Flaxseed oil is one of the best sources of n-3 fatty acids, thus its adulteration with refined oils can lead to a reduction in its nutritional value and overall quality. The purpose of this study was to use the differential scanning calorimetry (DSC) technique to detect adulterations of cold-pressed flaxseed oil with refined rapeseed oil (RP). Based on the melting phase transition curve, parameters such as peak temperature (T), peak height (h), and percentage of area (P) were determined for pure and adulterated flaxseed oils with a RP concentration of 5, 10, 20, 30, 50% (w/w). Significant linear correlations (p ≤ 0.05) between the RP concentration and all DSC parameters were observed, except for h1. In order to assess the usefulness of the DSC technique for detecting adulterations, three chemometric approaches were compared: 1) classification models (Linear Discriminant Analysis, LDA Adaptive Regression Splines, MARS, Support Vector Machine, SVM, Artificial Neural Networks, ANNs); 2) regression models (Multiple Linear Regression, MLR, MARS, SVM, ANNs, PLS) and 3) a combined model of Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA). With the LDA model, the highest accuracy of 99.5% in classifying the samples, followed by ANN> SVM > MARS was achieved. Among the regression models, the ANN model showed the highest correlation between observed and predicted values (R= 0.996), while other models showed goodness of fit as following MARS> SVM> MLR. Comparing OPLS-DA and PLS methods, higher values of R2X(cum) =0.986 and Q2 =0.973 were observed with the PLS model than OPLS-DA. These results demonstrate the usefulness of the DSC technique combined with chemometrics for predicting the adulteration of cold-pressed flaxseed oil with refined rapeseed oil.

Abscisic acid (ABA) is a conserved “stress hormone” in unicellular organisms, plants and animals. In mammals, ABA and its receptors LANCL1 and LANCL2 stimulate insulin-independent cell glucose uptake and oxidative metabolism: overexpression of LANCL1/2 increases, and their si-lencing conversely reduces, mitochondrial number, respiration and proton gradient dissipation in muscle cells and in brown adipocytes. We hypothesized that the ABA/LANCL hor-mone/receptors system could be involved in thermogenesis. Heat production by LANCL1/2-overexpressing vs. double-silenced cells was compared in rat H9c2 cardiomyocytes with two different methods: differential temperature measurements using sensitive thermistor probes, and differential isothermal calorimetry. Results indicate that overexpressing cells generate an approx. double amount of thermal power compared with double-silenced cells, and that addition of ABA further doubles heat production in overexpressing cells. With the temperature probes, we find a time-scale of approx. 4 min for thermogenesis to “turn on” after nutrient addition. These results identify the ABA/LANCL hormone receptors system as a hitherto unknown regu-lator of cell thermogenesis. Pharmacologic means of increasing metabolic energy dissipation are considered a promising strategy to reduce oxidative stress and lipid accumulation at a cellular and organismic level: from this study, LANCL1-2 proteins emerge as targetable controllers of ther-mogenesis through their natural ligand ABA.

The effect of Mg particles on PLA's thermal, chemical, physical, and mechanical properties has been studied. The thermal and physical properties have been studied by differential scanning calorimetry, analysing the stability of the α and α’-crystals of the PLA. A colloidal route was used to introduce Mg particles inside the PLA matrix, ensuring a good dispersion of the particles. Materials with Mg contents from 0 to 10 wt.% have been prepared, with additions of polyethyleneimine (PEI) and polyethylene glycol (PEG). Fourier Transform Infrared Spectroscopy has been used to confirm the influence of Mg, PEI, and PEG on PLA properties. The mechanical properties have been measured with a universal tensile test machine on printed filaments via Fused Filament Fabrication (FFF), which were naturally aged to stable conditions. Filaments with and without a notch were studied to obtain the materials' tensile strength, elastic modulus, and fracture toughness. Different analytical models to explain the results of the PLA-Mg were studied, in which the interface strength of the PLA-Mg composites was calculated.

