Search results for: high performance liquid chromatography (HPLC)

Authors: H. Li, L. Ji, J. Su

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Forward osmosis is an emerging technology for separation and has great potential in the concentration of liquid products such as protein, pharmaceutical, and natural products. In pharmacy industry, one of the very tough talks is to concentrate the product in a gentle way since some of the key components may lose bioactivity when exposed to heating or pressurization. Therefore, forward osmosis (FO), which uses inherently existed osmosis pressure instead of externally applied hydraulic pressure, is attractive for pharmaceutical enrichments in a much efficient and energy-saving way. Recently, coordination complexes have been explored as the new class of draw solutes in FO processes due to their bulky configuration and excellent performance in terms of high water flux and low reverse solute flux. Among these coordination complexes, ferric citrate complex with lots of hydrophilic groups and ionic species which make them good solubility and high osmotic pressure in aqueous solution, as well as its low toxicity, has received much attention. However, the chemistry of ferric complexation by citrate is complicated, and disagreement prevails in the literature, especially for the structure of the ferric citrate. In this study, we investigated the chemical reaction with various molar ratio of iron and citrate. It was observed that the ferric citrate complex (Fe-CA2) with molar ratio of 1:1 for iron and citrate formed at the beginning of the reaction, then Fecit would convert to ferric citrate complex at the molar ratio of 1:2 with the proper excess of citrate in the base solution. The structures of the ferric citrate complexes synthesized were systematically characterized by X-ray diffraction (XRD), UV-vis spectroscopy, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT-IR) and Thermogravimetric analysis (TGA). Fe-CA2 solutions exhibit osmotic pressures more than twice of that for NaCl solutions at the same concentrations. Higher osmotic pressure means higher driving force, and this is preferable for the FO process. Fe-CA2 and NaCl draw solutions were prepared with the same osmotic pressure and used in FO process for BSA protein concentration. Within 180 min, BSA concentration was enriched from 0.2 to 0.27 L using Fe-CA draw solutions. However, it was only increased from 0.20 to 0.22 g/L using NaCl draw solutions. A reverse flux of 11 g/m²h was observed for NaCl draw solutes while it was only 0.1 g/m²h for Fe-CA2 draw solutes. It is safe to conclude that Fe-CA2 is much better than NaCl as draw solute and it is suitable for the enrichment of liquid product.

Keywords: draw solutes, ferric citrate complex, forward osmosis, protein enrichment

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Authors: Jignasha Derasari, Patel Krishna M, Modi Jignasa G.

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Chemical stability of pharmaceutical molecules is a matter of great concern as it affects the safety and efficacy of the drug product.Stability testing data provides the basis to understand how the quality of a drug substance and drug product changes with time under the influence of various environmental factors. Besides this, it also helps in selecting proper formulation and package as well as providing proper storage conditions and shelf life, which is essential for regulatory documentation. The ICH guideline states that stress testing is intended to identify the likely degradation products which further help in determination of the intrinsic stability of the molecule and establishing degradation pathways, and to validate the stability indicating procedures. A simple, accurate and precise stability indicating RP- HPLC method was developed and validated for simultaneous estimation of Amiloride Hydrochloride and Furosemide in tablet dosage form. Separation was achieved on an Phenomenexluna ODS C18 (250 mm × 4.6 mm i.d., 5 µm particle size) by using a mobile phase consisting of Ortho phosphoric acid: Acetonitrile (50:50 %v/v) at a flow rate of 1.0 ml/min (pH 3.5 adjusted with 0.1 % TEA in Water) isocratic pump mode, Injection volume 20 µl and wavelength of detection was kept at 283 nm. Retention time for Amiloride Hydrochloride and Furosemide was 1.810 min and 4.269 min respectively. Linearity of the proposed method was obtained in the range of 40-60 µg/ml and 320-480 µg/ml and Correlation coefficient was 0.999 and 0.998 for Amiloride hydrochloride and Furosemide, respectively. Forced degradation study was carried out on combined dosage form with various stress conditions like hydrolysis (acid and base hydrolysis), oxidative and thermal conditions as per ICH guideline Q2 (R1). The RP- HPLC method has shown an adequate separation for Amiloride hydrochloride and Furosemide from its degradation products. Proposed method was validated as per ICH guidelines for specificity, linearity, accuracy; precision and robustness for estimation of Amiloride hydrochloride and Furosemide in commercially available tablet dosage form and results were found to be satisfactory and significant. The developed and validated stability indicating RP-HPLC method can be used successfully for marketed formulations. Forced degradation studies help in generating degradants in much shorter span of time, mostly a few weeks can be used to develop the stability indicating method which can be applied later for the analysis of samples generated from accelerated and long term stability studies. Further, kinetic study was also performed for different forced degradation parameters of the same combination, which help in determining order of reaction.

Keywords: amiloride hydrochloride, furosemide, kinetic study, stability indicating RP-HPLC method validation

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Authors: Erwin Chan, Aravind Subramaniyan, Siti Abdullah Fatehah, Steve Lian Kuling

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Foam assisted lift technology is proven across the industry to provide efficient deliquification in gas wells. Such deliquification is typically achieved by delivering the foamer chemical downhole via capillary strings. In highly liquid loaded wells where capillary strings are not readily available, foamer can be delivered via batch injection or bull-heading. The latter techniques differ from the former in that cap strings allow for liquid to be unloaded continuously, whereas foamer batches require that periodic batching be conducted for the liquid to be unloaded. Although batch injection allows for liquid to be unloaded in wells with suitable water to gas (WGR) ratio and condensate to gas (CGR) ratio without well intervention for capillary string installation, this technique comes with its own set of challenges - for foamer to de-liquify liquids, the chemical needs to reach perforation locations where gas bubbling is observed. In highly scaled perforation zones in certain wells, foamer delivered in batches is unable to reach the gas bubbling zone, thus achieving poor lift efficiency. This paper aims to discuss the techniques and challenges for unloading liquid via batch injection in scaled perforation wells X and Y, whose WGR is 6bbl/MMscf, whose scale build-up is observed at the bottom of perforation interval, whose water column is 400 feet, and whose ‘bubbling zone’ is less than 100 feet. Variables such as foamer Z dosage, batching technique, and well flow control valve opening times are manipulated during the duration of the trial to achieve maximum liquid unloading and gas rates. During the field trial, the team has found optimal values between the three aforementioned parameters for best unloading results, in which each cycle’s gas and liquid rates are compared with baselines with similar flowing tubing head pressures (FTHP). It is discovered that amongst other factors, a good agitation technique is a primary determinant for efficient liquid unloading. An average increment of 2MMscf/d against an average production of 4MMscf/d at stable FTHP is recorded during the trial.

