Search results for: isothermal titration calorimetry (ITC)

Authors: Maryam Nejat Dehkordi, Per Lincoln, Hassan Momtaz

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Interaction of Schiff base complexes of iron and manganese (iron [N, N’ Bis (5-(triphenyl phosphonium methyl) salicylidene) -1, 2 ethanediamine) chloride, [Fe Salen]Cl, manganese [N, N’ Bis (5-(triphenyl phosphonium methyl) salicylidene) -1, 2 ethanediamine) acetate) with DNA were investigated by spectroscopic and isothermal titration calorimetry techniques (ITC). The absorbance spectra of complexes have shown hyper and hypochromism in the presence of DNA that is indication of interaction of complexes with DNA. The linear dichroism (LD) measurements confirmed the bending of DNA in the presence of complexes. Furthermore, isothermal titration calorimetry experiments approved that complexes bound to DNA on the base of both electrostatic and hydrophobic interactions. Furthermore, ITC profile exhibits the existence of two binding phases for the complex. Antibacterial activity of ligand and complexes were tested in vitro to evaluate their activity against the gram positive and negative bacteria.

Keywords: Schiff base complexes, ct-DNA, linear dichroism (LD), isothermal titration calorimetry (ITC), antibacterial activity

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Authors: Rohit Singh Dangi, Ravi Kant Pal, Monica Sundd

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Acyl-CoA binding protein (ACBP) is a housekeeping protein which functions as an intracellular carrier of acyl-CoA esters. Given the fact that the amastigote stage (blood stage) of Leishmania depends largely on fatty acids as the energy source, of which a large part is derived from its host, these proteins might have an important role in its survival. In Leishmania major, genome sequencing suggests the presence of six ACBPs, whose function remains largely unknown. For functional and structural characterization, one of the ACBP genes was cloned, and the protein was expressed and purified heterologously. Acyl-CoA ester binding and stoichiometry were analyzed by isothermal titration calorimetry and Dynamic light scattering. Our results shed light on high affinity of ACBP towards longer acyl-CoA esters, such as myristoyl-CoA to arachidonoyl-CoA with single binding site. To understand the binding mechanism & dynamics, Nuclear magnetic resonance assignments of this protein are being done. The protein's crystal structure was determined at 1.5Å resolution and revealed a classical topology for ACBP, containing four alpha-helical bundles. In the binding pocket, the loop between the first and the second helix (16 – 26AA) is four residues longer from other extensively studied ACBPs (PfACBP) and it curls upwards towards the pantothenate moiety of CoA to provide a large tunnel space for long acyl chain insertion.

Keywords: acyl-coa binding protein (ACBP), acyl-coa esters, crystal structure, isothermal titration, calorimetry, Leishmania

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Authors: Rishi Sharma, S. N. Maiti

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The non-isothermal crystallization kinetics of PP/SEBS-g-MA blends up to 0-50% concentration of copolymer was studied by differential scanning calorimetry at four different cooling rates. Crystallization parameters were analyzed by Avrami and Jeziorny models. Primary and secondary crystallization processes were described by Avrami equation. Avrami model showed that all types of shapes grow from small dimensions during primary crystallization. However, three-dimensional crystal growth was observed during the secondary crystallization process. The crystallization peak and onset temperature decrease, however

Keywords: crystallization kinetics, non-isothermal, polypropylene, SEBS-g-MA

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Authors: Naveed Ahmad, Farooq Ahmad, Abdul Aal Al-Khazaal

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Rheology can be used as a tool to examine the crystallization kinetics of polymers and polymer composites, and it provides more accurate results than the commonly used conventional techniques like differential scanning calorimetry (DSC) when the crystallization kinetics are slow. Crystallization occurs when crystalline polymers are cooled below their thermodynamic melting point temperature. At the start of this process, there is a gradual change in the mechanical response of the material from the liquid to the solid state, which is due to the change at the microstructure level of the polymer and polymer composites. This is one of the main characteristics of the rheological methodology that sets it apart from the conventional DSC method. In the present work, we used both rheological and differential scanning calorimetric techniques to perform both isothermal and non-isothermal crystallization experiments on a range of syndiotactic polypropylenes/clay composites with varying doses of clay contents in order to investigate the crystallization behavior of the materials. The objective of this work is to explore the effect of clay contents on the crystallization behavior of the syndiotactic polypropylene/clay composites and to couple the rheological methods with more conventional techniques such as Differential Scanning Calorimetry (DSC). Time sweep tests at a constant heating rate of 40°C/minutes were used to investigate the crystallization kinetics using the Atomic Rheumetric Expansion System (ARES). Crystallization behavior was found to be strongly dependent on the clay contents of syndiotactic polypropylene/clay composites. Both melting point (Tₘ) and crystallization temperatures (T𝒸) were found to increase with an increase in clay contents. Excellent agreement is found between the results obtained by both the rheological and differential scanning calorimetric (DSC) methods.

Keywords: quiescent crystallization, polymer composites, rheology, differential scanning calorimetry, syndiotactic polypropylene/clay composites

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Authors: A. Azizi, M. Toubane, L. Chetibi

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Differential scanning calorimetry (DSC) is a widely used technique for the study of phase transformations, particularly in the study of precipitation. The kinetic of the precipitation and dissolution is always related to the concept of activation energy Ea. The determination of the activation energy gives important information about the kinetic of the precipitation reaction. In this work, we were interested in the study of the isothermal and non-isothermal treatments on the decomposition of the supersaturated solid solution in the alloy AZ91 (Mg-9 Al-Zn 1-0.2 Mn. mass fraction %), using Differential Calorimetric method. Through this method, the samples were heat treated up to 425° C, using different rates. To calculate the apparent activation energies associated with the formation of precipitated phases, we used different isoconversional methods. This study was supported by other analysis: X-ray diffraction and microhardness measurements.