This work presents the synthesis and self-organization of the calamitic fluorinated mesogen, 1,1,2,2-tetrafluoro-2-(1,1,2,2-tetrafluoro-4-iodobutoxy)ethanesulfonic acid, a potential model for perfluorosulfonic acid membranes (PFSA). The compound is derived in three steps from 1,1,2,2-tetrafluoro-2-(1,1,2,2-tetrafluoro-2-iodoethoxy)ethanesulfonyl fluoride, achieving an 78% overall yield. The resulting compound exhibits intricate thermal behavior. At 150 °C, a crystal-to-crystal transition is observed due to the partial disordering of calamitic molecules, which is followed by isotropization at 218 °C. Upon cooling, sample ordering occurs through the formation of large smectic liquid crystalline phase domains. This thermotropic state transforms into a layered crystal phase at lower temperatures, characterized by alternating hydrophilic and hydrophobic layers. Using X-ray diffraction, crystalline unit cell models at both room temperature and 170 °C were proposed. Computer simulations of the molecule across varying temperatures support the idea that thermal transitions correlate with a loss of molecular orientation. Importantly, the study underscores the pivotal role of precursor self-organization in aligning channels during membrane fabrication, ensuring controlled and oriented positioning.

Frontal Polymerization (FP) is recognized as a polymer synthesis method capable of generating a highly localized and self-propagating exothermic front, considered a more rapid and energy-efficient manufacturing scheme for polymer-based fiber-reinforced composite materials. This study conducts a numerical investigation based on the Finite Element Method into the initiation and propagation of frontal polymerization of acrylamide. Utilizing Differential Scanning Calorimetry (DSC) experiments, the study phenomenologically tests the curing kinetics reactions of acrylamide (AM) in deep eutectic solvent (DES)-based polymerizable systems, thereby establishing a curing kinetics model for the autocatalytic reaction of polyacrylamide. By coupling the heat conduction diffusion equation of the frontal polymerization reaction, the Finite Element Method is employed to solve the reaction-diffusion model, aiming to explore the evolution of temperature and degree of curing during the manufacturing process. The results demonstrate the reliability and accuracy of the nth-order autocatalytic model in the study of curing kinetics for DES-based synthesis, indicating that the front propagation speed of the AM-based FP reaction is influenced by the activation temperature, duration of activation temperature, and initial temperature of the solution. Experimental validation of the polyacrylamide manufacturing through frontal polymerization corroborates the accuracy and reliability of the model predictions, providing a reference for the numerical model study and temperature control in the synthesis of acrylamide composite hydrogels via FP.

The goal of this study is to find out how some properties of wood-polymer nanocomposites are affected by the processing technology, the nanomaterials, and the ratio of coupling agents. To meet this objective, the extruded and dry blended samples are made from wood flour with MAPP, ZnO nanoparticles (0, 1, 3, and 5 wt%), and polypropylene. The mechanical properties of the nanocomposites improve significantly with ZnO and MAPP loading. Due to the more homogeneous structure of nanocomposites, better mechanical results are obtained with the extrusion method. With ZnO and MAPP loading, the thermal stability of nanocomposites improves. The storage and loss modulus values indicate that the processing technology of nanocomposites could be a key factor in the resistance of the materials obtained by extrusion. The storage and loss modulus of nanocomposites manufactured by the extrusion technology are determined to be higher than those of the samples produced by the dry blending method.

This study deals with vibrational and crystallographic aspects of the thermally induced transformation of serpentine-like garnierite into quartz, forsterite, and enstatite occurring at about 620 °C. Powder specimens of garnierite have been annealed in static air between room temperature and 1000 °C. The resulting products from the transformations detected based on thermogravimetric and differential thermal analysis, have been extensively characterized via microRaman spectroscopy, and X-ray diffraction. Our study shows that serpentine-like garnierite consists of a mixture of different mineral species. Furthermore, these garnierites and their composition can provide details based on the mineralogy and the crystalline phases resulting from the thermal treatment.

