Search results for: fourier-transform infrared spectroscopy (FTIR)

Authors: Aleksandra BužArovska, Gordana Bogoeva Gaceva

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Biodegradable polymers have received significant scientific attention in tissue engineering (TE) application, in particular their composites consisting of inorganic nanoparticles. In the last 15 years, they are subject of intensive research by many groups, aiming to develop polymer scaffolds with defined biodegradability, porosity and adequate mechanical stability. The most important characteristic making these materials attractive for TE is their biodegradability, a process that could be time controlled and long enough to enable generation of a new tissue as a replacement for the degraded polymer scaffold. In this work poly(L-lactic acid) scaffolds, filled with TiO2 nanoparticles functionalized with oleic acid, have been prepared by thermally induced phase separation method (TIPS). The functionalization of TiO2 nanoparticles with oleic acid was performed in order to improve the nanoparticles dispersibility within the polymer matrix and at the same time to inhibit the cytotoxicity of the nanofiller. The oleic acid was chosen as amphiphilic molecule belonging to the fatty acid family because of its non-toxicity and possibility for mediation between the hydrophilic TiO2 nanoparticles and hydrophobic PLA matrix. The produced scaffolds were characterized with thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and mechanical compression measurements. The bioactivity for bone tissue engineering application was tested in supersaturated simulated body fluid. The degradation process was followed by Fourier transform infrared spectroscopy (FTIR). The results showed anisotropic morphology with elongated open pores (100 µm), high porosity (around 92%) and perfectly dispersed nanofiller. The compression moduli up to 10 MPa were identified independent on the nanofiller content. Functionalized TiO2 nanoparticles induced formation of hydroxyapatite clusters as much as unfunctionalized TiO2. The prepared scaffolds showed properties ideal for scaffold vascularization, cell attachment, growth and proliferation.

Keywords: biodegradation, bone tissue engineering, mineralization, PLA scaffolds

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Authors: Lucas Kurth de Azambuja, Loise Silveira da Silva, Gean Vitor Salmoria, Darlan Dallacosta, Carlos Rodrigo de Mello Roesler

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This work provides a physicochemical and thermal characterization assessment of three different hyaluronic acid (HA)-based injections used for rejuvenation skin treatments. The three products analyzed are manufactured by the same manufacturer and commercialized for application on different skin levels. According to the manufacturer, all three HA-based injections are crosslinked and have a concentration of 23 mg/mL of HA, and 0.3% of lidocaine. Samples were characterized by Fourier-transformed infrared (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and scanning electron microscope (SEM) techniques. FTIR analysis resulted in a similar spectrum when comparing the different products. DSC analysis demonstrated that the fusion points differ in each product, with a higher fusion temperature observed in specimen A, which is used for subcutaneous applications, when compared with B and C, which are used for the middle dermis and deep dermis, respectively. TGA data demonstrated a considerable mass loss at 100°C, which means that the product has more than 50% of water in its composition. TGA analysis also showed that Specimen A had a lower mass loss at 100°C when compared to Specimen C. A mass loss of around 220°C was observed on all samples, characterizing the presence of hyaluronic acid. SEM images displayed a similar structure on all samples analyzed, with a thicker layer for Specimen A when compared with B and C. This series of analyses demonstrated that, as expected, the physicochemical and thermal properties of the products differ according to their application. Furthermore, to better characterize the crosslinking degree of each product and their mechanical properties, a set of different techniques should be applied in parallel to correlate the results and, thereby, relate injection application with material properties.

Keywords: hyaluronic acid, characterization, soft-tissue fillers, injectable gels

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Authors: Hari Bezwada, Michelle Cheon, Ryan Divan, Hannah Escritor, Michelle Kagramian, Isha Korgaonkar, Maya MacAdams, Udgita Pamidigantam, Richard Pilny, Eleanor Race, Angadh Singh, Nathan Zhang, LeeAnn Nguyen, Fina Liotta

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Malaria is a deadly disease caused by the Plasmodium parasite, which continues to develop resistance to current antimalarial drugs. In this research project, the effectiveness of numerous thiazole derivatives was explored in inhibiting the PfPKG, a crucial part of the Plasmodium life cycle. This study involved the synthesis of six thiazole-derived amides to inhibit the PfPKG pathway. Nuclear Magnetic Resonance (NMR) spectroscopy and Infrared (IR) spectroscopy were used to characterize these compounds. Furthermore, AutoDocking software was used to predict binding affinities of these thiazole-derived amides in silico. In silico, compound 6 exhibited the highest predicted binding affinity to PfPKG, while compound 5 had the lowest affinity. Compounds 1-4 displayed varying degrees of predicted binding affinity. In-vitro, it was found that compound 4 had the best percent inhibition, while compound 5 had the worst percent inhibition. Overall, all six compounds had weak inhibition (approximately 30-39% at 10 μM), but these results provide a foundation for future drug discovery experiments.

Keywords: Medicinal Chemistry, Malaria, drug discovery, PfPKG, Thiazole, Plasmodium

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Authors: Nithin Krisshna Gunasekaran, Prathima Prabhu Tumkur, Nicole Nazario Bayon, Krishnan Prabhakaran, Joseph C. Hall, Govindarajan T. Ramesh

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Cerium oxide and turmeric have antioxidant properties, which have gained interest among researchers to study their applications in the field of biomedicine, such asanti-inflammatory, anticancer, and antimicrobial applications. In this study, the turmeric extract was prepared and mixed with cerium nitrate hexahydrate, stirred continuously to obtain a homogeneous solution and then heated on a hot plate to get the supernatant evaporated, then calcinated at 600°C to obtain the cerium oxide nanoparticles. Characterization of synthesized cerium oxide nanoparticles through Scanning Electron Microscopy determined the particle size to be in the range of 70 nm to 250 nm. Energy Dispersive X-Ray Spectroscopy determined the elemental composition of cerium and oxygen. Individual particles were identified through the characterization of cerium oxide nanoparticles using Field Emission Scanning Electron Microscopy, in which the particles were determined to be spherical and in the size of around 70 nm. The presence of cerium oxide was assured by analyzing the spectrum obtained through the characterization of cerium oxide nanoparticles by Fourier Transform Infrared Spectroscopy. The crystal structure of cerium oxide nanoparticles was determined to be face-centered cubic by analyzing the peaks obtained through theX-Ray Diffraction method. The crystal size of cerium oxide nanoparticles was determined to be around 13 nm by using the Debye Scherer equation. This study confirmed the synthesis of cerium oxide nanoparticles using turmeric extract.