Keywords: calorimetric, activation energy, AZ91 alloys, microstructural evolution

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Authors: Poonam Yadav, Dong Bok Lee

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Isothermal oxidation at 800°C for 50h and Cyclic oxidation at 600°C and 800°C for 40h of Pure Ti and Ti64 were performed in a muffle furnace. In Cyclic oxidation, massive scale spallation occurred, and the oxide scale cracks and peels off were observed at high temperature, it represents oxide scale that formed during cyclic oxidation was spalled out owing to stresses due to thermal shock generated during repetitive oxidation and subsequent cooling. The thickness of scale is larger in cyclic oxidation than the isothermal case. This is due to inward diffusion of oxygen through oxide scales and/or pores and cracks in cyclic oxidation.

Keywords: cyclic, diffusion, isothermal, cyclic

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Authors: Can Yao, Chang Dong Sheng

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The heat released by wood pellets during storage will cause self-heating and even self-ignition. In this work, the heat release rates of pine, fir wood and mahogany pellets at 30–70℃ were measured by TAM air isothermal calorimeter, and the kinetic analysis was performed by iso-conversion ratio and non-steady-state methods to evaluate its self-heating potential. The results show that the reaction temperature can significantly affect the heat release rate. The higher the temperature, the greater the heat release rate. The heat release rates of different kinds of wood pellets are obviously different, and the order of the heat release rates for the three pellets at 70℃ is pine > fir wood > mahogany. The kinetic analysis of the iso-conversion ratio method indicates that the distribution of activation energy for pine, fir wood and mahogany pellets under the release of 0.1–1.0 J/g specific heat are 58–102 kJ/mol, 59–108 kJ/mol and 59–112 kJ/mol, respectively. Their activation energies obtained from the non-steady-state kinetic analysis are 13.43 kJ/mol, 19.19 kJ/mol and 21.09 kJ/mol, respectively. Both kinetic analyses show that the magnitude of self-heating risk for the three pellet fuels is pine pellets > fir wood pellets > mahogany pellets.

Keywords: isothermal calorimeter, kinetics, self-heating, wood pellets

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Authors: Charine Faith H. Lagrimas, Rommel N. Galvan, Rizalinda L. de Leon

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An ongoing study, methyl laurate to be used as a refrigerant in an HVAC system, requires the crystallization kinetics of the said substance. Step-wise and normal forms of Avrami model parameters were used to describe the isothermal crystallization kinetics of methyl laurate at different temperatures from Differential Scanning Calorimetry (DSC) measurements. At 3 °C, parameters showed that methyl laurate exhibits a secondary crystallization. The primary crystallization occurred with instantaneous nuclei and spherulitic growth; followed by a secondary instantaneous nucleation with a lower growth of dimensionality, rod-like. At 4 °C to 6 °C, the exotherms from DSC implied that the system was under the isokinetic range. The kinetics behavior is the same which is instantaneous nucleation with one-dimensional growth. The differences for the isokinetic range temperatures are the activation energies (directly proportional to T) and nucleation rates (inversely proportional to T). From the images obtained during the crystallization of methyl laurate using an optical microscope, it is confirmed that the nucleation and crystal growth modes obtained from the optical microscope are consistent with the parameters from Avrami model.

Keywords: Avrami model, isothermal crystallization, lipids kinetics, methyl laurate

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Authors: Hang Tran, Victor Brial, Luca Sorelli, Claudiane Ouellet-Plamondon, David Conciatori, Laurent Birry

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Spend pot lining (SPL) is a by-product generated from primary aluminum production. SPL consists of two parts, the first cut is rich in carbonaceous materials, and the second cut is rich in aluminum and silicon oxides. After treating by the hydrometallurgical Low Caustic Leaching and Liming process, the refractory part of SPL becomes an inert material, called LCLL ash in this project. LCLL ash was calcined at different temperatures (800 and 1000°C) and Calcined LCLL ash ground as fines of cement and replacement a part of cement in concrete production. The effect of LCLL ash on the chemical properties, mechanical properties and fresh behavior of concrete was evaluated by isothermal calorimetry, compressive test, and slump test. These results were compared to the reference mixture.

Keywords: spend pot lining, concrete, cement, compressive strength, calorimetry

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Authors: Aleksandra Twarda, Dobrosława Krzemień, Grzegorz Dubin, Tad A. Holak

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Stabilin-2 belongs to the group of scavenger receptors and plays a crucial role in clearance of more than 10 ligands from the bloodstream, including hyaluronic acid, products of degradation of extracellular matrix and metabolic products. The Link domain, a defining feature of stabilin-2, has a sequence similar to Link domains in other hyaluronic acid receptors, such as CD44 or TSG-6, and is responsible for most of ligands binding. Present knowledge of signal transduction by stabilin-2, as well as ligands’ recognition and binding mechanism, is limited. Until now, no experimental structures have been solved for any segments of stabilin-2. It has recently been demonstrated that the stabilin-2 knock-out or blocking of the receptor by an antibody effectively opposes cancer metastasis by elevating the level of circulating hyaluronic acid. Moreover, loss of expression of stabilin-2 in a peri-tumourous liver correlates with increased survival. Solving of the crystal structure of stabilin-2 and elucidation of the binding mechanism of hyaluronic acid could enable the precise characterization of the interactions in the binding site. These results may allow for designing specific small-molecule inhibitors of stabilin-2 that could be used in cancer therapy. To carry out screening for crystallization of stabilin-2, we cloned constructs of the Link domain of various lengths with or without surrounding domains. The folding properties of the constructs were checked by nuclear magnetic resonance (NMR). It is planned to show the binding of hyaluronic acid to the Link domain using several biochemical methods, i.a. NMR, isothermal titration calorimetry and fluorescence polarization assay.