Keywords: foam, foamer, gas lift, liquid unloading, scale, batch injection

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Authors: Ramandeep Kaur, Ashok Kumar Malik

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Fabric Phase Sorptive Extraction (FPSE) combined with Gas chromatography Mass Spectrometry (GCMS) has been developed for the determination of nineteen organochlorine pesticides in various aqueous samples. The method consolidates the features of sol-gel derived microextraction sorbents with rich surface chemistry of cellulose fabric substrate which could directly extract sample from complex sample matrices and incredibly improve the operation with decreased pretreatment time. Some vital parameters such as kind and volume of extraction solvent and extraction time were examinedand optimized. Calibration curves were obtained in the concentration range 0.5-500 ng/mL. Under the optimum conditions, the limits of detection (LODs) were in the range 0.033 ng/mL to 0.136 ng/mL. The relative standard deviations (RSDs) for extraction of 10 ng/mL 0f OCPs were less than 10%. The developed method has been applied for the quantification of these compounds in aqueous and fruit juice samples. The results obtained proved the present method to be rapid and feasible for the determination of organochlorine pesticides in aqueous samples.

Keywords: fabric phase sorptive extraction, gas chromatography-mass spectrometry, organochlorine pesticides, sample pretreatment

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Authors: Boris Nemzer, Nebiyu Abshiru, Z. B. Pietrzkowski

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Coffee cherry is one of the most ubiquitous agricultural commodities which possess nutritional and human health beneficial properties. Between the two most widely used coffee cherries Coffea arabica (Arabica) and Coffea canephora (Robusta), Coffea arabica remains superior due to its sensory properties and, therefore, remains in great demand in the global coffee market. In this study, the phytochemical contents and pharmacokinetics of Coffeeberry® Energy (CBE), a commercially available Arabica whole coffee fruit caffeine extract, are investigated. For phytochemical screening, 20 mg of CBE was dissolved in an aqueous methanol solution for analysis by mass spectrometry (MS). Quantification of caffeine and chlorogenic acids (CGAs) contents of CBE was performed using HPLC. For the bioavailability study, serum samples were collected from human subjects before and after 1, 2 and 3 h post-ingestion of 150mg CBE extract. Protein precipitation and extraction were carried out using methanol. Identification of compounds was performed using an untargeted metabolomic approach on Q-Exactive Orbitrap MS coupled to reversed-phase chromatography. Data processing was performed using Thermo Scientific Compound Discover 3.3 software. Phytochemical screening identified a total of 170 compounds, including organic acids, phenolic acids, CGAs, diterpenoids and hydroxytryptamine. Caffeine & CGAs make up more than, respectively, 70% & 9% of the total CBE composition. For serum samples, a total of 82 metabolites representing 32 caffeine- and 50 phenolic-derived metabolites were identified. Volcano plot analysis revealed 32 differential metabolites (24 caffeine- and 8 phenolic-derived) that showed an increase in serum level post-CBE dosing. Caffeine, uric acid, and trimethyluric acid isomers exhibited 4- to 10-fold increase in serum abundance post-dosing. 7-Methyluric acid, 1,7-dimethyluric acid, paraxanthine and theophylline exhibited a minimum of 1.5-fold increase in serum level. Among the phenolic-derived metabolites, iso-feruloyl quinic acid isomers (3-, 4- and 5-iFQA) showed the highest increase in serum level. These compounds were essentially absent in serum collected before dosage. More interestingly, the iFQA isomers were not originally present in the CBE extract, as our phytochemical screen did not identify these compounds. This suggests the potential formation of the isomers during the digestion and absorption processes. Pharmacokinetics parameters (Cmax, Tmax and AUC0-3h) of caffeine- and phenolic-derived metabolites were also investigated. Caffeine was rapidly absorbed, reaching a maximum concentration (Cmax) of 10.95 µg/ml in just 1 hour. Thereafter, caffeine level steadily dropped from the peak level, although it did not return to baseline within the 3-hour dosing period. The disappearance of caffeine from circulation was mirrored by the rise in the concentration of its methylxanthine metabolites. Similarly, serum concentration of iFQA isomers steadily increased, reaching maximum (Cmax: 3-iFQA, 1.54 ng/ml; 4-iFQA, 2.47 ng/ml; 5-iFQA, 2.91 ng/ml) at tmax of 1.5 hours. The isomers remained well above the baseline during the 3-hour dosing period, allowing them to remain in circulation long enough for absorption into the body. Overall, the current study provides evidence of the potential health benefits of a uniquely formulated whole coffee fruit product. Consumption of this product resulted in a distinct serum profile of bioactive compounds, as demonstrated by the more than 32 metabolites that exhibited a significant change in systemic exposure.

Keywords: phytochemicals, mass spectrometry, pharmacokinetics, differential metabolites, chlorogenic acids

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Authors: Natia Jalagonia, Tinatin Kuchukhidze