Keywords: antioxidant, characterization, cerium oxide, synthesis, turmeric

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Authors: Lavanya Srinivasan

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Biometric identification is to identify unique features in a person like fingerprints, iris, ear, and voice recognition that need the subject's permission and physical contact. Gait biometric is used to identify the unique gait of the person by extracting moving features. The main advantage of gait biometric to identify the gait of a person at a distance, without any physical contact. In this work, the gait biometric is used for person re-identification. The person walking naturally compared with the same person walking with bag, coat, and case recorded using longwave infrared, short wave infrared, medium wave infrared, and visible cameras. The videos are recorded in rural and in urban environments. The pre-processing technique includes human identified using YOLO, background subtraction, silhouettes extraction, and synthesis Gait Entropy Image by averaging the silhouettes. The moving features are extracted from the Gait Entropy Energy Image. The extracted features are dimensionality reduced by the principal component analysis and recognised using different classifiers. The comparative results with the different classifier show that linear discriminant analysis outperforms other classifiers with 95.8% for visible in the rural dataset and 94.8% for longwave infrared in the urban dataset.

Keywords: biometric, gait, silhouettes, YOLO

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Authors: Sam Bahreini, Payam Hayati

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Metal-organic coordination [Cu(L)₄(SCN)₂] was synthesized applying ultrasonic irradiation, and its photocatalytic performance for the degradation of Remdesivir (RS) under sunlight irradiation was systematically explored for the first time in this study. The physicochemical properties of the synthesized photocatalyst were investigated using Fourier-transform infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), powder x-ray diffraction (PXRD), energy-dispersive x-ray (EDX), thermal gravimetric analysis (TGA), diffuse reflectance spectroscopy (DRS) techniques. Systematic examinations were carried out by changing irradiation time, temperature, solution pH value, contact time, RS concentration, and catalyst dosage. The photodegradation kinetic profiles were modeled in pseudo-first order, pseudo-second-order, and intraparticle diffusion models reflected that photodegradation onto [Cu(L)₄(SCN)₂] catalyst follows pseudo-first order kinetic model. The fabricated [Cu(L)₄(SCN)₂] nanostructure bandgap was determined as 2.60 eV utilizing the Kubelka-Munk formula from the diffuse reflectance spectroscopy method. Decreasing chemical oxygen demand (COD) (from 70.5 mgL-1 to 36.4 mgL-1) under optimal conditions well confirmed mineralizing of the RS drug. The values of ΔH° and ΔS° was negative, implying the process of adsorption is spontaneous and more favorable in lower temperatures.

Keywords: Photocatalytic degradation, COVID-19, density functional theory (DFT), molecular electrostatic potential (MEP)

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Authors: Li Long, Thomas Ortlepp

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A theoretical model for the optimization of thermopile sensor performance is developed for thermoelectric-based infrared radiation detection. It is shown that the performance of polycrystalline silicon film thermopile sensor can be optimized according to the thermoelectric quality factor, sensor layer structure factor, and sensor layout geometrical form factor. Based on the properties of electrons, phonons, grain boundaries, and their interactions, the thermoelectric quality factor of polycrystalline silicon is analyzed with the relaxation time approximation of the Boltzmann transport equation. The model includes the effect of grain structure, grain boundary trap properties, and doping concentration. The layer structure factor is analyzed with respect to the infrared absorption coefficient. The optimization of layout design is characterized by the form factor, which is calculated for different sensor designs. A double-layer polycrystalline silicon thermopile infrared sensor on a suspended membrane has been designed and fabricated with a CMOS-compatible process. The theoretical approach is confirmed by measurement results.

Keywords: polycrystalline silicon, relaxation time approximation, specific detectivity, thermal conductivity, thermopile infrared sensor

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Authors: Anika Zafiah M. Rus, Nur Munirah Abdullah, M. F. L. Abdullah

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The fabrication and characterization of composite films of graphite- bioepoxy is described. Free-standing thin films of ~0.1 mm thick are prepared using a simple solution mixing with mass proportion of 7/3 (bioepoxy/graphite) and drop casting at room temperature. Fourier transform infra-red spectroscopy (FTIR) and Ultraviolet-visible (UV-vis) spectrophotometer are performed to evaluate the changes in chemical structure and adsorption spectra arising with the increasing of graphite weight loading (wt.%) into the biopolymer matrix. The morphologic study shows a homogeneously dispersed and strong particle bonding between the graphite and the bioepoxy, with conductivity of the film 103 S/m, confirming the efficiency of the processes.