Keywords: stabilin-2, Link domain, X-ray crystallography, NMR, hyaluronic acid, cancer

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Authors: Mufath Zorgani, Carlos Garcia-Mateo, Mohammad Jahazi

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In this study, the influence of pre-strained austenite on the extent of isothermal bainite transformation in medium-carbon, high-silicon steel was investigated. Different amounts of deformations were applied at 600°C on the austenite right before quenching to the region, where isothermal bainitic transformation is activated. Four different temperatures of 325, 350, 375, and 400°C considering similar holding time 1800s at each temperature, were selected to investigate the extent of isothermal bainitic transformation. The results showed that the deformation-free austenite transforms to the higher volume fraction of CFB bainite when the isothermal transformation temperature reduced from 400 to 325°C, the introduction of plastic deformation in austenite prior to the formation of bainite invariably involves a delay of the same or identical isothermal treatment. On the other side, when the isothermal transformation temperature and deformation increases, the volume fraction and the plate thickness of bainite decreases and the amount of retained austenite increases. The shape of retained austenite is mostly representing blocky-shape one due to the less amount of transformed bainite. Moreover, the plate-like shape bainite cannot be resolved when the deformation amount reached 30%, and the isothermal transformation temperatures are of 375 and 400°C. The amount of retained austenite and the percentage of its transformation to martensite during the final cooling stage play a significant role in the variation of hardness level for different thermomechanical regimes.

Keywords: ausforming, carbide free bainite, dilatometry, microstructure

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Authors: Poonam Yadav, Dong Bok Lee

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In this study, the Ti-6Al-4V alloy was isothermally and cyclically oxidized at 800oC for 40 hours in air, and its oxidation behavior was characterized in terms of its oxidation rate, scaling rate, and scale spallation tendency. The isothermal oxidation tests indicated that Ti-6Al-4V oxidized fast and almost linearly, forming thick oxide scales. However, the scales that formed during isothermal oxidation were adherent. The cyclic oxidation tests indicated that the scales that formed on Ti-6Al-4V were highly susceptible to spallation owing to the large growth stress arisen and the thermal stress imposed during thermal cyclings. The formed scales frequently delaminated into several pieces owing to the excessive stress aroused by the repetitive thermal shock. Particularly, excessive oxidation and heavy spallation occurred at the edge of Ti-6Al-4V during cyclic oxidation.

Keywords: cyclic, isothermal, oxidation, spallation

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Authors: Rita Ghosh, Joykrishna Dey

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PEG-based amphiphiles are of tremendous importance for its widespread applications in pharmaceutics, household purposes, and drug delivery. Previously, a number of single PEG-tailed amphiphiles having significant applications have been reported from our group. Therefore, it was of immense interest to explore the properties and application potential of PEG-based double tailed amphiphiles. Herein, for the first time, two novel double PEG-tailed amphiphiles having different PEG chain lengths have been developed. The self-assembly behavior of the newly developed amphiphiles in aqueous buffer (pH 7.0) was thoroughly investigated at 25 oC by a number of techniques including, 1H-NMR, and steady-state and time-dependent fluorescence spectroscopy, dynamic light scattering, transmission electron microscopy, atomic force microscopy, and isothermal titration calorimetry. Despite having two polar PEG chains both molecules were found to have strong tendency to self-assemble in aqueous buffered solution above a very low concentration. Surprisingly, the amphiphiles were shown to form stable vesicles spontaneously at room temperature without any external stimuli. The results of calorimetric measurements showed that the vesicle formation is driven by the hydrophobic effect (positive entropy change) of the system, which is associated with the helix-to-random coil transition of the PEG chain. The spectroscopic data confirmed that the bilayer membrane of the vesicles is constituted by the PEG chains of the amphiphilic molecule. Interestingly, the vesicles were also found to exhibit structural transitions upon addition of salts in solution. These properties of the vesicles enable them as potential candidate for drug delivery.

Keywords: double-tailed amphiphiles, fluorescence, microscopy, PEG, vesicles

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Authors: Tse-An Pan, Sheng-Long Lee

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The effect of non-isothermal aging on the mechanical properties and corrosion resistance of Al-9Zn-2.3Mg-1.9Cu (AA7056) alloys was investigated. The results revealed that thick materials were limited to retrogression and re-aging treatment (RRA). It could not reach the retrogression temperature in the RRA treatment. Compared with the RRA treatment, the non-isothermal aging (NIA) treatment produced discontinuous precipitates at grain boundaries, while the intragranular precipitates were fine and dense. The strength was similar to that of the RRA treatment; the corrosion resistance of the alloy was significantly improved by NIA aging. NIA treatment was less affected by the thickness of the alloy. The difference between the actual temperature and the setting temperature of the alloy is minimal during the aging process. The combination of properties could overcome the fact that RRA treatment cannot handle thick materials.