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Polymer electrolytes (PE) play an important part in electrochemical devices such as batteries and fuel cells. To achieve optimal performance, the PE must maintain a high ionic conductivity and mechanical stability at both high and low relative humidity. The polymer electrolyte also needs to have excellent chemical stability for long and robustness. According to the prevailing theory, ionic conduction in polymer electrolytes is facilitated by the large-scale segmental motion of the polymer backbone, and primarily occurs in the amorphous regions of the polymer electrolyte. Crystallinity restricts polymer backbone segmental motion and significantly reduces conductivity. Consequently, polymer electrolytes with high conductivity at room temperature have been sought through polymers which have highly flexible backbones and have largely amorphous morphology. The interest in polymer electrolytes was increased also by potential applications of solid polymer electrolytes in high energy density solid state batteries, gas sensors and electrochromic windows. Conductivity of 10-3 S/cm is commonly regarded as a necessary minimum value for practical applications in batteries. At present, polyethylene oxide (PEO)-based systems are most thoroughly investigated, reaching room temperature conductivities of 10-7 S/cm in some cross-linked salt in polymer systems based on amorphous PEO-polypropylene oxide copolymers.. It is widely accepted that amorphous polymers with low glass transition temperatures Tg and a high segmental mobility are important prerequisites for high ionic conductivities. Another necessary condition for high ionic conductivity is a high salt solubility in the polymer, which is most often achieved by donors such as ether oxygen or imide groups on the main chain or on the side groups of the PE. It is well established also that lithium ion coordination takes place predominantly in the amorphous domain, and that the segmental mobility of the polymer is an important factor in determining the ionic mobility. Great attention was pointed to PEO-based amorphous electrolyte obtained by synthesis of comb-like polymers, by attaching short ethylene oxide unit sequences to an existing amorphous polymer backbone. The aim of presented work is to obtain of solid polymer electrolyte membranes using PMHS as a matrix. For this purpose the hydrosilylation reactions of α,ω-bis(trimethylsiloxy)methyl¬hydrosiloxane with allyl triethylene-glycol mo¬nomethyl ether and vinyltriethoxysilane at 1:28:7 ratio of initial com¬pounds in the presence of Karstedt’s catalyst, platinum hydrochloric acid (0.1 M solution in THF) and platinum on the carbon catalyst in 50% solution of anhydrous toluene have been studied. The synthesized olygomers are vitreous liquid products, which are well soluble in organic solvents with specific viscosity ηsp ≈ 0.05 - 0.06. The synthesized olygomers were analysed with FTIR, 1H, 13C, 29Si NMR spectroscopy. Synthesized polysiloxanes were investigated with wide-angle X-ray, gel-permeation chromatography, and DSC analyses. Via sol-gel processes of doped with lithium trifluoromethylsulfonate (triflate) or lithium bis¬(trifluoromethylsulfonyl)¬imide polymer systems solid polymer electrolyte membranes have been obtained. The dependence of ionic conductivity as a function of temperature and salt concentration was investigated and the activation energies of conductivity for all obtained compounds are calculated

Keywords: synthesis, PMHS, membrane, electrolyte

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Authors: Arif Budiman

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Any organization or company that wishes to achieve vision, mission, and goals of the organization is required to implement a performance management system or known as the Performance Management System (PMS) in every part of the whole organization. PMS is a tool to help visualize the direction and work program of the organization to achieve the goal. The challenge is PMS should not stop merely as a visualization tool to achieve the vision and mission of the organization, but PMS should also be able to create a high-performance culture that is inherent in each individual of the organization. Establishment of a culture within an organization requires the support of top leaders and also requires a system or governance that encourages every individual in the organization to be involved in any work program of the organization. Keywords of creating a high-performance culture are the formation of communication pattern involving the whole individual, either vertically or horizontally, and performed consistently and persistently by all individuals in each line of the organization. PT Pertamina (Persero) as the state-owned national energy company holds a system to internalize the culture of high performance through a system called Performance Management System Cycle (PMS Cycle). This system has 7 stages of the cycle, those are: (1) defining vision, mission and strategic plan of the company, (2) defining key performance indicator of each line and the individual (‘expectation setting conversation’), (3) defining performance target and performance agreement, (4) monitoring performance on a monthly regular basis (‘pulse check’), (5) implementing performance dialogue between leaders and staffs periodically every 3 months (‘performance dialogue’), (6) defining rewards and consequences based on the achievement of the performance of each line and the individual, and (7) calculating the final performance value achieved by each line and individual from one period of the current year. Perform PMS is a continual communication running throughout the year, that is why any three performance discussion that should be performed, include expectation setting conversations, pulse check and performance dialogue. In addition, another significant point and necessary undertaken to complete the assessment of individual performance assessment is soft competencies through 360-degree assessment by leaders, staffs, and peers.

Keywords: 360-degree assessment, expectation setting conversation, performance management system cycle, performance dialogue, pulse check

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Authors: Hend Ben Tkhayat , Khaled Al Zahabi, Husam Younes

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Introduction: Vildagliptin (VG), a dipeptidyl peptidase-4 inhibitor (DPP-4), was proven to be an active agent for the treatment of type 2 diabetes. VG works by enhancing and prolonging the activity of incretins which improves insulin secretion and decreases glucagon release, therefore lowering blood glucose level. It is usually used with various classes, such as insulin sensitizers or metformin. VG is currently only marketed as an immediate-release tablet that is administered twice daily. In this project, we aim to formulate an extended-release with a zero-order profile tableted lipid microparticles of VG that could be administered once daily ensuring the patient’s convenience. Method: The spray-congealing technique was used to prepare VG microparticles. Compritol® was heated at 10 oC above its melting point and VG was dispersed in the molten carrier using a homogenizer (IKA T25- USA) set at 13000 rpm. VG dispersed in the molten Compritol® was added dropwise to the molten Gelucire® 50/13 and PEG® (400, 6000, and 35000) in different ratios under manual stirring. The molten mixture was homogenized and Carbomer® amount was added. The melt was pumped through the two-fluid nozzle of the Buchi® Spray-Congealer (Buchi B-290, Switzerland) using a Pump drive (Master flex, USA) connected to a silicone tubing wrapped with silicone heating tape heated at the same temperature of the pumped mix. The physicochemical properties of the produced VG-loaded microparticles were characterized using Mastersizer, Scanning Electron Microscope (SEM), Differential Scanning Calorimeter (DSC) and X‐Ray Diffractometer (XRD). VG microparticles were then pressed into tablets using a single punch tablet machine (YDP-12, Minhua pharmaceutical Co. China) and in vitro dissolution study was investigated using Agilent Dissolution Tester (Agilent, USA). The dissolution test was carried out at 37±0.5 °C for 24 hours in three different dissolution media and time phases. The quantitative analysis of VG in samples was realized using a validated High-Pressure Liquid Chromatography (HPLC-UV) method. Results: The microparticles were spherical in shape with narrow distribution and smooth surface. DSC and XRD analyses confirmed the crystallinity of VG that was lost after being incorporated into the amorphous polymers. The total yields of the different formulas were between 70% and 80%. The VG content in the microparticles was found to be between 99% and 106%. The in vitro dissolution study showed that VG was released from the tableted particles in a controlled fashion. The adjustment of the hydrophilic/hydrophobic ratio of excipients, their concentration and the molecular weight of the used carriers resulted in tablets with zero-order kinetics. The Gelucire 50/13®, a hydrophilic polymer was characterized by a time-dependent profile with an important burst effect that was decreased by adding Compritol® as a lipophilic carrier to retard the release of VG which is highly soluble in water. PEG® (400,6000 and 35 000) were used for their gelling effect that led to a constant rate delivery and achieving a zero-order profile. Conclusion: Tableted spray-congealed lipid microparticles for extended-release of VG were successfully prepared and a zero-order profile was achieved.