Poly lactic acid (PLA) has made inroads for commercial market segment with lot many unique characteristics such as tenacity, low flame rate, moisture regain percentage, loss of ignition percentage, heat of combustion, UV resistance, Elastic recovery and higher melting point allowed it to be the fastest moving material in today's commercial market. An attempt has been made to test the feasibility and biocompatibility aspect of PLA with cement mix. The basic strength and physical test results were carried out and published in an article, to the continuation of the work, micro-structural study was conducted to evaluate the elemental characteristics. Thermo gravimetric analysis revealed that PLA either in granular form or filament will hold good for the inclusion into construction applications, provided degradation aspects are to be looked out for improvisation. From DSC it was found that PLA in filament form is the best inclusion material for construction application, however the tenacity of fibers has to checked, as currently available filaments in market does not have high tenacity value. From EDX reports, 30% inclusion of PLA as replacement for fine aggregate has constituent members as Calcium carbonate(CaCO3), Silica(SiO2) and Wollastonite (CaK) resulted in best composition among the rest. FESEM images revealed that, proper gradation in size, rough surface of PLA granular form or filament form will definitely enhance the mechanical/physical or even chemical behavior of PLA.

Dye sensitized solar cell technology is having an important role in renewable energy research due to its features and low cost manufacturing processes. Devices based on this technology appear very well suited for integration into glazing systems due to their characteristics of transparency, color tuning and manufacturing directly on glass substrates. Field data of thermal and electrical characteristics of dye sensitized solar modules (DSM) are important since they can be used as input of building simulation models for the evaluation of their energy saving potential when integrated into buildings. However still few works in the literature provide this information. The study here presented wants to contribute to fill this gap providing a thermal and electrical characterization of a DSM in real operating conditions using a method developed in house. This method uses experimental data coming from test boxes exposed outdoor and dynamic simulation to provide thermal transmittance and solar heat gain coefficient (SHGC) of a DSM prototype. The device exhibits an U-value of 3.6 W/m²K, confirmed by an additional measurement carried on in the lab using a heat flux meter, and a SHGC of 0.2, value compliant with literature results. Electrical characterization evidences an increase of module power with respect to temperature causing DSM suitable for integration in building facades.

A homogenized, supersaturated Al-Zn-Mg-Zr alloy was processed by severe plastic deformation (SPD) using high-pressure torsion (HPT) technique for different revolutions at room temperature to get ultrafine-grained (UFG) microstructure. The microstructure and mechanical properties of the UFG samples were then studied by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), as well as by tensile and hardness measurements. Emphasis was placed on the effect of shear strain on the evolution of microstructure of the investigated alloy. Experimental results have shown a very interesting evolution of the decomposed microstructure in a wide range of shear strains imposed by HPT. While the global properties, such as the average grain size (~200 nm) and hardness (~2.2 GPa) appeared unchanged, the local microstructure was continuously transformed. After 1 turn of HPT, the decomposed UFG structure contains relatively large precipitates inside grains. In the sample processed by 5 turns in HPT, segregation of Zn atoms into grain boundaries (GBs) can also be observed. After 10 turns, more Zn atoms have segregated into GBs and only smaller size precipitates can be observed inside grains. The intensive segregation of solute atoms into GBs may significantly affect the ductility of the materials, leading to its ultralow-temperature superplasticity. Our findings pave the way for achieving advanced microstructural and mechanical properties in nanostructured metals and alloys by engineering their precipitation and segregation by means of applying different HPT regimes.

The effect of the melt cooling rate on the atomic ordering of austenite and, as a consequence, on the martensitic transformation of a nonstoichiometric alloy of the Ni-Mn-In system has been studied. In-situ TEM observations revealed differences in the mechanism of phase transformations of the alloy subjected to different cooling conditions. It is shown that during quenching a high density of antiphase boundaries (APB) is formed and the alloy is in the austenite-martensitic (10M and 14M) state up to a temperature of 120K. In a slowly cooled alloy, a lower APB density is observed, and a two-stage transformation L21/B2 → 10M → 14M occurs in the range of 150–120 K.