Keywords: Al-Zn-Mg-Cu alloy, corrosion, retrogression, re-aging, non-isothermal aging

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Authors: Kevin A. Droguett, Edwin G. Pérez, Denis Fuentealba, Margarita E. Aliaga, Angélica M. Fierro

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Supramolecular chemistry is a field of growing interest. Moreover, studying the formation of host-guest complexes between macrocycles and dyes is highly attractive due to their potential applications. Examples of the above are drug delivery, catalytic process, and sensing, among others. There are different dyes of interest in the literature; one example is the quinolinone derivatives. Those molecules have good optical properties and chemical and thermal stability, making them suitable for developing fluorescent probes. Secondly, several macrocycles can be seen in the literature. One example is the cucurbiturils. This water-soluble macromolecule family has a hydrophobic cavity and two identical carbonyl portals. Additionally, the thermodynamic analysis of those supramolecular systems could help understand the affinity between the host and guest, their interaction, and the main stabilization energy of the complex. In this work, two 7-(diethylamino) quinoline-2 (1H)-one derivative (QD1-2) and their interaction with cucurbit[7]uril (CB[7]) were studied from an experimental and in-silico point of view. For the experimental section, the complexes showed a 1:1 stoichiometry by HRMS-ESI and isothermal titration calorimetry (ITC). The inclusion of the derivatives on the macrocycle lends to an upward shift in the fluorescence intensity, and the pKa value of QD1-2 exhibits almost no variation after the formation of the complex. The thermodynamics of the inclusion complexes was investigated using ITC; the results demonstrate a non-classical hydrophobic effect with a minimum contribution from the entropy term and a constant binding on the order of 106 for both ligands. Additionally, dynamic molecular studies were carried out during 300 ns in an explicit solvent at NTP conditions. Our finding shows that the complex remains stable during the simulation (RMSD ~1 Å), and hydrogen bonds contribute to the stabilization of the systems. Finally, thermodynamic parameters from MMPBSA calculations were obtained to generate new computational insights to compare with experimental results.

Keywords: host-guest complexes, molecular dynamics, quinolin-2(1H)-one derivatives dyes, thermodynamics

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Authors: Minhal Abidi, Moinuddin

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Diabetes mellitus (DM) induced metabolic abnormalities causes oxidative stress which leads to the pathogenesis of complications associated with diabetes like retinopathy, nephropathy periodontitis etc. Combination of glycation and oxidation 'glycoxidation' occurs when oxidative reactions affect the early state of glycation products. Low density lipoprotein (LDL) is prone to glycoxidative attack by sugars and methylglyoxal (MGO) being a strong glycating agent may have severe impact on its structure and consequent role in diabetes. Pro-inflammatory cytokines like IL1β and TNFα produced by the action of gram negative bacteria in periodontits (PD) can in turn lead to insulin resistance. This work discusses modifications to LDL as a result of glycoxidation. The changes in the protein molecule have been characterized by various physicochemical techniques and the immunogenicity of the modified molecules was also evaluated as they presented neo-epitopes. Binding of antibodies present in diabetes patients to the native and glycated LDL has been evaluated. Role of modified epitopes in the generation of antibodies in diabetes and periodontitis has been discussed. The structural perturbations induced in LDL were analyzed by UV–Vis, fluorescence, circular dichroism and FTIR spectroscopy, molecular docking studies, thermal denaturation studies, Thioflavin T assay, isothermal titration calorimetry, comet assay. MALDI-TOF, ketoamine moieties, carbonyl content and HMF content were also quantitated in native and glycated LDL. IL1β and TNFα levels were also measured in the type 2 DM and PD patients. We report increased carbonyl content, ketoamine moieties and HMF content in glycated LDL as compared to native analogue. The results substantiate that in hyperglycemic state MGO modification of LDL causes structural perturbations making the protein antigenic which could obstruct normal physiological functions and might contribute in the development of secondary complications in diabetic patients like periodontitis.

Keywords: advanced glycation end products, diabetes mellitus, glycation, glycoxidation, low density lipoprotein, periodontitis

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Authors: Faisal A. Salih, V. V. Egorov

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Verapamil is a drug used in medicine for arrhythmia, angina, and hypertension as a calcium channel blocker. In this study, a Verapamil-selective electrode was prepared, and the concentrations of the components in the membrane were as follows: PVC (32.8 wt %), O-NPhOE (66.6 wt %), and KTPClPB (0.6 wt % or approximately 0.01 M). The inner solution containing verapamil hydrochloride 1 x 10⁻³ M was introduced, and the electrodes were conditioned overnight in 1 x 10⁻³ M verapamil hydrochloride solution in 1 x 10⁻³ M orthophosphoric acid. These studies have demonstrated that O-NPhOE and KTPClPB are the best plasticizers and ion exchangers, while both direct potentiometry and potentiometric titration methods can be used for the determination of verapamil hydrochloride in tablets and injection solutions. Normalized weights of verapamil per tablet (80.4±0.2, 80.7±0.2, 81.0±0.4 mg) were determined by direct potentiometry and potentiometric titration, respectively. Weights of verapamil per average tablet weight determined by the methods of direct potentiometry and potentiometric titration were" 80.4±0.2, 80.7±0.2 mg determined for the same set of tablets, respectively. The masses of verapamil in solutions for injection, determined by direct potentiometry for two ampoules from one set, were (5.00±0.015, 5.004±0.006) mg. In all cases, good reproducibility and excellent correspondence with the declared quantities were observed.