Keywords: vildagliptin, spray congealing, microparticles, controlled release

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Authors: Y. A. Prada, Fanny Guzman, Rafael Cabanzo, John J. Castillo, Enrique Mejia-Ospino

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In this work, we show the important results about of synthesis of photoluminiscents gold nanoclusters using a small peptide as template for biosensing applications. Interestingly, we design one peptide (NBC2854) homologue to conservative domain from 215 250 residue of a galactolectin protein which can recognize the proteophosphoglycans (PPG) from Leishmania. Peptide was synthetized by multiple solid phase synthesis using FMoc group methodology in acid medium. Finally, the peptide was purified by High-Performance Liquid Chromatography using a Vydac C-18 preparative column and the detection was at 215 nm using a Photo Diode Array detector. Molecular mass of this peptide was confirmed by MALDI-TOF and to verify the α-helix structure we use Circular Dichroism. By means of the methodology used we obtained a novel fluorescents gold nanoclusters (AuNC) using NBC2854 as a template. In this work, we described an easy and fast microsonic method for the synthesis of AuNC with ≈ 3.0 nm of hydrodynamic size and photoemission at 630 nm. The presence of cysteine residue in the C-terminal of the peptide allows the formation of Au-S bond which confers stability to Peptide-based gold nanoclusters. Interactions between the peptide and gold nanoclusters were confirmed by X-ray Photoemission and Raman Spectroscopy. Notably, from the ultrafine spectra shown in the MALDI-TOF analysis which containing only 3-7 KDa species was assigned to Au₈-₁₈[NBC2854]₂ clusters. Finally, we evaluated the Peptide-gold nanocluster as an optical biosensor based on fluorescence spectroscopy and the fluorescence signal of PPG (0.1 µg-mL⁻¹ to 1000 µg-mL⁻¹) was amplified at the same wavelength emission (≈ 630 nm). This can suggest that there is a strong interaction between PPG and Pep@AuNC, therefore, the increase of the fluorescence intensity can be related to the association mechanism that take place when the target molecule is sensing by the Pep@AuNC conjugate. Further spectroscopic studies are necessary to evaluate the fluorescence mechanism involve in the sensing of the PPG by the Pep@AuNC. To our best knowledge the fabrication of an optical biosensor based on Pep@AuNC for sensing biomolecules such as Proteophosphoglycans which are secreted in abundance by parasites Leishmania.

Keywords: biosensing, fluorescence, Leishmania, peptide-gold nanoclusters, proteophosphoglycans

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Authors: Ki Woong Lee

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The Center for Axion and Precision Physics Research is studying the search for dark matter using 12 tesla superconducting magnets. A dilution refrigerator is being used for search experiments, and superconducting magnets, superconducting cavities. The dilution refrigerator requires a stable cryogenic environment using liquid helium. Accordingly, a cryogenic system for a stable supply of liquid helium is to be established. This cryogenic system includes the liquefying, supply, storage, and purification of liquid helium. This article presents the basic design, construction, and operation plans for building cryogenic systems.

Keywords: cryogenic system, dilution refrigerator, superconducting magnet, helium recovery system

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Authors: S. Mousavian, A. Abedianpour, A. Khanmohammadi, S. Hematian, Gh. Eidi Veisi

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Ionic liquids are finding a wide range of applications from reaction media to separations and materials processing. In these applications, Vapor–Liquid equilibrium (VLE) is the most important one. VLE for six systems at 353 K and activity coefficients at infinite dilution 〖(γ〗_i^∞) for various solutes (alkanes, alkenes, cycloalkanes, cycloalkenes, aromatics, alcohols, ketones, esters, ethers, and water) in the ionic liquids (1-ethyl-3-methylimidazolium bis (trifluoromethylsulfonyl)imide [EMIM][BTI], 1-hexyl-3-methyl imidazolium bis (trifluoromethylsulfonyl) imide [HMIM][BTI], 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide [OMIM][BTI], and 1-butyl-1-methylpyrrolidinium bis (trifluoromethylsulfonyl) imide [BMPYR][BTI]) have been used to train neural networks in the temperature range from (303 to 333) K. Densities of the ionic liquids, Hildebrant constant of substances, and temperature were selected as input of neural networks. The networks with different hidden layers were examined. Networks with seven neurons in one hidden layer have minimum error and good agreement with experimental data.

Keywords: ionic liquid, neural networks, VLE, dilute solution

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Authors: Meimei Wen, Chang Nyung Kim

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In the current study, three-dimensional liquid metal (LM) magneto-hydrodynamic (MHD) flows in a manifold with three sub-channels under a uniform magnetic field are numerically investigated. In the manifold, the electrical current can cross channel walls, thus having influence on the flow distribution in each sub-channel. A case with various arrangements of electric conductivity for different parts of channel walls is considered, yielding different current distributions as well as flow distributions in each sub-channel. Here, the imbalance of mass flow rates in the three sub-channels is addressed. Meanwhile, predicted are detailed behaviors of the flow velocity, pressure, current and electric potential of LM MHD flows with three sub-channels. Commercial software CFX is used for the numerical simulation of LM MHD flows.

