bio-oil, acetic acid which is one of its main components can be converted to hydrogen with high selectivity over effective catalysts in steam reforming process. Steam reforming of acetic acid as model compound has been intensively investigated for hydrogen production using various metal oxide supported nickel catalysts and yet they seem to be rapidly deactivated depending on the support utilized. A catalyst support such as Ce1-xZrxO2 mixed oxide was proposed for alleviating this problem with the anticipation of enhancing hydrogen yield. However, catalyst preparation methods play a significant role in catalytic activity and performance of the catalysts. In this work, Ce0.75Zr0.25O2 mixed oxide solid solution support was prepared by urea hydrolysis using microwave as heat source. After that nickel metal was incorporated at 15 wt% by incipient wetness impregnation method. The catalysts were characterized by several techniques including BET, XRD, H2-TPR, XRF, SEM, and TEM as well as tested for the steam reforming of acetic acid at various operating conditions. Preliminary results showed that a hydrogen yield of ca. 32% with a relatively high acetic conversion was attained at 650°C.

Keywords: acetic acid, steam reforming, microwave, nickel, ceria, zirconia

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Authors: Konstantza Tonova, Ivan Svinyarov, Milen G. Bogdanov

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Ionic liquids consisting of pairs of imidazolium or phosphonium cation and chloride or saccharinate anion were synthesized and compared with respect to their extraction efficiency towards the fermentative L-lactic acid. The acid partitioning in the equilibrated biphasic systems of ionic liquid and water was quantified through the extraction degree and the partition coefficient. The water transfer from the aqueous into the ionic liquid-rich phase was also always followed. The effect of pH, which determines the state of lactic acid in the aqueous source was studied. The effect of other salting-out substances that modify the ionic liquid/water equilibrium was also investigated in view to reveal the best liquid-liquid system with respect to low toxicity, high extraction and back extraction efficiencies and performance simplicity.

Keywords: ionic liquids, biphasic system, extraction, lactic acid

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Authors: Rotchanaphan Hengaroonprasan, Malinee Sriariyanun, Prapakorn Tantayotai, Supacharee Roddecha, Kraipat Cheenkachorn

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Lignocellolusic material is a substance that is resistant to be degraded by microorganisms or hydrolysis enzymes. To be used as materials for biofuel production, it needs pretreatment process to improve efficiency of hydrolysis. In this work, chemical pretreatments on rice straw using three diluted organic acids, including acetic acid, citric acid, oxalic acid, were optimized. Using Response Surface Methodology (RSM), the effect of three pretreatment parameters, acid concentration, treatment time, and reaction temperature, on pretreatment efficiency were statistically evaluated. The results indicated that dilute oxalic acid pretreatment led to the highest enhancement of enzymatic saccharification by commercial cellulase and yielded sugar up to 10.67 mg/ml when using 5.04% oxalic acid at 137.11 oC for 30.01 min. Compared to other acid pretreatment by acetic acid, citric acid, and hydrochloric acid, the maximum sugar yields are 7.07, 6.30, and 8.53 mg/ml, respectively. Here, it was demonstrated that organic acids can be used for pretreatment of lignocellulosic materials to enhance of hydrolysis process, which could be integrated to other applications for various biorefinery processes.

Keywords: lignocellolusic biomass, pretreatment, organic acid response surface methodology, biorefinery

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Authors: M. Unis, S. Turky, A. Elalem, A. Meshrghi

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The Esterification kinetics of acetic acid with isopropnol in the presence of sulfuric acid as a homogenous catalyst was studied with isothermal batch experiments at 60,70 and 80°C and at a different molar ratio of isopropnol to acetic acid. Investigation of kinetics of the reaction indicated that the low of molar ratio is favored for esterification reaction, this is due to the reaction is catalyzed by acid. The maximum conversion, approximately 60.6% was obtained at 80°C for molar ratio of 1:3 acid : alcohol. It was found that increasing temperature of the reaction, increases the rate constant and conversion at a certain mole ratio, that is due to the esterification is exothermic. The homogenous reaction has been described with simple power-law model. The chemical equilibrium combustion calculated from the kinetic model in agreement with the measured chemical equilibrium.