Keywords: absorbance peak, biopolymer, graphite- bioepoxy composites, particle bonding

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Authors: Padmesh Tirunelveli Narayanapillai, Joel Sharwinkumar, Gaitri Saravanan

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The biosorption of Xylenol Orange (XO) and Eriochrome Black T (EBT) from aqueous solutions by chemically activated Cocos nucifera and mango seed as a low-cost, natural, and eco-friendly biosorbents was investigated. The study for biosorption of XO and EBT was optimized by different experimental parameters, initial pH 2–7, temperature 30–60 °C, biosorbent dosage 0.1 – 0.5 g, and XO: EBT dye proportions 0 – 100 by weight %. Physicochemical characteristic studies were conducted by Fourier Transform Infrared (FTIR). The equilibrium uptake was increased with an increase in the initial dye concentrations in the solution. Biosorption kinetic data were properly fitted with the pseudo-second-order kinetic model. The experimental isotherms data were analyzed using Langmuir, Freundlich, Redlich-Peterson, and Toth isotherm equations. Thermodynamic parameters ∆Go, ∆Ho, and ∆So were calculated indicating that the biosorption of Xo and EBT dye is a spontaneous and endothermic process. The Langmuir model gave the best fit by higher correlation coefficient (R2 =0.9971) for both biosorbents at optimum circumstances as pH 3, temperature 30°C, dosage 0.5 g for chemically activated Cocos nucifera and 0.4 g for chemically activated mango seeds it assumes as monolayer adsorption. The maximum dye removal efficiency was determined as 79.75% with chemically activated mango seeds compared to chemically activated Cocos nucifera. In summary, this research work showed that chemically modified activated mango seed can be effectively used as a promising low-cost biosorbent for the removal of different XO and EBT mixed dye combinations from aqueous solutions.

Keywords: mixed dye proportions, xylenol orange and eriochrome black t, chemically activated cocos nucifera and mango seed, kinetic, isotherm and thermodynamic studies, FTIR

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Authors: L. M. Ombaka, R. S. Oosthuizen, P. G. Ndungu, V. O. Nyamori

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Understanding the role of nitrogen species on the catalytic properties of nitrogen-doped carbon nanotubes (N-CNTs) as catalysts supports is critical as nitrogen species influence the support’s properties. To evaluate the influence of pyrrolic nitrogen on the physicochemical properties and catalytic activity of N-CNTs supported Pd (Pd/N-CNTs); N-CNTs containing varying pyrrolic contents were synthesized. The catalysts were characterised by the use of transmission electron microscope (TEM), scanning electron microscope, X-ray photoelectron spectroscopy (XPS), X-ray diffraction, Fourier transform infrared spectroscopy, and temperature programmed reduction. TEM analysis showed that the Pd nanoparticles were mainly located along the defect sites on N-CNTs. XPS analysis revealed that the abundance of Pd0 decreased while that of Pd2+ increased as the quantity of pyrrolic nitrogen increased. The increase of Pd2+ species was accredited to the formation of stable Pd-N coordination complexes which prevented further reduction of Pd2+ to Pd0 during synthesis. The formed Pd-N complexes increased the stability and dispersion of Pd2+ nanoparticles. The selective hydrogenation of nitrobenzophenone to aminobenzophenone over Pd/N-CNTs was compared to that of Pd on carbon nanotubes (Pd/CNTs). Pd/N-CNTs showed a higher catalytic activity and selectivity compared with Pd/CNTs. Pyrrolic nitrogen functional groups significantly promoted the selectivity towards aminobenzophenone formation.

Keywords: pyrrolic N-CNTs, hydrogenation reactions, chemical vapour deposition technique

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Authors: Ifeoma Maryjane Iloamaeke, Kelvin Obazie, Mmesoma Offornze, Chiamaka Marysilvia Ifeaghalu, Cecilia Aduaka, Ugomma Chibuzo Onyeije, Claudine Ifunanaya Ogu, Ngozi Anastesia Okonkwo

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This work investigated the effects of pH, settling time, and coagulant dosages on the removal of color, turbidity, and heavy metals from paint industrial wastewater using the seed of Artocarpus heterophyllus (AH) by the coagulation-flocculation process. The paint effluent was physicochemically characterized, while AH coagulant was instrumentally characterized by Scanning Electron Microscope (SEM), Fourier Transform Infrared (FTIR), and X-ray diffraction (XRD). A Jar test experiment was used for the coagulation-flocculation process. The result showed that paint effluent was polluted with color, turbidity (36000 NTU), mercury (1.392 mg/L), lead (0.252 mg/L), arsenic (1.236 mg/L), TSS (63.40mg/L), and COD (121.70 mg/L). The maximum color removal efficiency was 94.33% at the dosage of 0.2 g/L, pH 2 at a constant time of 50 mins, and 74.67% at constant pH 2, coagulant dosage of 0.2 g/L and 50 mins. The highest turbidity removal efficiency was 99.94% at 0.2 g/L and 50 mins at constant pH 2 and 96.66% at pH 2 and 0.2 g/L at constant time of 50 mins. The mercury removal efficiency of 99.29% was achieved at the optimal condition of 0.8 g/L coagulant dosage, pH 8, and constant time of 50 mins and 99.57% at coagulant dosage of 0.8 g/L, time of 50 mins constant pH 8. The highest lead removal efficiency was 99.76% at a coagulant dosage of 10 g/L, time of 40 mins at constant pH 10, and 96.53% at pH 10, coagulant dosage of 10 g/L and constant time of 40 mins. For arsenic, the removal efficiency is 75.24 % at 0.8 g/L coagulant dosage, time of 40 mins, and constant pH of 8. XRD imaging before treatment showed that Artocarpus heterophyllus coagulant was crystalline and changed to amorphous after treatment. The SEM and FTIR results of the AH coagulant and sludge suggested there were changes in the surface morphology and functional groups before and after treatment. The reaction kinetics were modeled best in the second order.