Keywords: CFX, liquid metal, manifold, MHD flow

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Authors: Flavien Marteau, Pedro Affonso Nóbrega, Pascal Biwole, Nicolas Autrusson, Iona De Bievre, Christian Beauger

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Effective water management is essential for the optimal performance of fuel cells. For this reason, many vehicle systems use a membrane humidifier, a passive device that humidifies the air before the cathode inlet. Although they offer good performance, humidifiers are voluminous, costly, and fragile, hence the desire to find an alternative. Direct water injection could be an option, although this method lacks maturity. It consists of injecting liquid water as a spray in the dry heated air coming out from the compressor. This work focuses on the evaluation of direct water injection and its performance compared to the membrane humidifier selected as a reference. Two architectures were experimentally tested to humidify an industrial 2 kW short stack made up of 20 cells of 150 cm² each. For the reference architecture, the inlet air is humidified with a commercial membrane humidifier. For the direct water injection architecture, a pneumatic nozzle was selected to generate a fine spray in the air flow with a Sauter mean diameter of about 20 μm. Initial performance was compared over the entire range of current based on polarisation curves. Then, the influence of various parameters impacting water management was studied, such as the temperature, the gas stoichiometry, and the water injection flow rate. The experimental results obtained confirm the possibility of humidifying the fuel cell using direct water injection. This study, however shows the limits of this humidification method, the mean cell voltage being significantly lower in some operating conditions with direct water injection than with the membrane humidifier. The voltage drop reaches 30 mV per cell (4 %) at 1 A/cm² (1,8 bara, 80 °C) and increases in more demanding humidification conditions. It is noteworthy that the heat of compression available is not enough to evaporate all the injected liquid water in the case of DWI, resulting in a mix of liquid and vapour water entering the fuel cell, whereas only vapour is present with the humidifier. Variation of the injection flow rate shows that part of the injected water is useless for humidification and seems to cross channels without reaching the membrane. The stack was successfully humidified thanks to direct water injection. Nevertheless, our work shows that its implementation requires substantial adaptations and may reduce the fuel cell stack performance when compared to conventional membrane humidifiers, but opportunities for optimisation have been identified.

Keywords: cathode humidification, direct water injection, membrane humidifier, proton exchange membrane fuel cell

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Authors: Hemant Upadhyay, Tarun Kumar Kundu

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It is utmost important for a blast furnace operator to understand the mechanisms governing the liquid flow, accumulation, drainage and heat transfer between various phases in blast furnace hearth for a stable and efficient blast furnace operation. Abnormal drainage behavior may lead to high liquid build up in the hearth. Operational problems such as pressurization, low wind intake, and lower material descent rates, normally be encountered if the liquid levels in the hearth exceed a critical limit when Hearth coke and Deadman start to float. Similarly, hot metal temperature is an important parameter to be controlled in the BF operation; it should be kept at an optimal level to obtain desired product quality and a stable BF performance. It is not possible to carry out any direct measurement of above due to the hostile conditions in the hearth with chemically aggressive hot liquids. The objective here is to develop a mathematical model to simulate the variation in hot metal / slag accumulation and temperature during the tapping of the blast furnace based on the computed drainage rate, production rate, mass balance, heat transfer between metal and slag, metal and solids, slag and solids as well as among the various zones of metal and slag itself. For modeling purpose, the BF hearth is considered as a pressurized vessel, filled with solid coke particles. Liquids trickle down in hearth from top and accumulate in voids between the coke particles which are assumed thermally saturated. A set of generic mass balance equations gives the amount of metal and slag intake in hearth. A small drainage (tap hole) is situated at the bottom of the hearth and flow rate of liquids from tap hole is computed taking in account the amount of both the phases accumulated their level in hearth, pressure from gases in the furnace and erosion behaviors of tap hole itself. Heat transfer equations provide the exchange of heat between various layers of liquid metal and slag, and heat loss to cooling system through refractories. Based on all that information a dynamic simulation is carried out which provides real time information of liquids accumulation in hearth before and during tapping, drainage rate and its variation, predicts critical event timings during tapping and expected tapping temperature of metal and slag on preset time intervals. The model is in use at JSPL, India BF-II and its output is regularly cross-checked with actual tapping data, which are in good agreement.

Keywords: blast furnace, hearth, deadman, hotmetal

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Authors: Kane Esien, Eadaoin McCourt, Peter Nockemann, Soveig Felton

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Magnetic ionic liquids (MILs) are a class of ionic liquid incorporating one or more magnetic atoms into the anion or cation of the ionic liquid, endowing the ionic liquid with magnetic properties alongside the existing properties of ionic liquids. MILs have applications in e.g. fluid-fluid separations, electrochemistry, and polymer chemistry. In this study three different types of Bis-Lanthanoates, that exist in different phases, have been synthesised and characterised (Ln = lanthanide): 1) imidazolium lanthanide acetate – [C4Mim]2[Ln2(OAc)8] – forms a crystalline solid at room temperature, 2) phosphonium lanthanide acetate – [P666 14]2[Ln2(OAc)8] – is in a solid glassy state, and 3) phosphonium lanthanide octanoate – [P666 14]2[Ln2(Oct)8] – is an ionic liquid. X-ray diffraction of the crystalline solid imidazolium lanthanide acetate – [C4Mim]2[Ln2(OAc)8] confirm that the Ln(III) ions form dimers, bridged by carboxyl groups, but cannot yield information about samples phosphonium lanthanide acetate – [P666 14]2[Ln2(OAc)8] (glass) and phosphonium lanthanide octanoate – [P666 14]2[Ln2(Oct)8] (ionic liquid) since these lack long-range order. SQUID magnetometry studies show that all three samples have effective magnetic moments consistent with non-interacting Ln(III) ions at room temperature but deviate from this behavior in the same way below 50 K. Through modeling the magnetic response, we are able to show that we have formed magnetic dimers, in all compounds, that are weakly antiferromagnetically interacting

Keywords: dimeric ionic liquids, interactions, SQUID, structure

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Authors: Benoit Atge, Alice Dhersin, Oscar Da Silva Cacao, Beatrice Martinez, Dominique Ducint, Catherine Verdun-Esquer, Isabelle Baldi, Mathieu Molimard, Antoine Villa, Mireille Canal-Raffin