Keywords: artificial flavors, esterification, chemical equilibria, isothermal

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Authors: Usarat Thawornchaisit, Kamalasiri Juthaisong, Kasama Parsongjeen, Phonsiri Phoengchan

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In this study, sludge samples that were collected from the wastewater treatment plant of a printed circuit board manufacturing industry in Thailand were subjected to acid extraction using sulfuric acid as the chemical extracting agent. The effects of sulfuric acid concentration (A), the ratio of a volume of acid to a quantity of sludge (B) and extraction time (C) on the efficiency of copper extraction were investigated with the aim of finding the optimal conditions for maximum removal of copper from the wastewater treatment sludge. Factorial experimental design was employed to model the copper extraction process. The results were analyzed statistically using analysis of variance to identify the process variables that were significantly affected the copper extraction efficiency. Results showed that all linear terms and an interaction term between volume of acid to quantity of sludge ratio and extraction time (BC), had statistically significant influence on the efficiency of copper extraction under tested conditions in which the most significant effect was ascribed to volume of acid to quantity of sludge ratio (B), followed by sulfuric acid concentration (A), extraction time (C) and interaction term of BC, respectively. The remaining two-way interaction terms, (AB, AC) and the three-way interaction term (ABC) is not statistically significant at the significance level of 0.05. The model equation was derived for the copper extraction process and the optimization of the process was performed using a multiple response method called desirability (D) function to optimize the extraction parameters by targeting maximum removal. The optimum extraction conditions of 99% of copper were found to be sulfuric acid concentration: 0.9 M, ratio of the volume of acid (mL) to the quantity of sludge (g) at 100:1 with an extraction time of 80 min. Experiments under the optimized conditions have been carried out to validate the accuracy of the Model.

Keywords: acid treatment, chemical extraction, sludge, waste management

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Authors: Phillip Minnaar, Neil Jolly, Louisa Beukes, Santiago Benito-Saez

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Dovyalis caffra is a tree found on the African continent. Limited information exists on the effect of acetous fermentation on the phytochemicals of Kei-apple fruit. The phytochemical content of vinegars is derived from compounds present in the fruit the vinegar is made of. Kei-apple fruit juice was co-inoculated with Schizosaccharomyces pombe and Saccharomyces cerevisiae to induce alcoholic fermentation (AF). Acetous fermentation followed AF, using an acetic acid bacteria consortium as an inoculant. Juice had the lowest pH and highest total acidity (TA). The wine had the highest pH and vinegars lowest TA. Total soluble solids and L-malic acid decreased during AF and acetous fermentation. Volatile acidity concentration was not different among vinegars. Gallic, syringic, caffeic, p-coumaric, and chlorogenic acids increased during acetous fermentation, whereas ferulic, sinapic, and protocatechuic acids decreased. Chlorogenic acid was the most abundant phenolic acid in both wines and vinegars. It is evident from this investigation that Kei-apple vinegar is a source of plant-derived phenolics, which evolved through fermentation. However, the AAB selection showed minimal performance with respect to VA production. Acetic acid bacteria selection for acetous fermentation should be reconsidered, and the reasons for the decrease of certain phenolic acids during acetous fermentation needs to be investigated.

Keywords: acetic acid bacteria, acetous fermentation, liquid chromatography, phenolic acids

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Authors: Fatima Ghebghoub

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The solvent extraction of cobalt (II) from sulfate medium using di(2-ethylhexy1) phosphoric acid (D2EHPA, HL) at 25°C has been investigated. The influence of the following parameters was studied: the equilibrium pH, the concentration of the extractant and the nature of diluent. The effect of the diluent using polar and non-polar solvents in the extraction of nickel(II) is discussed. The extracted nickel (II species were found to be CoL2 in 1-octanol and methyl isobutyl ketone and CoL2.2HL in toluene, dichloromethane, chloroform, carbon tetrachloride and cyclohexane. The extraction constants are evaluated for the different diluents.

Keywords: liquid-liquid extraction, cobalt(II), di(2-ethylhexyl) phosphoric acid, diluent effect

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Authors: Hummera Rafique, Aamer Saeed