This study aimed to develop chitosan-based apigenin spray dried solid dispersion using 1:1,1:1.5,1:2 w/w ratios. The results of process yield and drug assay were found to be (87.5%, 94.2%, and 95.86%), (95.2 ±1.34%), (99.5 ±0.85%), and (97.6 ±2.42%), respectively, for AC1, AC2, and AC3. Flow properties indicate the free flow of powders. FTIR revealed compatibility among chitosan and apigenin, and DSC and XRD showed prepared solid dispersion was on a molecular level and available in amorphous. In contrast, SEM images reflect irregular block and near-spherical shape elongated particles in the selected AC2. The antimicrobial examination reflects that AC2 was more effective against Gram-positive, negative, and fungal strains. AC2 SDSDs has more anti-oxidant property compared to pure flavonoid (AGN). Anti-proliferative activity against A549 lung cancer cell lines showed better anti-cancer activity by AC2 SDSDs. The selected AC2 SDSD filled in a 3D shell pill and further characterized for 3D shell pill for dissolution profiles and stability studies. The product has sustained release and similar release profiles after three months of storage. The findings suggest that the AC2 SDSDs may be a promising candidate for further development as a 3D printed drug delivery system for treating multiple disease conditions using model flavonoid- apigenin.

Abstract: Agarose is known to form a homogeneous thermoreversible gel in aqueous medium over a critical polymer concentration. The solid-liquid phase transitions are thermoreversible but depend on the molecular structure of the agarose sample tested. Then, in a first step, the structure was characterised by 1H and 13C NMR in D2O and in DMSO which is a solvent of agarose whatever the temperature. A low yield in methyl substituent on the D-galactose unit was determined. Then, evolution of the 1H NMR spectrum was followed as a function of temperature in increasing and decreasing temperature process from 25 to 80°C. A large thermal hysteresis is obtained and discussed. It helps to interpret rheological behaviour. In fact, NMR signals are related to proton relaxation and especially to proton involved in H-bonds between water and -OH agarose for tightly bound water and agarose/agarose in chain packing. In a second step, water was exchanged against ethanol which is a non solvent of agarose. A stable gel was demonstrated and characterised by rheology to be compared with aqueous behaviour. Bound water playing the role of plasticizer is probably removed and the gel is much stronger (and brittle) in ethanol with a larger thermal stability. It is the first time that such gel is characterised without phase transition when passing from a good-solvent to a non-solvent. This extends the domains of application of agarose.

This paper describes the dielectric relaxation spectroscopy (DRS) method for obtaining glass transition temperature and the onset of crystallinity of skim milk powder (SMP). The methodology consists of exposing SMP samples to numerous constant temperatures, T, and water activities, a_w, and measuring the relaxation time. Measurements are based on changes in the loss-tangent height at its peak frequency. Glass transition times are identified at peaks in the loss-tangent height versus time curve and the onset of crystallinity times are identified when the loss-tangent height collapses. The analysis leads to two boundary curves: glass transition T_g, a_w curve and the onset of crystallinity T_c, a_w curve. They separate the SMP stable (long shelf life) and unstable (short shelf life) regions. Two curve fitting algorithms were developed for (a) a_w², t_g curve where t_g is the time to glass transition and a_w², t_c curve where time t_c is the time to onset of crystallinity and (b) T_g, a_w and T_c, a_w boundary curves. Finally, the DRS data are compared to differential scanning calorimetry (DSC) results.

When focusing on materials science in civil engineering, the current trend is to investigate the use of innovative solutions in order to enhance thermal and energy performances. This trend is amplified with the need for a sustainable development strategy for the construction sector. This paper assesses the integration of a Phase Change Material (PCM) in cement intended for building construction. The key characteristic of PCMs is their capacity to absorb energy and restore it. In building construction, this feature could be harnessed to save energy by incorporating PCMs in the materials used. In this study, passive integration of PCM in cement was tested and thermal properties of such an integration was assessed. The results provide insights into how PCMs affect cement as part of the concrete mixture, thus identifying the contribution of PCM-based cements in concrete mixtures.