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Introduction: Healthcare workers' exposure to antineoplastic drugs (AD) is a burning issue for occupational medicine practitioners. Biological monitoring of occupational exposure (BMOE) is an essential tool for assessing AD contamination of healthcare workers. In addition to BMOE, surface sampling is a useful tool in order to understand how workers get contaminated, to identify sources of environmental contamination, to verify the effectiveness of surface decontamination way and to ensure monitoring of these surfaces. The objective of this work was to develop a complete tool including a kit for surface sampling and a quantification analytical method for AD traces detection. The development was realized with the three following criteria: the kit capacity to sample in every professional environment (healthcare services, veterinaries, etc.), the detection of very low AD traces with a validated analytical method and the easiness of the sampling kit use regardless of the person in charge of sampling. Material and method: AD mostly used in term of quantity and frequency have been identified by an analysis of the literature and consumptions of different hospitals, veterinary services, and home care settings. The kind of adsorbent device, surface moistening solution and mix of solvents for the extraction of AD from the adsorbent device have been tested for a maximal yield. The AD quantification was achieved by an ultra high-performance liquid chromatography method coupled with tandem mass spectrometry (UHPLC-MS/MS). Results: With their high frequencies of use and their good reflect of the diverse activities through healthcare, 15 AD (cyclophosphamide, ifosfamide, doxorubicin, daunorubicin, epirubicin, 5-FU, dacarbazin, etoposide, pemetrexed, vincristine, cytarabine, methothrexate, paclitaxel, gemcitabine, mitomycin C) were selected. The analytical method was optimized and adapted to obtain high sensitivity with very low limits of quantification (25 to 5000ng/mL), equivalent or lowest that those previously published (for 13/15 AD). The sampling kit is easy to use, provided with a didactic support (online video and protocol paper). It showed its effectiveness without inter-individual variation (n=5/person; n= 5 persons; p=0,85; ANOVA) regardless of the person in charge of sampling. Conclusion: This validated tool (sampling kit + analytical method) is very sensitive, easy to use and very didactic in order to control the chemical risk brought by AD. Moreover, BMOE permits a focal prevention. Used in routine, this tool is available for every intervention of occupational health.

Keywords: surface contamination, sampling kit, analytical method, sensitivity

Procedia PDF Downloads 129

Authors: Sunaitan Al Mutairi, Kumar Vallatharasu, Batool Ismaeel

Abstract:

The Water Knock-Out (WKO) facility project is to handle the undesirable impact of the increasing water production rate in South and East Kuwait (S&EK) areas and break the emulsions and ensure sufficient separation of water at the new upstream facility, to reduce the load on the existing separation equipment in the Gathering Centers (GC). As the existing separation equipment in the Gathering Centers are not efficient to separate the emulsions, the Compact Electrostatic Coalescer (CEC) and Vessel Internal Electrostatic Coalescer (VIEC) technologies have been selected for enhancing the liquid-liquid separation by using the alternating voltage/frequency on electrical fields, to handle the increasing water-cut in S&EK. In the Compact Electrostatic Coalescer (CEC) technology method, the CEC equipment is installed downstream of the inlet separator externally, whereas in the Vessel Internal Electrostatic Coalescer (VIEC) technology method, the VIEC is built inside the treater vessel, downstream of the inlet separator with advanced internals for implementing electrocoalescence of water particles and hence enhancing liquids separation. The CEC and VIEC technologies used in the Water Knockout Facility project has the ability to resolve the increasing water cut in the S&EK area and able to enhance the liquid-liquid separation in the WKO facility separation equipment. In addition, the WKO facility is minimizing the load on the existing Gathering Center’s separation equipment, by tackling the high water-cut wells, upstream of each GC. The required performances at the outlet of the WKO facility are Oil in Water 100ppmv, Water in Oil 15% volume, liquid carryover in gas 0.1 US gal/MMSCFD, for the water cut ranging from 37.5 to 75% volume. The WKO facility project is used to sustain, support and maintain Greater Burgan production at 1.7 Million Barrels of Oil Per Day (MMBOPD), by handling the increasing water production rate.

Keywords: emulsion, increasing water-cut, production, separation equipment

Procedia PDF Downloads 243

Authors: Yang Luo, Chang Nyung Kim

Abstract:

This study numerically analyzes a steady-state, three-dimensional liquid-metal magnetohydrodynamic flows in a conduit with multiple channels under a uniform magnetic field. The geometry of the conduit is of a four-parallel-channels system including one inflow channel and three outflow channels. The liquid-metal flows in the inflow channel, then turns 1800 in the transition segment, finally flows into three different outflow channels simultaneously. This kind of channel system can induce counter flow and co-flow, which is rarely investigated before. The axial velocity in the side layer near the first partitioning wall, which is located between the inflow channel and the first outflow channel, is the highest. ‘M-shaped’ velocity profiles are obtained in the side layers of the inflow and outflow channels. The interdependency of the current, fluid velocity, pressure, electric potential is examined in order to describe the electromagnetic characteristics of the liquid-metal flows.

Keywords: liquid-metal, multiple channels, magnetic field, magnetohydrodynamic

Procedia PDF Downloads 280

Authors: M. O. Bayram, H. B. Gencdal, N. O. Fercan, B. Basbug

Abstract:

Liquid limit, which is used as a measure of soil strength, can be detected by Casagrande and fall-cone testing methods. The two methods majorly diverge from each other in terms of operator dependency. The Casagrande method that is applied according to ASTM D4318-17 standards may give misleading results, especially if the calibration process is not performed well. To reveal the effect of calibration for drop height and amount of soil paste placement in the Casagrande cup, a series of tests were carried out by multipoint method as it is specified in the ASTM standards. The tests include the combination of 6 mm, 8 mm, 10 mm, and 12 mm drop heights and under-filled, half-filled, and full-filled Casagrande cups by kaolinite samples. It was observed that during successive tests, the drop height of the cup deteriorated; hence the device was recalibrated before and after each test to provide the accuracy of the results. Besides, the tests by under-filled and full-filled samples for higher drop heights revealed lower liquid limit values than the lower drop heights revealed. For the half-filled samples, it was clearly seen that the liquid limit values didn’t change at all as the drop height increased, and this explains the function of standard specifications.

Keywords: calibration, casagrande cup method, drop height, kaolinite, liquid limit, placing form

Procedia PDF Downloads 158

Authors: I. Ben Kaddour, S. Larbaoui

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Since their first synthesis in 1984, silicoaluminophosphates have proven their effectiveness as a good adsorbent and catalyst in several environmental and energy applications. In this work, the photocatalytic reaction of the photo-degradation of a pharmaceutical product in water was carried out in the presence of a series of materials based on titanium oxide, anatase phase, supported on the microporous framework of the SAPO4-5 at different levels, under ultraviolet light. These photo-catalysts were characterized by different physicochemical analysis methods in order to determine their structural, textural, and morphological properties, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), microscopy scanning electronics (SEM), nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS). In this study, liquid chromatography coupled with spectroscopy of mass (LC-MS) was used to determine the nature of the intermediate products formed during the photocatalytic degradation of DCF.