Keywords: Artocarpus heterophyllus, coagulation-flocculation, coagulant dosages, setting time, paint effluent

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Authors: Sleman Yahya Rasul

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Due to their transparency, various types of glass are utilized in numerous applications where clear visibility is essential. One such application involves environments where radiography, radiotherapy, and X-ray devices are used, all of which involve exposure to radiation. As is well-known, radiation can be lethal to humans. Consequently, there is a need for glass that can absorb and block these harmful rays in such settings. Effective protection from radiation typically requires materials with high atomic numbers and densities. Currently, lead oxide-infused glasses are commonly used for this purpose, but due to the toxicity of lead oxide, there is a demand for safer alternatives. HfO2 has been selected as an additive for boro-tellurite (M1-M2-M3) glasses intended for radiation shielding because it has a high atomic number, high density, and is non-toxic. In this study, new glasses will be developed as alternatives to leaded glasses by incorporating x mol% HfO2 into the boro-tellurite glass structure. The glass compositions will be melted and quenched using the traditional method in an alumina crucible at temperatures between 900–1100°C. The resulting glasses will be evaluated for their elastic properties (including elastic modulus, shear modulus, bulk modulus, and Poisson ratio), density, hardness, and fracture toughness. X-ray diffraction (XRD) will be used to examine the amorphous nature of the glasses, while Differential Thermal Analysis (DTA) will provide thermal analysis. Optical properties will be assessed through UV-Vis and Photoluminescence Spectroscopy, and structural properties will be studied using Raman spectroscopy and FTIR spectroscopy. Additionally, the radiation shielding capabilities will be investigated by measuring parameters such as mass attenuation coefficient, half-value thickness, mean free path, effective atomic number (Z_eff), and effective electron density (N_e). The aim of this study is to develop new, lead-free glasses with excellent optical properties and high mechanical strength to replace the leaded glasses currently used for radiation shielding.

Keywords: boro-tellurite glasses, hfo2, radiation shielding, mechanical properties, elastic properties, optical properties

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Authors: Kholod Khairy Salama, Shabban Hassan Thabet

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In the present study, a comprehensive investigation has been undertaken into an Egyptian mural painting with feet wear slippers approach to choose the most successful restoration methods. The mural painting under examination dates back to the Amarna period; it was detached from a wall of an unknown tomb in Egypt, and currently, it is initially displayed in a showcase at the Egyptian Museum – Tahrir Square – Cairo, Egypt. The main objectives of this research were to (a) reveal the pigment used in the mural painting, (b) reveal the medium used with colours, (c) determine the technique of manufacturing, (e) determine the ground support, and (f) reveal the main deterioration aspects. The analytical techniques used for investigation were Optical Microscopy, Raman, X-ray Florescence, X-ray diffraction, and Fourier transform infrared coupled with attenuated total reflectance “FTIR-ATR”. The investigation revealed that the vital deterioration factors affecting the object. This research aims to examine and analyze the mural painting to choose the suitable method for the restoration process (a) define the colours through comparative analysis to choose the suitable material for cleaning, (b) define the natural structure of the ground support layer, which appeared as mud layer (c) determine the medium used with colours (d) diagnosis the presence of the white wash layer, and (e) choose the suitable restoration methods according to the results. Conclusion: This study focused mainly on the physical and chemical properties of the mural painting compound and the main changes that happened to the mural painting material, which caused deterioration and fall down of the painting parts, so we can find the best and optimum restoration ways for this object.

Keywords: mural paintings, Tal Al-Amarna, digital microscope, Raman, XRF, XRD, FTIR

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Authors: Hiroyuki Aoki

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Molecular imaging has attracted much attention recently, which visualizes biological molecules, cells, tissue, and so on. Among various in vivo imaging techniques, the fluorescence imaging method has been widely employed as a useful modality for small animals in pre-clinical researches. However, the higher signal intensity is needed for highly sensitive in vivo imaging. The objective of the current study is the development of a fluorescent imaging agent with high brightness for the tumor imaging of a mouse. The strategy to enhance the fluorescence signal of a bio-imaging agent is the increase of the absorption of the excitation light and the fluorescence conversion efficiency. We developed a nano-particle fluorescence imaging agent consisting of a π-conjugated polymer emitting a fluorescence signal in a near infrared region. A large absorption coefficient and high emission intensity at a near infrared optical window for biological tissue enabled highly sensitive in vivo imaging with a tumor-targeting ability by an EPR (enhanced permeation and retention) effect. The signal intensity from the π-conjugated fluorescence imaging agent is larger by two orders of magnitude compared to a quantum dot, which has been known as the brightest imaging agent. The π-conjugated polymer nano-particle would be a promising candidate in the in vivo imaging of small animals.

Keywords: fluorescence, conjugated polymer, in vivo imaging, nano-particle, near-infrared

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Authors: Burcu Doymus, Fatma N. Kok, Sakip Onder

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Titanium and titanium-based materials are commonly used to replace or regenerate the injured or lost tissues because of accidents or illnesses. Hospital infections and strong bond formation at the implant-tissue interface are directly affecting the success of the implantation as weak bonding with the native tissue and hospital infections lead to revision surgery. The purpose of the presented study is to modify the surface of the titanium substrates with nano/microspheres for local drug delivery and to prevent hospital infections. Firstly, titanium surfaces were silanized with APTES (3-Triethoxysilylpropylamine) following the negatively charged oxide layer formation. Then characterization studies using Scanning Electron Microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were done on the modified surfaces. Secondly, microspheres/nanospheres were prepared with chitosan that is a natural polymer and having valuable properties such as non-toxicity, high biocompatibility, low allergen city and biodegradability for biomedical applications. Antibiotic (ciprofloxacin) loaded micro/nanospheres have been fabricated using emulsion cross-linking method and have been immobilized onto the titanium surfaces with different immobilization techniques such as covalent bond and entrapment. Optimization studies on size and drug loading capacities of micro/nanospheres were conducted before the immobilization process. Light microscopy and SEM were used to visualize and measure the size of the produced micro/nanospheres. Loaded and released drug amounts were determined by using UV- spectrophotometer at 278 nm. Finally, SEM analysis and drug release studies on the micro/nanospheres coated Ti surfaces were done. As a conclusion, it was shown that micro/nanospheres were immobilized onto the surfaces successfully and drug release from these surfaces was in a controlled manner. Moreover, the density of the micro/nanospheres after the drug release studies was higher on the surfaces where the entrapment technique was used for immobilization. Acknowledgement: This work is financially supported by The Scientific and Technological Research Council Of Turkey (Project # 217M220)

Keywords: chitosan, controlled drug release, nanosphere, nosocomial infections, titanium