Keywords: verapamil, potentiometry, ion-selective electrode, lipophilic physiologically active amines

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Authors: S. Gvazava, N. Khidasheli, G. Gordeziani, A. DL. Batako

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The work presented in this paper studied the tribological characteristics (wear resistance, friction coefficient) of austempered ductile iron (ADI) with different combinations of structural composition (upper bainite, lower bainite, retained austenite) in dry sliding friction. A range of structural states of the metal matrix was obtained by changing the regimes of isothermal quenching of high-strength cast iron. The tribological tests were carried out using two sets of isothermal quenched cast irons. After austenitization at 900°С for 60 minutes, the specimens from the first group were isothermally quenched at the 300°С temperature and the specimens from the second set – at 400°С. The investigations showed that the isothermal quenching increases the friction coefficient of high-strength cast irons. The friction coefficient was found to be in the range from 0.4 to 0.55 for cast irons, depending on the structures of the metal matrix. The quenched cast irons having lower bainite demonstrate higher wear resistance in dry friction conditions. The dependence of wear resistance on the amount of retained austenite in isothermal quenched cast irons has a nonlinear characteristic and reaches its maximum value when the content of retained austenite is about 15-22%. The boron micro-additives allowed to reduce the friction coefficient of ADI and increase their wear resistance by 1.5-1.7 times.

Keywords: wear resistance, dry sliding, austempering, ADI, friction coefficient, retained austenite, isothermal quenching

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Authors: Mohammed S. Razali, Kamel Khimeche, Dahah Hichem, Ammar Boudjellal, Djamel E. Kaderi, Nourddine Ramdani

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The use of additive manufacturing technologies has revolutionized various aspects of our daily lives. In particular, 3D printing has greatly advanced biomedical applications. While fused filament fabrication (FFF) technologies have made it easy to produce or prototype various medical devices, it is crucial to minimize the risk of contamination. New materials with antibacterial properties, such as those containing compounded silver nanoparticles, have emerged on the market. In a previous study, we prepared a newly sintered seashell filler (SSh) from bio-based seashells found along the Mediterranean coast using a suitable heat treatment process. We then prepared a series of polylactic acid (PLA) and polybutylene succinate (PBS) biocomposites filled with these SSh particles using a melt mixing technique with a twin-screw extruder to use them as feedstock filaments for 3D printing. The study consisted of two parts: evaluating the antibacterial activity of newly prepared biocomposites made of PLA and PBS reinforced with a sintered seashell in the first part and experimental and modeling analysis of the non-isothermal crystallization kinetics of these biocomposites in the second part. In the first part, the bactericidal activity of the biocomposites against three different bacteria, including Gram-negative bacteria such as (E. coli and Pseudomonas aeruginosa), as well as Gram-positive bacteria such as (Staphylococcus aureus), was examined. The PLA-based biocomposite containing 20 wt.% of SSh particles exhibited an inhibition zone with radial diameters of 8mm and 6mm against E. coli and Pseudo. Au, respectively, while no bacterial activity was observed against Staphylococcus aureus. In the second part, the focus was on investigating the effect of the sintered seashell filler particles on the non-isothermal crystallization kinetics of PLA and PBS 3D-printing composite materials. The objective was to understand the impact of the filler particles on the crystallization mechanism of both PLA and PBS during the cooling process of a melt-extruded filament in (FFF) to manage the dimensional accuracy and mechanical properties of the final printed part. We conducted a non-isothermal melt crystallization kinetic study of a series of PLA-SS and PBS-SS composites using differential scanning calorimetry at various cooling rates. We analyzed the obtained kinetic data using different crystallization kinetic models such as modified Avrami, Ozawa, and Mo's methods. Dynamic mode describes the relative crystallinity as a function of temperature; it found that time half crystallinity (t1/2) of neat PLA decreased from 17 min to 7.3 min for PLA+5 SSh and the (t1/2) of virgin PBS was reduced from 3.5 min to 2.8 min for the composite containing 5wt.% of SSh. We found that the coated SS particles with stearic acid acted as nucleating agents and had a nucleation activity, as observed through polarized optical microscopy. Moreover, we evaluated the effective energy barrier of the non-isothermal crystallization process using the Iso conversional methods of Flynn-Wall-Ozawa (F-W-O) and Kissinger-Akahira-Sunose (K-A-S). The study provides significant insights into the crystallization behavior of PLA and PBS biocomposites.

Keywords: avrami model, bio-based reinforcement, dsc, gram-negative bacteria, gram-positive bacteria, isoconversional methods, non-isothermal crystallization kinetics, poly(butylene succinate), poly(lactic acid), antbactirial activity

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Authors: Marine Regnier, Pascal Bost, Matthieu Horgnies