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Synthesis of structural analogues of various well known bioactive natural 3,4-dihydroisocoumarins viz. Scorzocreticin, Annulatomarin, Montroumarin, and Thunberginol B, have been carried out starting from 3,5-dimethoxy-4-methylphenyl acetic acid. 3,5-Dimethoxy-4-methylphenyl acetic acid was then condensed with various aryl acid chlorides (a-e) to afford the corresponding 6,8-dimethoxy-7-methyl-3-aryl isocoumarins (5a-e). The alkaline hydrolysis of isocoumarins yields keto-acids (3a-e), which were then reduced to hydroxyacids, followed by cyclodehydration with acetic anhydride furnish corresponding 3,4-dihydroisocoumarins (7a-e). Finally, demethylation of 3,4-dihydroisocoumarins was carried out to afford 6,8-dihydroxy-7-methyl-3-aryl-3,4-dihydroisocoumarins (7a-e). Antibacterial evaluation of all the synthesized compounds were carried out against ten bacterial strains, it was concluded that isocoumarins (5a-e) and 3,4-dihydroisocoumarins (7a-e) are more active against gram positive bacteria then gram negative. However, the 6,8-dihydroxy-3,4-dihydroisocoumarin derivatives (8a-e) are more active against gram negative then gram positive.

Keywords: 3, 5-Dimethoxy-4-methylhomophthalic acid, natural 3, 4-Dihydroisocoumarin analogues, antibacterial activity, isocoumarins, demethylation

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Authors: A. Thakur, P. S. Panesar, M. S. Saini

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Extraction of lactic acid by emulsion liquid membrane technology (ELM) using n-trioctyl amine (TOA) in n-heptane as carrier within the organic membrane along with sodium carbonate as acceptor phase was optimized by using response surface methodology (RSM). A three level Box-Behnken design was employed for experimental design, analysis of the results and to depict the combined effect of five independent variables, vizlactic acid concentration in aqueous phase (cl), sodium carbonate concentration in stripping phase (cs), carrier concentration in membrane phase (ψ), treat ratio (φ), and batch extraction time (τ) with equal volume of organic and external aqueous phase on lactic acid extraction efficiency. The maximum lactic acid extraction efficiency (ηext) of 98.21%from aqueous phase in a batch reactor using ELM was found at the optimized values for test variables, cl, cs,, ψ, φ and τ as 0.06 [M], 0.18 [M], 4.72 (%,v/v), 1.98 (v/v) and 13.36 min respectively.

Keywords: emulsion liquid membrane, extraction, lactic acid, n-trioctylamine, response surface methodology

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Authors: Bahdja Guerfi, N. Hadhoum, I. Azouz, M. Bendoumia, S. Bouafia, F. Z. Hadjadj Aoul

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Background: 'Penicillin V' is a narrow, bactericidal antibiotic of the beta-lactam family of the naturally occurring penicillin group. It is limited to infections due to the germs defined as sensitive. The objective of this work was to identify and to characterize Penicillin V acid and its related compounds by High-performance liquid chromatography (HPLC). Methods: Firstly phenoxymethylpenicillin was identified by an infrared absorption. The organoleptic characteristics, pH, and determination of water content were also studied. The dosage of Penicillin V acid active substance and the determination of its related compounds were carried on waters HPLC, equipped with a UV detector at 254 nm and Discovery HS C18 column (250 mm X 4.6 mm X 5 µm) which is maintained at room temperature. The flow rate was about 1 ml per min. A mixture of water, acetonitrile and acetic acid (65:35:01) was used as mobile phase for phenoxyacetic acid ‘impurity B' and a mixture of water, acetonitrile and acetic acid (650:150:5.75) for the assay and 4-hydroxypenicillin V 'impurity D'. Results: The identification of Penicillin V acid active substance and the evaluation of its chemical quality showed conformity with USP 35th edition. The Penicillin V acid content in the raw material is equal to 1692.22 UI/mg. The percentage content of phenoxyacetic acid and 4-hydroxypenicillin V was respectively: 0.035% and 0.323%. Conclusion: Through these results, we can conclude that the Penicillin V acid active substance tested is of good physicochemical quality.

Keywords: characterization, HPLC, Penicillin V acid, related substances

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Authors: Hasan Basri Jumin

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The in vitro flowering of orange jessamine plantlets derived from protoplast was affected by the manipulation of plant growth regulators, sugar and light conditions. MT basal medium containing 5% sucrose and supplemented with 0.001 mg 1-1 indole-acetic-acid was found to be a suitable medium for development of globular somatic embryos derived from protoplasts to form heart-shaped somatic embryos with cotyledon-like structures. The highest percentage (85 %) of flowering was achieved with plantlet on half-strength MT basal medium containing 5% sucrose and 0.001 mg1-1 indole-acetic-acid in light. Exposure to darkness for more than 3 weeks followed by re-exposure to light reduced flowering. Flowering required a 10-day exposure to indole-acetic-acid. Photoperiod with 18 h and 79.4 µmol m-2 s-1 light intensity promoted in vitro flowering in high frequencies. The sucrose treatment affected the flower bud size distribution. Flower buds originating from plantlet derived from protoplasts developed into normal flowers.