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

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Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: green chemistry, 1H-indole, heteroaromatic, organic electrosynthesis

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Authors: B. Kurbanova, M. Karibayev, N. Almas, K. Ospanov, K. Aimaganbetov, T. Kuanyshbekov, K. Akatan, S. Kabdrakhmanova

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Proton exchange membranes (PEMs) operating at high temperatures above 100 °C with the excellent mechanical, chemical and thermochemical stability have been received much attention, because of their practical application of proton exchange membrane fuel cells (PEMFCs). Nowadays, a huge number of polymers and polymer-mixed various membranes have been investigated for this application, all of which offer both pros and cons. However, PEMFCs are still lack of ideal membranes with unique properties. In this work, carboxymethylcellulose (CMC) based membranes with dispersive graphene oxide (GO) sheets were fabricated and investigated for PEMFCs application. These membranes and pristine GO were studied by a combination of XRD, XPS, Raman, Brillouin, FTIR, thermo-mechanical analysis (TGA and Dynamic Mechanical Analysis) and SEM microscopy, while substantial studies on the proton transport properties were provided by Electrochemical Impedance Spectroscopy (EIS) measurements. It was revealed that the addition of CMC to the GO boosts proton conductivity of the whole membrane, while GO provides good mechanical and thermomechanical stability to the membrane. Further, the continuous and ordered nanochannels with well-tailored chemical structures were obtained by irradiation of heavy ions Kr⁺¹⁷ with an energy of 1.75 MeV/nucleon on the heavy ion accelerator. The formation of these nanochannels led to the significant increase of proton conductivity at 50% Relative Humidity. Also, FTIR and XPS measurement results show that ion irradiation eliminated the GO’s surface oxygen chemical bonds (C=O, C-O), and led to the formation of C = C, C – C bonds, whereas these changes connected with an increase in conductivity.

Keywords: proton exchange membranes, graphene oxide, fuel cells, carboxymethylcellulose, ion irradiation

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Authors: Kwangin Kim, Taewon Yoo, Haksoo Han

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Polyimide is a superior polymer in the electronics industry, and we conducted a study to synthesize poly(amide-imide) at low temperatures. Poly(amide-imide) was synthesized at low-temperature curing to offer a thermal stable membrane with low residual stress and good processability. As a result, the low crack polymer with good processability could be used to various applications such as semiconductors, integrated circuits, coating materials, membranes, and display. The synthesis of poly(amide-imide) at low temperatures was confirmed by Fourier transform infrared spectroscopy (FT-IR). Thermal stabilities of the polymer was confirmed by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC).

Keywords: poly(amide-imide), residual stress, thermal stability

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Authors: S. Cichosz, A. Masek

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A new cellulose hybrid modification approach, which is undoubtedly a scientific novelty, is introduced. The study reports the properties of cellulose (Arbocel UFC100 – Ultra Fine Cellulose) and characterizes cellulose filled polymer composites based on an ethylene-norbornene copolymer (TOPAS Elastomer E-140). Moreover, the approach of physicochemical two-stage cellulose treatment is introduced: solvent exchange (to ethanol or hexane) and further chemical modification with maleic anhydride (MA). Furthermore, the impact of the drying process on cellulose properties was investigated. Suitable measurements were carried out to characterize cellulose fibers: spectroscopic investigation (Fourier Transform Infrared Spektrofotometer-FTIR, Near InfraRed spectroscopy-NIR), thermal analysis (Differential scanning calorimetry, Thermal gravimetric analysis ) and Karl Fischer titration. It should be emphasized that for all UFC100 treatments carried out, a decrease in moisture content was evidenced. FT-IR reveals a drop in absorption band intensity at 3334 cm-1, the peak is associated with both –OH moieties and water. Similar results were obtained with Karl Fischer titration. Based on the results obtained, it may be claimed that the employment of ethanol contributes greatly to the lowering of cellulose water absorption ability (decrease of moisture content to approximately 1.65%). Additionally, regarding polymer composite properties, crucial data has been obtained from the mechanical and thermal analysis. The highest material performance was noted in the case of the composite sample that contained cellulose modified with MA after a solvent exchange with ethanol. This specimen exhibited sufficient tensile strength, which is almost the same as that of the neat polymer matrix – in the region of 40 MPa. Moreover, both the Payne effect and filler efficiency factor, calculated based on dynamic mechanical analysis (DMA), reveal the possibility of the filler having a reinforcing nature. What is also interesting is that, according to the Payne effect results, fibers dried before the further chemical modification are assumed to allow more regular filler structure development in the polymer matrix (Payne effect maximum at 1.60 MPa), compared with those not dried (Payne effect in the range 0.84-1.26 MPa). Furthermore, taking into consideration the data gathered from DSC and TGA, higher thermal stability is obtained in case of the materials filled with fibers that were dried before the carried out treatments (degradation activation energy in the region of 195 kJ/mol) in comparison with the polymer composite samples filled with unmodified cellulose (degradation activation energy of approximately 180 kJ/mol). To author’s best knowledge this work results in the introduction of a novel, new filler hybrid treatment approach. Moreover, valuable data regarding the properties of composites filled with cellulose fibers of various moisture contents have been provided. It should be emphasized that plant fiber-based polymer bio-materials described in this research might contribute significantly to polymer waste minimization because they are more readily degraded.