Keywords: photocatalysis, titanium dioxide, SAPO-5, diclofenac

Procedia PDF Downloads 66

Authors: Laissa Mae Francisco, John Rolex Ingreso, Anna Krizel Menguito, Criselda Robrigado, Rej Maegan Tuazon

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This study aims to determine and describe the existing relationship between number sense proficiency and problem-solving performance of grade seven students from Victorino Mapa High School, Manila. A paper pencil exam containing of 50-item number sense test and 5-item problem-solving test which measures their number sense proficiency and problem-solving performance adapted from McIntosh, Reys, and Bana were used as the research instruments. The data obtained from this study were interpreted and analyzed using the Pearson – Product Moment Coefficient of Correlation to determine the relationship between the two variables. It was found out that students who were low in number sense proficiency tend to be the students with poor problem-solving performance and students with medium number sense proficiency are most likely to have an average problem-solving performance. Likewise, students with high number sense proficiency are those who do excellently in problem-solving performance.

Keywords: number sense, performance, problem solving, proficiency

Procedia PDF Downloads 435

Authors: Weiwei Shan, Wenjing Ding, Juan Ning, Chao He, Zijuan Wang

Abstract:

Gravity circulation loop for the cryopumps of the space simulator is introduced, and two phase mathematic model of flow heat transfer is analyzed as well. Based on this model, the liquid nitrogen (LN₂) gravity circulation loop including its equipment and layout is designed and has served as LN₂ feeding system for cryopumps in one large space simulator. With the help of control software and human machine interface, this system can be operated flexibly, simply, and automatically under four conditions. When running this system, the results show that the cryopumps can be cooled down and maintained under the required temperature, 120 K.

Keywords: cryopumps, gravity circulation loop, liquid nitrogen, two-phase

Procedia PDF Downloads 398

Authors: Zlatina Peteva, Stanislava Georgieva, Mona Stancheva, Lubomir Makedonsky

Abstract:

Yessotoxins (YTX) and pectenotoxins (PTX) are lipophilic polyether marine biotoxins that accumulate in shellfish and are regulated in the European Union. Aim of this study is investigation of the presence of YTXs and PTXs in Black Sea mussel (Mytilus galloprovincialis) on the North Black Sea cast of Bulgaria. YTX and PTX-2 have been identified in samples of the digestive glands of wild and cultivated samples. Mussel samples are harvested from two locations in important farming area on the Bulgarian North Black Sea coast in the period September 2016 – May 2017. Samples are analyzed by liquid chromatography tandem mass spectrometry (LC–MS/MS). In about 50 % of the samples analyzed the obtained concentration of YTX ranged from 10 – 5000 pg/g hepatopancreas and PTX-2 ranged from 300-7000 pg/g hepatopancreas. This is to our knowledge the first report of occurrence of lipophilic toxins in mussels from Bulgaria.

Keywords: yessotoxins, pectenotoxins, Black sea, mussels

Procedia PDF Downloads 149

Authors: M. V. Bartashevich

Abstract:

The problem of heat transfer at thin laminar liquid film is solved numerically. A thin film of liquid flows down an inclined surface under conditions of variable heat flux on the wall. The use of thin films of liquid allows to create the effective technologies for cooling surfaces. However, it is important to investigate the most suitable cooling regimes from a safety point of view, in order, for example, to avoid overheating caused by the ruptures of the liquid film, and also to study the most effective cooling regimes depending on the character of the distribution of the heat flux on the wall, as well as the character of the blowing of the film surface, i.e., the external shear stress on its surface. In the statement of the problem on the film surface, the heat transfer coefficient between the liquid and gas is set, as well as a variable external shear stress - the intensity of blowing. It is shown that the combination of these factors - the degree of uniformity of the distribution of heat flux on the wall and the intensity of blowing, affects the efficiency of heat transfer. In this case, with an increase in the intensity of blowing, the cooling efficiency increases, reaching a maximum, and then decreases. It is also shown that the more uniform the heating of the wall, the more efficient the heat sink. A separate study was made for the flow regime along the horizontal surface when the liquid film moves solely due to external stress influence. For this mode, the analytical solution is used for the temperature at the entrance region for further numerical calculations downstream. Also the influence of the degree of uniformity of the heat flux distribution on the wall and the intensity of blowing of the film surface on the heat transfer efficiency was also studied. This work was carried out at the Kutateladze Institute of Thermophysics SB RAS (Russia) and supported by FASO Russia.

Keywords: Heat Flux, Heat Transfer Enhancement, External Blowing, Thin Liquid Film

Procedia PDF Downloads 148

Authors: Monica Rosa Loizzo, Tiziana Falco, Marco Bonesi, Maria Concetta Tenuta, Mariarosaria Leporini, Rosa Tundis

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Extra Virgin Olive Oil (EVOO) is a major source of fat in the Mediterranean diet and its nutritional properties are the main reason for the increment of its consumption all over the world in recent years. In terms of olive oil production, Italy ranks the second in the world. EVOO is obtained exclusively by physical methods from the fruit of Olea europea L. Frantoio cv is spread in all the Italian territory. The aim of this work is to identify the phenolic and fatty acids profile of EVOO from Frantoio cv growing in different area of Calabria (Italy). The phenolic profile was obtained by HPLC coupled to a diode array detector and mass spectrometry. Analyses revealed the presence of phenolic alcohols, phenolic acid, several secoiridoids, and two flavones as main components. Hydroxytyrosol and tyrosol are present in reasonable content. Fatty acids were monitored by gas chromatography. Oleic acid was the most abundant compounds. A moderate level of linoleic acid, in accordance with the general observations for oils derived from Mediterranean countries, was also found.