Keywords: indole-acetc-acid, light-intensity, Murraya-paniculata, photoperiod, plantlet, Zeatin

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Authors: A. Bara, D. Barkat

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The liquid-liquid extraction of copper (II) from aqueous solution by capric acid (HL) in chloroform at 25°C has been studied. The ionic strength effect of the aqueous phase shows that the extraction of copper(II) increases with the increase in ionic strength. with different ionic strengths 1, 0.5, 0.25, 0.125 and 0.1M in the aqueous phase. Cu (II) is extracted as the complex CuL2(ClO4).

Keywords: liquid-liquid extraction, ionic strength, copper (II), capric acid

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Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

Abstract:

Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

Procedia PDF Downloads 116

Authors: Peter O. Osifo, Hein W. J. P. Neomagus, Hein V. D. Merwe

Abstract:

Chitosan materials from different sources of raw materials were characterized in order to determine optimal preparation conditions and parameters for membrane production. The membrane parameters such as molecular weight, viscosity, and degree of deacetylation were used to evaluate the membrane performance for zinc ion adsorption. The molecular weight of the chitosan was found to influence the viscosity of the chitosan/acetic acid solution. An increase in molecular weight (60000-400000 kg.kmol-1) of the chitosan resulted in a higher viscosity (0.05-0.65 Pa.s) of the chitosan/acetic acid solution. The effect of the degree of deacetylation on the viscosity is not significant. The effect of the membrane production parameters (chitosan- and acetic acid concentration) on the viscosity is mainly determined by the chitosan concentration. For higher chitosan concentrations, a membrane with a better adsorption capacity was obtained. The membrane adsorption capacity increases from 20-130 mg Zn per gram of wet membrane for an increase in chitosan concentration from 2-7 mass %. Chitosan concentrations below 2 and above 7.5 mass % produced membranes that lack good mechanical properties. The optimum manufacturing conditions including chitosan concentration, acetic acid concentration, sodium hydroxide concentration and crosslinking for chitosan membranes within the workable range were defined by the criteria of adsorption capacity and flux. The adsorption increases (50-120 mg.g-1) as the acetic acid concentration increases (1-7 mass %). The sodium hydroxide concentration seems not to have a large effect on the adsorption characteristics of the membrane however, a maximum was reached at a concentration of 5 mass %. The adsorption capacity per gram of wet membrane strongly increases with the chitosan concentration in the acetic acid solution but remains constant per gram of dry chitosan. The optimum solution for membrane production consists of 7 mass % chitosan and 4 mass % acetic acid in de-ionised water. The sodium hydroxide concentration for phase inversion is at optimum at 5 mass %. The optimum cross-linking time was determined to be 6 hours (Percentage crosslinking of 18%). As the cross-linking time increases the adsorption of the zinc decreases (150-50 mg.g-1) in the time range of 0 to 12 hours. After a crosslinking time of 12 hours, the adsorption capacity remains constant. This trend is comparable to the effect on flux through the membrane. The flux decreases (10-3 L.m-2.hr-1) with an increase in crosslinking time range of 0 to 12 hours and reaches a constant minimum after 12 hours.

Keywords: chitosan, membrane, waste water, heavy metal ions, adsorption

Procedia PDF Downloads 353

Authors: A. Mirzaei, S. Zolghadri, M. Athari-Allaf, H. Yousefnia, A. R. Jalilian

Abstract:

Rheumatoid arthritis is the most common autoimmune disease, leading to the destruction of the joints. The aim of this study was the preparation of 90Y-chitosan complex as a novel agent for radiosynovectomy. The complex was prepared in the diluted acetic acid solution. At the optimized condition, the radiochemical purity of higher than 99% was obtained by ITLC method on Whatman No. 1 and by using a mixture of methanol/water/acetic acid (4:4:2) as the mobile phase. The complex was stable in acidic media (pH=3) and its radiochemical purity was above 98% even after 48 hours. The biodistribution data in rats showed that there was no significant leakage of the injected activity even after 48 h. Considering all of the excellent features of the complex, 90Y-chitosan can be used to manipulate synovial inflammation effectively.

Keywords: chitosan, Y-90, radiosynovectomy, biodistribution

Procedia PDF Downloads 453