Keywords: cellulose fibers, solvent exchange, moisture content, ethylene-norbornene copolymer

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Authors: Patrik Scajev, Pavels Onufrijevs, Algirdas Mekys, Tadas Malinauskas, Dominykas Augulis, Liudvikas Subacius, Kuo-Chih Lee, Jevgenijs Kaupuzs, Arturs Medvids, Hung Hsiang Cheng

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In this study, we focused on the optoelectronic properties of the photodiodes prepared by using 200 nm thick Ge₀.₉₅Sn₀.₀₅ epitaxial layers on Ge/n-Si substrate with aluminum contacts. Photodiodes were formed on non-irradiated and Nd: YAG laser irradiated Ge₀.₉₅Sn₀.₀₅ layers. The samples were irradiated by pulsed Nd: YAG laser with 136.7-462.6 MW/cm² intensity. The photodiodes were characterized by using short laser pulses with the wavelength in the 2.0-2.6 μm range. The laser-irradiated diode was found more sensitive in the long-wavelength range due to laser-induced Sn atoms redistribution providing formation of graded bandgap structure. Sub-millisecond photocurrent relaxation in the diodes revealed their suitability for image sensors. Our findings open the perspective for improving the photo-sensitivity of GeSn alloys in the mid-infrared by pulsed laser processing.

Keywords: GeSn, laser processing, photodetector, infrared

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Authors: H. Apaza, L. Chévez, H. Loro

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Plastic and microplastic pollution in human food chain is a big problem for human health that requires more elaborated techniques that can identify their presences in different kinds of food. Hyperspectral imaging technique is an optical technique than can detect the presence of different elements in an image and can be used to detect plastics and microplastics in a scene. To do this statistical techniques are required that need to be evaluated and compared in order to find the more efficient ones. In this work, two problems related to the presence of plastics are addressed, the first is to detect and identify pieces of plastic immersed in almond seeds, and the second problem is to detect and quantify microplastic in almond flour. To do this we make use of the analysis hyperspectral images taken in the range of 900 to 1700 nm using 4 unmixing techniques of hyperspectral imaging which are: least squares unmixing (LSU), non-negatively constrained least squares unmixing (NCLSU), fully constrained least squares unmixing (FCLSU), and scaled constrained least squares unmixing (SCLSU). NCLSU, FCLSU, SCLSU techniques manage to find the region where the plastic is found and also manage to quantify the amount of microplastic contained in the almond flour. The SCLSU technique estimated a 13.03% abundance of microplastics and 86.97% of almond flour compared to 16.66% of microplastics and 83.33% abundance of almond flour prepared for the experiment. Results show the feasibility of applying near-infrared hyperspectral image analysis for the detection of plastic contaminants in food.

Keywords: food, plastic, microplastic, NIR hyperspectral imaging, unmixing

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Authors: Maha A. Younus, Dhefaf H. Badri, Maha A. Al Abayaji, Taha M. Salih

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Polymer metal complexes of poly vinyl alcohol and Cu (II), Ni (II), Mn (II) and Co (III) were prepared from the reaction of PVA with three different percentages of urea. The compound was characterized by fourier transform infrared spectrometry (FTIR) analysis and differential scanning calorimetric (DSC) Analysis. It has been established that the polymer and its metal complexes showed good activities against nine pathogenic bacteria (Escherichia coli, Klebsiellapneumonae, Staphylococcusaureus, Staphylococcus Albus, Salmonella Typhoid, Pseudomonas Aeruginosa, Shigella Dysentery, Proteus Morgani, Brucella Militensis). The polymer metal complexes show activity higher than that of the free polymer. The increasing activities were in the order (polymer < pol-Mn< pol-Co < pol-Ni ˂ pol-Cu). The ability of these compounds to show antimicrobial properties suggests that they can be further evaluated for medicinal and/or environmental applications.

Keywords: antimicrobial activity, PVA, polymer-metal complex, urea

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Authors: Igor Izosimov

Abstract:

This work is devoted to applications of the Time-resolved laser-induced luminescence (TRLIF) spectroscopy and time-resolved laser-induced chemiluminescence spectroscopy for detection of lanthanides and actinides. Results of the experiments on Eu, Sm, U, and Pu detection in solutions are presented. The limit of uranyl detection (LOD) in urine in our TRLIF experiments was up to 5 pg/ml. In blood plasma LOD was 0.1 ng/ml and after mineralization was up to 8pg/ml – 10pg/ml. In pure solution, the limit of detection of europium was 0.005ng/ml and samarium, 0.07ng/ml. After addition urine, the limit of detection of europium was 0.015 ng/ml and samarium, 0.2 ng/ml. Pu, Np, and some U compounds do not produce direct luminescence in solutions, but when excited by laser radiation, they can induce chemiluminescence of some chemiluminogen (luminol in our experiments). It is shown that multi-photon scheme of chemiluminescence excitation makes chemiluminescence not only a highly sensitive but also a highly selective tool for the detection of lanthanides/actinides in solutions.

Keywords: actinides/lanthanides detection, laser spectroscopy with time resolution, luminescence/chemiluminescence, solutions

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Authors: Mercedes Bertotto, Marcelo Bello, Hector Goicoechea, Veronica Fusca

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The National Service of Agri-Food Health and Quality (SENASA), controls honey to detect contamination by synthetic or natural chemical substances and establishes and controls the traceability of the product. The utility of near-infrared spectroscopy for the detection of adulteration of honey with high fructose corn syrup (HFCS) was investigated. First of all, a mixture of different authentic artisanal Argentinian honey was prepared to cover as much heterogeneity as possible. Then, mixtures were prepared by adding different concentrations of high fructose corn syrup (HFCS) to samples of the honey pool. 237 samples were used, 108 of them were authentic honey and 129 samples corresponded to honey adulterated with HFCS between 1 and 10%. They were stored unrefrigerated from time of production until scanning and were not filtered after receipt in the laboratory. Immediately prior to spectral collection, honey was incubated at 40°C overnight to dissolve any crystalline material, manually stirred to achieve homogeneity and adjusted to a standard solids content (70° Brix) with distilled water. Adulterant solutions were also adjusted to 70° Brix. Samples were measured by NIR spectroscopy in the range of 650 to 7000 cm⁻¹. The technique of specular reflectance was used, with a lens aperture range of 150 mm. Pretreatment of the spectra was performed by Standard Normal Variate (SNV). The ant colony optimization genetic algorithm sample selection (ACOGASS) graphical interface was used, using MATLAB version 5.3, to select the variables with the greatest discriminating power. The data set was divided into a validation set and a calibration set, using the Kennard-Stone (KS) algorithm. A combined method of Potential Functions (PF) was chosen together with Partial Least Square Linear Discriminant Analysis (PLS-DA). Different estimators of the predictive capacity of the model were compared, which were obtained using a decreasing number of groups, which implies more demanding validation conditions. The optimal number of latent variables was selected as the number associated with the minimum error and the smallest number of unassigned samples. Once the optimal number of latent variables was defined, we proceeded to apply the model to the training samples. With the calibrated model for the training samples, we proceeded to study the validation samples. The calibrated model that combines the potential function methods and PLSDA can be considered reliable and stable since its performance in future samples is expected to be comparable to that achieved for the training samples. By use of Potential Functions (PF) and Partial Least Square Linear Discriminant Analysis (PLS-DA) classification, authentic honey and honey adulterated with HFCS could be identified with a correct classification rate of 97.9%. The results showed that NIR in combination with the PT and PLS-DS methods can be a simple, fast and low-cost technique for the detection of HFCS in honey with high sensitivity and power of discrimination.