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Some of the problems to be solved for the concrete industry are linked to the use of low-reactivity cement, the hardening of concrete under cold-weather and the manufacture of pre-casted concrete without costly heating step. The development of these applications needs to accelerate the hydration kinetics, in order to decrease the setting time and to obtain significant compressive strengths as soon as possible. The mechanisms enhancing the hydration kinetics of alite or Portland cement (e.g. the creation of nucleation sites) were already studied in literature (e.g. by using distinct additions such as titanium dioxide nanoparticles, calcium carbonate fillers, water-soluble polymers, C-S-H, etc.). However, the goal of this study was to establish a clear ranking of the efficiency of several types of additions by using a robust and reproducible methodology based on isothermal calorimetry (performed at 20°C). The cement was a CEM I 52.5N PM-ES (Blaine fineness of 455 m²/kg). To ensure the reproducibility of the experiments and avoid any decrease of the reactivity before use, the cement was stored in waterproof and sealed bags to avoid any contact with moisture and carbon dioxide. The experiments were performed on Portland cement pastes by using a water-to-cement ratio of 0.45, and incorporating different compounds (industrially available or laboratory-synthesized) that were selected according to their main composition and their specific surface area (SSA, calculated using the Brunauer-Emmett-Teller (BET) model and nitrogen adsorption isotherms performed at 77K). The intrinsic effects of (i) dry powders (e.g. fumed silica, activated charcoal, nano-precipitates of calcium carbonate, afwillite germs, nanoparticles of iron and iron oxides , etc.), and (ii) aqueous solutions (e.g. containing calcium chloride, hydrated Portland cement or Master X-SEED 100, etc.) were investigated. The influence of the amount of addition, calculated relatively to the dry extract of each addition compared to cement (and by conserving the same water-to-cement ratio) was also studied. The results demonstrated that the X-SEED®, the hydrated calcium nitrate, the calcium chloride (and, at a minor level, a solution of hydrated Portland cement) were able to accelerate the hydration kinetics of Portland cement, even at low concentration (e.g. 1%wt. of dry extract compared to cement). By using higher rates of additions, the fumed silica, the precipitated calcium carbonate and the titanium dioxide can also accelerate the hydration. In the case of the nano-precipitates of calcium carbonate, a correlation was established between the SSA and the accelerating effect. On the contrary, the nanoparticles of iron or iron oxides, the activated charcoal and the dried crystallised hydrates did not show any accelerating effect. Future experiments will be scheduled to establish the ranking of these additions, in terms of accelerating effect, by using low-reactivity cements and other water to cement ratios.

Keywords: acceleration, hydration kinetics, isothermal calorimetry, Portland cement

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Authors: Masato Nishi, Tetsushi Kaburagi, Masashi Kurose, Tei Hirashima, Tetsusei Kurasiki

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The process of thermoforming a carbon fiber reinforced thermoplastic (CFRTP) has increased its presence in the automotive industry for its wide applicability to the mass production car. A non-isothermal forming for CFRTP can shorten its cycle time to less than 1 minute. In this paper, the textile reinforcement FE model which the authors proposed in a previous work is extended to the CFRTP model for non-isothermal forming simulation. The effect of thermoplastic is given by adding shell elements which consider thermal effect to the textile reinforcement model. By applying Reuss model to the stress calculation of thermoplastic, the proposed model can accurately predict in-plane shear behavior, which is the key deformation mode during forming, in the range of the process temperature. Using the proposed model, thermoforming simulation was conducted and the results are in good agreement with the experimental results.

Keywords: carbon fiber reinforced thermoplastic, finite element analysis, pre-impregnated textile composite, non-isothermal forming

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Authors: Rhoda Afriyie Mensah, Lin Jiang, Solomon Asante-Okyere, Xu Qiang, Cong Jin

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Flammability analysis of extruded polystyrene (XPS) has become crucial due to its utilization as insulation material for energy efficient buildings. Using the Kissinger-Akahira-Sunose and Flynn-Wall-Ozawa methods, the degradation kinetics of two pure XPS from the local market, red and grey ones, were obtained from the results of thermogravity analysis (TG) and microscale combustion calorimetry (MCC) experiments performed under the same heating rates. From the experiments, it was discovered that red XPS released more heat than grey XPS and both materials showed two mass loss stages. Consequently, the kinetic parameters for red XPS were higher than grey XPS. A comparative evaluation of activation energies from MCC and TG showed an insignificant degree of deviation signifying an equivalent apparent activation energy from both methods. However, different activation energy profiles as a result of the different chemical pathways were presented when the dependencies of the activation energies on extent of conversion for TG and MCC were compared.

Keywords: flammability, microscale combustion calorimetry, thermogravity analysis, thermal degradation, kinetic analysis

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Authors: Tao Liu, Qingliang Yu, H. J. H. Brouwers

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Among the reaction products in the alkali-activated ground granulated blast furnace slag (AAS), the layered double hydroxides (LDHs) have a remarkable capacity of chloride and heavy metal ions absorption. The promotion of LDH phases in the AAS matrix can increase chloride resistance. The objective of this study is that use the different dosages of sodium aluminate to activate slag, consequently promoting the formation of in-situ LDH. The hydration kinetics of the sodium aluminate activated slag (SAAS) was tested by the isothermal calorimetry. Meanwhile, the reaction products were determined by X-ray diffraction (XRD), thermogravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FTIR). The sodium hydroxide-activated slag is selected as the reference. The results of XRD, TGA, and FTIR showed that the formation of LDH in SAAS was increased by the aluminate dosages.