Keywords: extra virgin olive oils, frantoio cv, phenolic compounds, fatty acids

Procedia PDF Downloads 361

Authors: Chebbah Kaoutar, Marchioni Eric, Menad Ahmed, Mekkiou Ratiba, Sarri Djamel, Ameddah Souad, Boumaza Ouahiba, Seghiri Ramdane, Benayache Samir, Benayache Fadila

Abstract:

This study was designed to estabilish a preliminary phytochemical screening, evaluate the phenolic and flavonoid content according to the Folin-Ciocalteu procedure, and aluminum chloride method respectively and to determine qualitatively, using HPLC-UV method, the most important products present in ethyl acetate (EtOAc) and n-butanol (n-BuOH) extracts of the aerial parts of Genista cephalantha Spach. from East Algeria. The antioxidant activity of these extracts was spectrophotometrically tested by measuring their ability to scavenge a stable DPPH free radical and by β-Carotene/linoleic acid bleaching assay. Evaluated extracts showed a good activity in both antioxidant system assays.

Keywords: phenolic compounds, flavonoids, HPLC-DAD-UV, antioxidant activity, genista cephalantha, fabaceae

Procedia PDF Downloads 528

Authors: Masoud Gholam Ale Mohammad, Mojtaba Hafezi Birgani

Abstract:

An experimental study of saturated pool boiling on a single artificial nucleation site without and with the application of an electric field on the boiling surface has been conducted. N-pentane is boiling on a copper surface and is recorded with a high speed camera providing high quality pictures and movies. The accuracy of the visualization allowed establishing an experimental bubble growth law from a large number of experiments. This law shows that the evaporation rate is decreasing during the bubble growth, and underlines the importance of liquid motion induced by the preceding bubble. Bubble rise is therefore studied: once detached, bubbles accelerate vertically until reaching a maximum velocity in good agreement with a correlation from literature. The bubbles then turn to another direction. The effect of applying an electric field on the boiling surface in finally studied. In addition to changes in the bubble shape, changes are also shown in the liquid plume and the convective structures above the surface. Lower maximum rising velocities were measured in the presence of electric fields, especially with a negative polarity.

Keywords: single and double bubbles, electric field, boiling, rising

Procedia PDF Downloads 225

Authors: M. Javadzadeh, H. Khoshsima

Abstract:

In this article, we present a layout printing way for producing Fresnel zone on 1294-1b doped liquid crystal with Methyl-Red azo dye. We made a Fresnel zone mask with 25 zones and radius of 5 mm using lithography technique. With layout printing way, we recorded mask’s pattern on cell with λ=532 nm solid-state diode pump laser. By recording Fresnel zone pattern on cell and making Fresnel pattern on the surface of cell, odd and even zones, will form. The printed pattern, because of Azo dye’s photoisomerization, was permanent. Experimentally, we saw focal length tunability from 32 cm to 43 cm.

Keywords: liquid crystal, lens, Fresnel zone, diffraction, Fresnel lens

Procedia PDF Downloads 202

Authors: Omolola R. Ayepola, Nicole L. Brooks, Oluwafemi O. Oguntibeju

Abstract:

The liver plays an important role in the regulation of blood glucose and is a target organ of hyperglycaemia. Hyperglycemia plays a crucial role in the onset of various liver diseases and may culminate into hepatopathy if untreated. Alteration in antioxidant defense and increase in oxidative stress that results in tissue injury is characteristic of diabetes. We evaluated the protective effects of kolaviron-a biflavonoid complex, on hepatic antioxidants, lipid peroxidation and apoptosis in the liver of diabetic rats. To induce type I diabetes, rats were injected with streptozotocin intraperitoneally at a single dose of 50 mg/kg. Oral treatment of diabetic rats with kolaviron (100 mg/kg) started on the 6th day after diabetes induction and continued for 6 weeks (5 times weekly). Diabetic rats exhibited a significant increase in the peroxidation of hepatic lipids as observed from the elevated level of malondialdehyde (MDA) estimated by High-Performance Liquid Chromatography. In addition, Oxygen Radical Absorbance Capacity (ORAC), ratio of reduced to oxidized glutathione (GSH/GSSG) and catalase (CAT) activity was decreased in the liver of diabetic rats. TUNEL assay revealed increased apoptotic cell death in the liver of diabetic rats. Examination of Pancreatic beta-cells by immunohistochemical methods revealed beta cell degeneration and reduction in beta cell/ islet area in the diabetic controls. Kolaviron-treatment increased the area of insulin immunoreactive beta-cells significantly. Kolaviron attenuated lipid peroxidation and apoptosis in the liver of diabetic rats, increased CAT activity GSH levels and the resultant GSH: GSSG. The ORAC of kolaviron-treated diabetic liver was restored to near-normal values. Kolaviron protects the liver against oxidative and apoptotic damage induced by hyperglycemia. The antidiabetic effect of kolaviron may also be related to its beneficial effects on beta-cell function.

Keywords: diabetes mellitus, kolaviron, oxidative stress, liver, apoptosis

Procedia PDF Downloads 383

Authors: Ahmed Tafraoui, Gilles Escadeillas, Thierry Vidal

Abstract:

The southern Algeria is known for its huge sand dunes that cover part of its territory (Sahara). This sand has features that allow a glimpse of a recovery in the construction field in the form of Ultra High Performance Concrete (UHPC). This type of concrete using a large amount of silica fume, ultra fine addition that gives very high performance but is also relatively rare and expensive. Replacing it with another addition to equivalent properties, such as metakaolin, can also be considered. The objective of this study is to both enhance the sand dunes of Erg south west western Algeria but also reduce manufacturing costs of Ultra High Performance Concrete to incorporating metakaolin to instead of silica fume. Performances to determine mechanical performance are instantaneous, compression and bending. Initially, we characterized the Algerian sand dune. Then, we have to find a formulation of UHPC, adequate in terms of implementation and to replace silica fume by metakaolin. Finally, we studied the actual value of the sand dune. Concrete obtained have very high mechanical performance, up to a compressive strength of 250 MPa, a tensile strength of 45 MPa by bending with the method of heat treatment. This study shows that the enhancement of dune sand studied is quite possible in UHPC, and in particular UHPC bundles and the replacement of silica fume by metakaolin do not alter the properties of these concretes.

Keywords: Ultra High Performance Concrete, sand dune, formulations, silica fume, metakaolin, strength

Procedia PDF Downloads 468