The vulcanization of rubber compounds is an exothermal process. A carbon black-filled and natural rubber-based (NR) formulation was mixed with different levels of sulfur (0.5, 1.0, 2.0, 4.0 and 6.0 phr) and studied with Differential Scanning Calorimetry (DSC) for the determination of the vulcanization enthalpy. It was found that the vulcanization enthalpy is dependent from the amount of sulfur present in the compound and the vulcanization heat released was -18.4 kJ/mol S if referred to the entire rubber compound formulation or -46.0 kJ/mol S if the heat released is referred only to the NR present in the compound. The activation energy for the vulcanization of the rubber compounds was also determined by a DSC study at 49 kJ/mol and found quite independent from the sulfur content of the compounds under study. A simplified thermochemical model is proposed to explain the main reactions occurring during the vulcanization. The model correctly predicts that the vulcanization is an exothermal process although it gives an overestimation of the vulcanization enthalpy which is larger for the EV vulcanization package and smaller for the conventional vulcanization system. If the devulcanization is conducted mechanochemically in order to break selectively the sulfur-based crosslinks, then the natural rubber compounds recovered from used tires can be re-vulcanized again and the exothermicity of such process can be measured satisfactorily with DSC analysis. This paper not only proposes a simplified mechanism of vulcanization and devulcanization but also proposes an analytical method to check the devulcanization status of the recycled rubber compound in order to distinguish truly devulcanized rubber from reclaimed rubber.

Bone cement, mainly based in PMMA, is commonly used in different arthroplasty surgical proce-dures, and its use is essential for prosthesis fixation. However, its manufacturing process reaches high temperatures that can produce necrosis in the patients' surrounding tissues. In order to con-tribute to avoid this problem, the addition of graphene could delay the polymerisation of the MMA and, simultaneously, contribute to the optimisation of the composite material's properties. This article analysed the effect of the addition of different percentages of Highly Reduced Graphene Oxide (HRGO) with different wt. % (0,10, 0,50 and 1,00) and surface densities (150, 300, 500 and 750 m2/g) on the physical, mechanical, and thermal properties of commercial PMMA-based bone cement and its processing. It was noticed that a lower sintering temperature would be reached with this addition, making it less harmful to use in surgery and as it reduces its adverse effects. In contrast, the materials' density does not show significant changes, which indicates that the addi-tion of HRGO does not significantly increase its porosity. Lastly, the mechanical properties are re-duced by almost 20 %. Nevertheless, these properties are high enough so that these new materials can still fulfil their structural function.

Patients who have undergone surgery in early life may be at elevated risk for neuropathic pain in later life. The risk factors for this susceptibility are not fully understood. Here, we used a mouse chronic pain model to test the hypothesis that early exposure to general anesthetic (GA) causes cellular and molecular alterations in dorsal spinal cord (DSC) and dorsal root ganglion (DRG) that produces a predisposition to neuropathic pain via an upregulation of the mammalian target of the rapamycin (mTOR) signaling pathway. Mice were exposed to isoflurane at postnatal day 7 (P7) and underwent spared nerve injury at P28 which causes chronic pain. Selected groups were treated with rapamycin, an mTOR inhibitor, for eight weeks. Behavioral tests show early isoflurane exposure enhances susceptibility to chronic pain, and rapamycin treatment improves outcomes. Immunohistochemistry, Western blotting, and q-PCR indicates that isoflurane upregulates mTOR expression and neural activity in DSC and DRG. Accompanying upregulation of mTOR and rapamycin-reversible changes in chronic pain-associated markers, including N-cadherin, cAMP response element-binding protein (CREB), purinergic P2Y12 receptor, glial fibrillary acidic protein (GFAP) in DSC; and connexin 43, phospho-extracellular signal-regulated kinase (p-ERK), GFAP, Iba1 in DRG, were observed. We conclude that early GA exposure alters the development of pain circuits such that mice are subsequently more vulnerable to chronic neuropathic pain states.