Keywords: ground granulated blast furnace slag, sodium aluminate activated slag, in-situ LDH formation, chloride absorption

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Authors: Jose Neri, Fabrice Canto, Alastair Magnaldo, Laurent Guillerme, Vincent Dugas

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A miniaturized and automated approach for the volumetric titration of free nitric acid in U(VI) solutions is presented. Free acidity measurement refers to the acidity quantification in solutions containing hydrolysable heavy metal ions such as U(VI), U(IV) or Pu(IV) without taking into account the acidity contribution from the hydrolysis of such metal ions. It is, in fact, an operation having an essential role for the control of the nuclear fuel recycling process. The main objective behind the technical optimization of the actual ‘beaker’ method was to reduce the amount of radioactive substance to be handled by the laboratory personnel, to ease the instrumentation adjustability within a glove-box environment and to allow a high-throughput analysis for conducting more cost-effective operations. The measurement technique is based on the concept of the Taylor-Aris dispersion in order to create inside of a 200 μm x 5cm circular cylindrical micro-channel a linear concentration gradient in less than a second. The proposed analytical methodology relies on the actinide complexation using pH 5.6 sodium oxalate solution and subsequent alkalimetric titration of nitric acid with sodium hydroxide. The titration process is followed with a CCD camera for fluorescence detection; the neutralization boundary can be visualized in a detection range of 500nm- 600nm thanks to the addition of a pH sensitive fluorophore. The operating principle of the developed device allows the active generation of linear concentration gradients using a single cylindrical micro channel. This feature simplifies the fabrication and ease of use of the micro device, as it does not need a complex micro channel network or passive mixers to generate the chemical gradient. Moreover, since the linear gradient is determined by the liquid reagents input pressure, its generation can be fully achieved in faster intervals than one second, being a more timely-efficient gradient generation process compared to other source-sink passive diffusion devices. The resulting linear gradient generator device was therefore adapted to perform for the first time, a volumetric titration on a chip where the amount of reagents used is fixed to the total volume of the micro channel, avoiding an important waste generation like in other flow-based titration techniques. The associated analytical method is automated and its linearity has been proven for the free acidity determination of U(VI) samples containing up to 0.5M of actinide ion and nitric acid in a concentration range of 0.5M to 3M. In addition to automation, the developed analytical methodology and technique greatly improves the standard off-line oxalate complexation and alkalimetric titration method by reducing a thousand fold the required sample volume, forty times the nuclear waste per analysis as well as the analysis time by eight-fold. The developed device represents, therefore, a great step towards an easy-to-handle nuclear-related application, which in the short term could be used to improve laboratory safety as much as to reduce the environmental impact of the radioanalytical chain.

Keywords: free acidity, lab-on-a-chip, linear concentration gradient, Taylor-Aris dispersion, volumetric titration

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Authors: Wen Po Cheng, Chen Zhao Feng, Ruey Fang Yu, Lin Jia Jun, Lin Ji Ye, Chen Yuan Wei

Abstract:

Humic acid was used as the removal target for evaluating the coagulation efficiency in this study. When the coagulant ions mix with a humic acid solution, a Fluorescence quenching effect may be observed conditionally. This effect can be described by Stern-Volmer linear equation which can be used for quantifying the quenching value (Kq) of the Fluorescence quenching effect. In addition, a Complex-Formation Titration (CFT) theory was conducted and the result was used to explain the electron-neutralization capability of the coagulant (AlCl₃) at different pH. The results indicated that when pH of the ACl₃ solution was between 6 and 8, fluorescence quenching effect obviously occurred. The maximum Kq value was found to be 102,524 at pH 6. It means that the higher the Kq value is, the better complex reaction between a humic acid and aluminum salts will be. Through the Kq value study, the optimum pH can be quantified when the humic acid solution is coagulated with aluminum ions.

Keywords: humic acid, fluorescence quenching effect, complex reaction, titration

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Authors: Lin-Lin Liu, Song-Qi Hu, Yin Wang

Abstract:

Paraffin-based fuels are regarded to be a promising fuel of hybrid rocked motor because of the high regression rate, low price, and environmental friendliness. Graphene Oxide (GO) is an attractive energetic material which is expected to be widely used in propellants, explosives, and some high energy fuels. Paraffin-based fuels with paraffin and GO as raw materials were prepared, and the oxidation process of the samples was investigated by thermogravimetric analysis differential scanning calorimetry (TG/DSC) under oxygen (O₂) and nitrous oxide (N₂O) atmospheres. The oxidation reaction kinetics of the fuels was estimated through the non-isothermal measurements and model-free isoconversional methods based on the experimental results of TGA. The results show that paraffin-based fuels are easier oxidized under O₂ rather than N₂O with atmospheres due to the lower activation energy; GO plays a catalytic role for the oxidation of paraffin-based fuels under the both atmospheres, and the activation energy of the oxidation process decreases with the increase of GO; catalytic effect of GO on the oxidation of paraffin-based fuels are more obvious under O₂ atmospheres than under N₂O atmospheres.

Keywords: graphene oxide, paraffin-based fuels, oxidation, activation energy, TGA

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Authors: Joanna Gerszon, Aleksandra Rodacka

Abstract:

In the pathogenesis of neurodegenerative diseases such as Alzheimer's disease and Parkinson's disease, protein and peptide aggregation processes play a vital role in contributing to the formation of intracellular and extracellular protein deposits. One of the major components of these deposits is the oxidatively modified glyceraldehyde-3-phosphate dehydrogenase (GAPDH). Therefore, the purpose of this research was to answer the question whether piceatannol, a stilbene derivative, counteracts and/or slows down oxidative stress-induced GAPDH aggregation. The study also aimed to determine if this natural occurring compound prevents unfavorable nuclear translocation of GAPDH in hippocampal cells. The isothermal titration calorimetry (ITC) analysis indicated that one molecule of GAPDH can bind up to 8 molecules of piceatannol (7.3 ± 0.9). As a consequence of piceatannol binding to the enzyme, the loss of activity was observed. Parallel with GAPDH inactivation the changes in zeta potential, and loss of free thiol groups were noted. Nevertheless, the ligand-protein binding does not influence the secondary structure of the GAPDH. Precise molecular docking analysis of the interactions inside the active center allowed to presume that these effects are due to piceatannol ability to assemble a covalent binding with nucleophilic cysteine residue (Cys149) which is directly involved in the catalytic reaction. Molecular docking also showed that simultaneously 11 molecules of ligand can be bound to dehydrogenase. Taking into consideration obtained data, the influence of piceatannol on level of GAPDH aggregation induced by excessive oxidative stress was examined. The applied methods (thioflavin-T binding-dependent fluorescence as well as microscopy methods - transmission electron microscopy, Congo Red staining) revealed that piceatannol significantly diminishes level of GAPDH aggregation. Finally, studies involving cellular model (Western blot analyses of nuclear and cytosolic fractions and confocal microscopy) indicated that piceatannol-GAPDH binding prevents GAPDH from nuclear translocation induced by excessive oxidative stress in hippocampal cells. In consequence, it counteracts cell apoptosis. These studies demonstrate that by binding with GAPDH, piceatannol blocks cysteine residue and counteracts its oxidative modifications, that induce oligomerization and GAPDH aggregation as well as it prevents hippocampal cells from apoptosis by retaining GAPDH in the cytoplasm. All these findings provide a new insight into the role of piceatannol interaction with GAPDH and present a potential therapeutic strategy for some neurological disorders related to GAPDH aggregation. This work was supported by the by National Science Centre, Poland (grant number 2017/25/N/NZ1/02849).

Keywords: glyceraldehyde-3-phosphate dehydrogenase, neurodegenerative disease, neuroprotection, piceatannol, protein aggregation

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Authors: Novriyanti Lubis, Riska Prasetiawati, Wulan Septiani

Abstract:

The quantitative analysis of vitamin C content from variations beverage packaging containing red guava (Psidium Guajava Linn) fruit juice had been done. In this study, four samples were obtained from the shopping center in Garut and Bandung City. Samples were tested quantitatively by 2,6-dichlorophenol indophenol titration method. The results showed different concentration of 4 samples consist of tetra pack packaging, tin, glass, and plastic bottles, such as; 17.99 mg/100 gr, 31.46 mg/100 gr, 13.00 mg/100 gr, and 12.01 mg/100 gr, respectively. These results indicated that the packaging variations affected the level of vitamin C content which was characterized by decreased levels of vitamin C. It means the levels of vitamin C from this research were not in accordance with nutritional value information on the packaging. Tetra pack packaging was the most stable compared to other packaging even though it had a shorter expired date than with other.

Keywords: vitamin C, variations beverage packaging, red guava, titration 2, 6- dichlorophenol indophenol

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Authors: Olena Mayboroda, Angel Gonzalez Benito, Jonathan Sabate Del Rio, Marketa Svobodova, Sandra Julich, Herbert Tomaso, Ciara K. O'Sullivan, Ioanis Katakis

Abstract:

DNA amplification is required for most molecular diagnostic applications but conventional PCR has disadvantages for field testing. Isothermal amplification techniques are being developed to respond to this problem. One of them is the Recombinase Polymerase Amplification (RPA) that operates at isothermal conditions without sacrificing specificity and sensitivity in easy-to-use formats. In this work RPA was used for the optical detection of solid-phase amplification of the potential biowarfare agent Yersinia pestis. Thiolated forward primers were immobilized on the surface of maleimide-activated microtitre plates for the quantitative detection of synthetic and genomic DNA, with elongation occurring only in the presence of the specific template DNA and solution phase reverse primers. Quantitative detection was achieved via the use of biotinylated reverse primers and post-amplification addition of streptavidin-HRP conjugate. The overall time of amplification and detection was less than 1 hour at a constant temperature of 37oC. Single-stranded and double-stranded DNA sequences were detected achieving detection limits of 4.04*10-13 M and 3.14*10-16 M, respectively. The system demonstrated high specificity with negligible responses to non-specific targets.

Keywords: recombinase polymerase amplification, Yersinia pestis, solid-phase detection, ELONA

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Authors: Palwinder Singh, Baljit Kaur, Sukhmeet Kaur

Abstract:

Amongst a library of rationally designed small peptides, (H)Gly-Gly-Phe-Leu(OMe) was identified, reducing prostaglandin production of COX-2 with IC50 60 nM vs. 6000 nM for COX-1. The 5 mg Kg-1 dose of this compound rescued albino mice by 80% from capsaicin-induced paw licking and recovered it by 60% from carrageenan-induced inflammation. The mode of action of the compound for targeting COX-2, iNOS, and VGSC was investigated by using substances P, L-arginine, and veratrine, respectively, as the biomarkers. The interactions of the potent compound with COX-2 were supported by the isothermal calorimetry experiments showing Ka 6.10±1.10x104 mol-1 and ΔG -100.3 k J mol-1 in comparison to Ka 0.41x103 ±0.09 mol-1 and ΔG -19.2±0.06 k J mol-1 for COX-1. This compound did not show toxicity up to 2000 mg Kg-1 dose. Furthermore, beyond the conventional mode of working with anti-inflammatory agents through enzyme inhibition, COX-2 was provided with a peptide-based alternate substrate. Proline-centered pentapeptide iso-conformational to arachidonic acid exhibited appreciable selectivity for COX-2 overcoming acetic acid and formalin-induced pain in rats to almost 80% and was treated as a substrate by the enzyme. Hence, we suggest small peptides as highly potent and promising candidates for their further development into an anti-inflammatory drug.

Keywords: small peptides, cyclooxygenase, inflammation, substrate

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