Keywords: adulteration, multivariate analysis, potential functions, regression

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Authors: F. Zouai, F. Z. Benabid, S. Bouhelal, D. Benachour

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Nanocomposite polymer / clay are relatively important area of research. These reinforced plastics have attracted considerable attention in scientific and industrial fields because a very small amount of clay can significantly improve the properties of the polymer. The polymeric matrices used in this work are two saturated polyesters ie polyethylene terephthalate (PET) and polyethylene naphthalate (PEN).The success of processing compatible blends, based on poly(ethylene terephthalate) (PET)/ poly(ethylene naphthalene) (PEN)/clay nanocomposites in one step by reactive melt extrusion is described. Untreated clay was first purified and functionalized ‘in situ’ with a compound based on an organic peroxide/ sulfur mixture and (tetramethylthiuram disulfide) as the activator for sulfur. The PET and PEN materials were first separately mixed in the molten state with functionalized clay. The PET/4 wt% clay and PEN/7.5 wt% clay compositions showed total exfoliation. These compositions, denoted nPET and nPEN, respectively, were used to prepare new n(PET/PEN) nanoblends in the same mixing batch. The n(PET/PEN) nanoblends were compared to neat PET/PEN blends. The blends and nanocomposites were characterized using various techniques. Microstructural and nanostructural properties were investigated. Fourier transform infrared spectroscopy (FTIR) results showed that the exfoliation of tetrahedral clay nanolayers is complete and the octahedral structure totally disappears. It was shown that total exfoliation, confirmed by wide angle X-ray scattering (WAXS) measurements, contributes to the enhancement of impact strength and tensile modulus. In addition, WAXS results indicated that all samples are amorphous. The differential scanning calorimetry (DSC) study indicated the occurrence of one glass transition temperature Tg, one crystallization temperature Tc and one melting temperature Tm for every composition. This was evidence that both PET/PEN and nPET/nPEN blends are compatible in the entire range of compositions. In addition, the nPET/nPEN blends showed lower Tc and higher Tm values than the corresponding neat PET/PEN blends. In conclusion, the results obtained indicate that n(PET/PEN) blends are different from the pure ones in nanostructure and physical behavior.

Keywords: blends, exfoliation, DRX, DSC, montmorillonite, nanocomposites, PEN, PET, plastograph, reactive melt-mixing

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Authors: Aura Maria Lopera Echavarria, Angela Maria Lema Perez, Daniela Medrano David, Pedronel Araque Marin, Marta Elena Londoño Lopez

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Bone regeneration is the process by which the formation of new bone is stimulated. Bone fractures can originate at any time due to trauma, infections, tumors, congenital malformations or skeletal diseases. Currently there are different strategies to treat bone defects that in some cases, regeneration does not occur on its own. That is why they are treated with bone substitutes, which provide a necessary environment for the cells to synthesize new bone. The Demineralized Bone Matrix (DBM) is widely used as a bone implant due to its good properties, such as osteoinduction and bioactivity. However, the use of DBM is limited, because its presentation is powder, which is difficult to implant with precision and is susceptible to migrating to other sites through blood flow. That is why the DBM is commonly incorporated into a variety of vehicles or carriers. The objective of this project is to evaluate the bioactive and confinement properties of a bone substitute based on demineralized bone matrix (DBM). Also, structural and morphological properties were evaluated. Bone substitute was obtained from EIA Biomaterials Laboratory of EIA University and the DBM was facilitated by Tissue Bank Foundation. Morphological and structural properties were evaluated by scanning electron microscopy (SEM), X-ray diffraction (DRX) and Fourier transform infrared spectroscopy with total attenuated reflection (FTIR-ATR). Water absorption capacity and degradation were also evaluated during three months. The cytotoxicity was evaluated by the MTT test. The bioactivity of the bone substitute was evaluated through immersion of the samples in simulated body fluid during four weeks. Confinement tests were performed on tibial fragments of a human donor with bone defects of determined size, to ensure that the substitute remains in the defect despite the continuous flow of fluid. According of the knowledge of the authors, the methodology for evaluating samples in a confined environment has not been evaluated before in real human bones. The morphology of the samples showed irregular surface and presented some porosity. DRX confirmed a semi-crystalline structure. The FTIR-ATR determined the organic and inorganic phase of the sample. The degradation and absorption measurements stablished a loss of 3% and 150% in one month respectively. The MTT showed that the system is not cytotoxic. Apatite clusters formed from the first week were visualized by SEM and confirmed by EDS. These calcium phosphates are necessary to stimulate bone regeneration and thanks to the porosity of the developed material, osteinduction and osteoconduction are possible. The results of the in vitro evaluation of the confinement of the material showed that the migration of the bone filling to other sites is negligible, although the samples were subjected to the passage of simulated body fluid. The bone substitute, putty type, showed stability, is bioactive, non-cytotoxic and has handling properties for specialists at the time of implantation. The obtained system allows to maintain the osteoinductive properties of DBM and it can fill completely fractures in any way; however, it does not provide a structural support, that is, it should only be used to treat fractures without requiring a mechanical load.