The present study aimed to investigate the effect of cold deformation on the precipitation kinetics of a binary CuSc alloy containing 0.4 wt.% scandium using the experimental analysis method of differential scanning calorimetry (DSC). Non-deformed and 75% cross-section reduced cold-rolled, supersaturated specimens were tested at non-isothermal DSC runs at up to five different heating rates. The DSC results showed that cold deformation significantly accelerated the precipitation process in the binary alloy, leading to a decrease in the initial and peak temperatures of the exothermic reactions. The activation energies calculated with the Kissinger method, indicated that the precipitation activation energy decreased with increasing cold deformation. The findings of this study provide worthy implications to further optimize the processing of Cu-Sc alloys with improved mechanical properties.

In this study, 12 organic waste materials were subjected to TG/DTG thermogravimetric analysis and DSC calorimetric analysis. These analyses provided basic information about thermochemical transformations and degradation rates during organic waste pyrolysis. Waste materials were chosen to cover the most abundant waste that can be found in the municipal solid waste stream. Based on TG results, kinetic parameters according to Coats–Redfern method were determined. The pyrolysis activation energy was the highest for cotton 134.5 kJ∙(mol∙K)-1 and the lowest for leather 25.2 kJ∙(mol∙K)-1. The DSC analysis showed number of transformations occurred during pyrolysis for each material. For each transformation, normalized energy required for transformation, or released during transformation were determined and then summarized to present energy balance. The study found that only for three waste materials: PET (-220.1 J⸱g-1), leather (-66.9 J⸱g-1), and chicken meat (-130.3 J⸱g-1) energy balance was negative, while the highest positive balance value was found for potato peelings (367.8 J⸱g-1). The obtained results may be applied for the modelling of energy and mass balance of municipal solid waste pyrolysis.

The morphology of virgin reactor powder (RP) of high-density polyethylene HDPE with MW = 160,000 g/mol was investigated with the help of DSC, SEM, SAXS and WAXS methods. The morphological SEM analysis showed, that the main morphological units of RP are macro- and micro-shish kebab structures with significantly different geometric dimensions, as well as individual lamellae of folded chain crystals. Quantitative analysis of an asymmetric SAXS reflection made it possible to reveal the presence of several periodic morphoses in the RP with long periods from 20 nm to 60 nm and to correlate them with the observed powder morphology. According to the DSC crystallinity data, the thickness of the lamellae in each long period was estimated. Their surface energy was calculated in the framework of the Gibbs-Thompson theory. The presence of regular and irregular folds on the surface of the different shish-kebab lamellae is discussed. The percentage of identified morphoses in the RP was calculated. It has been suggested that the specific structure of HDPE RP is due to the peculiarity of polymer crystallization during suspension synthesis in a quasi-stationary regime, in which local overheating and inhomogeneous distribution of shear stresses in a chemical reactor are possible.

In this article, the research team has systematically developed a method to model the kinematics and dynamics of a 3-wheeled robot subjected to external disturbances and sideways wheel sliding. These models will be used to design control laws that compensate for wheel slippage, model uncertainties, and external disturbances. These are control algorithms developed based on Dynamic Surface Control (DSC). Adaptive trajectory tracking DSC algorithm using fuzzy logic system (AFDSC) and radial neural network (RBFNN) with fuzzy logic system to overcome the disadvantages of DSC and expand the application domain for wheeled Mobile Robots (WMR). However, this Adaptive Fuzzy Neural Network Dynamic Surface Control (AFNNDSC) adaptive controller ensures the closed system is stable and follows the preset trajectory in the presence of wheel slippage model uncertainty and is affected by significant amplitude disturbances. The stability and convergence of the closed-loop system are guaranteed based on the Lyapunov analysis. The AFNNDSC adaptive controller is evaluated by simulation on MATLAB/Simulink software and in a steady state. The maximum position error on the right wheel and left wheel is 0.000572 (m) and 0.000523 (m), and the angular velocity tracking error in the right and left wheels of the control method is 0.000394 (rad/s). The experimental results show the correctness of the theoretical analysis, the effectiveness of the proposed controller, and the possibility of practical application.