Keywords: bone regeneration, cytotoxicity, demineralized bone matrix, hydrogel

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Authors: Abdul Mutalib Md Jani, Abdul Hadi Mahmud, Mohd Tajuddin Mohd Ali

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The rapid growth of interest in surface modification of nanostructures materials that exhibit improved structural and functional properties is attracting more researchers. The unique properties of highly ordered nanoporous anodic aluminium oxide (NAAO) membrane have been proposed as a platform for biosensing applications. They exhibit excellent physical and chemical properties with high porosity, high surface area, tunable pore sizes and excellent chemical resistance. In this study, NAAO was functionalized with 3-aminopropyltriethoxysilane (APTES) to prepared silane-modified NAAO. Amine functional groups are formed on the surface of NAAO during silanization and were characterized using Fourier Transform Infrared spectroscopy (FTIR). The synthesis of multi segment of peptide on NAAO surfaces can be realized by changing the surface chemistry of the NAAO membrane via click chemistry. By click reactions, utilizing alkyne terminated with amino group, various peptides tagged on NAAO can be envisioned from chiral natural or unnatural amino acids using standard coupling methods (HOBt, EDCI and HBTU). This strategy seemly versatile since coupling strategy of dipeptide with another amino acids, leading to tripeptide, tetrapeptide or pentapeptide, can be synthesized without purification. When an appropriate terminus is selected, multiple segments of amino acids can be successfully synthesized on the surfaces. The immobilized NAAO should be easily separated from the reaction medium by conventional filtration, thus avoiding complicated purification methods. Herein, we proposed to synthesize multi fragment peptide as a model for capturing and attaching various small biomolecules on NAAO surfaces and can be also applied as biosensing device, drug delivery systems and biocatalyst.

Keywords: nanoporous anodic aluminium oxide, silanization, peptide synthesise, click chemistry

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Authors: Ji-Yeul Bae, Hyung Mo Bae, Jihyuk Kim, Hyung Hee Cho

Abstract:

An air to air infrared missile poses a significant threat to the survivability of an aircraft due to an advanced sensitivity of sensor and maneuverability of the missile. Therefore, recent military aircraft is equipped with MAW (Missile Approach Warning) to take an evasive maneuver and to deploy countermeasures like chaff and flare. In this research, an effect of MAW sensitivity and resulting evasive maneuver on the survivability of the fighter aircraft is studied. A single engine fighter jet with Mach 0.9 flying at an altitude of 5 km is modeled in the research and infrared signature of the aircraft is calculated by numerical simulation. The survivability is assessed in terms of lethal range. The MAW sensitivity and maneuverability of an aircraft is used as variables. The result showed that improvement in survivability mainly achieved when the missile approach from the side of the aircraft. And maximum 30% increase in survivability of the aircraft is achieved when existence of the missile is noticed at 7 km distance. As a conclusion, sensitivity of the MAW seems to be more important factor than the maneuverability of the aircraft in terms of the survivability.

Keywords: air to air missile, missile approach warning, lethal range, survivability

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Authors: H. Zouaoui, D. Abdi, B. Nessark, F. Habelhames, A. Bahloul

Abstract:

Among the conjugated organic polymers, the polythiophenes constitute a particularly important class of conjugated polymers, which has been extensively studied for the relation between the geometrical structure and the optic and electronic properties, while the polythiophene is an intractable material. They are, furthermore, chemically and thermally stable materials, and are very attractive for exploitation of their physical properties. The polythiophenes are extensively studied due to the possibility of synthesizing low band gap materials by using substituted thiophenes as precursors. Low band gap polymers may convert visible light into electricity and some photoelectrochemical cells based on these materials have been prepared. Polythiophenes (PThs) are good candidates for polymer optoelectronic devices such as polymer solar cells (PSCs) polymer light-emitting diodes (PLEDs) field-effect transistors (FETs) electrochromics and biosensors. In this work, MnO2 has been synthesized by hydrothermal method and analyzed by infrared spectroscopy. The polybithiophene+MnO2 composite films were electrochemically prepared by cyclic voltammetry technic on a conductor glass substrate ITO (indium–tin-oxide). The composite films are characterized by cyclic voltammetry, impedance spectroscopy and photoelectrochemical analyses. The results confirmed the presence of manganese dioxide nanoparticles in the polymer layer. An application has been made by using these deposits as an electrode in a photoelectrochemical cell for measuring photocurrent tests. The composite films show a significant photocurrent intensity 80 μA.cm-2.

Keywords: polybithiophene, MnO2, photoelectrochemical cells, composite films

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Authors: Raquel C. A. G. Mota, Livia R. Menezes, Emerson O. da Silva

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Both silver nanoparticles and titanium dioxide have been extensively used in tissue engineering since they’ve been approved by the Food and Drug Administration (FDA), and present a bactericide effect when added to a polymeric matrix. In this work, the focus is on fabricating binary systems with both nanoparticles so that the synergistic effect can be investigated. The systems were tested by Nuclear Magnetic Resonance (NMR), Thermogravimetric Analysis (TGA), Fourier-Transformed Infrared (FTIR), and Differential Scanning Calorimetry (DSC), and X-ray Diffraction (XRD), and had both their bioactivity and bactericide effect tested. The binary systems presented different properties than the individual systems, enhancing both the thermal and biological properties as was to be expected. The crystallinity was also affected, as indicated by the finding of the DSC and XDR techniques, and the NMR showed a good dispersion of both nanoparticles in the polymer matrix. These findings indicate the potential of combining TiO₂ and silver nanoparticles in biomedicine.

Keywords: metallic nanoparticles, nanotechnology, polymer nanocomposites, polymer science

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