Search results for: (FTIR) spectroscopy

Authors: M. Sikoń, E. Bidzińska

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An attempt to apply EPR (Electron Paramagnetic Resonance) spectroscopy to experimental analysis of the mechanical state of the loaded material is considered in this work. Theory concerns the participation of electrons in transfer of mechanical action. The model of measurement is shown by applying classical mechanics and quantum mechanics. Theoretical analysis is verified using EPR spectroscopy twice, once for the free spacemen and once for the mechanical loaded spacemen. Positive results in the form of different spectra for free and loaded materials are used to describe the mechanical state in continuum based on statistical mechanics. Perturbation of the optical electrons in the field of the mechanical interactions inspires us to propose new optical properties of the materials with mechanical stresses.

Keywords: Cosserat medium, EPR spectroscopy, optical active electrons, optical activity

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Authors: Fuad Abdullah Alatawi

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Microbial infections-based diseases are a significant public health issue around the world, mainly when antibiotic-resistant bacterium types evolve. In this research, we explored the anti-bacterial and anti-cancer potency of iron-oxide (Fe₂O₃) nanoparticles prepared from F. macrocarpa fruit extract. The chemical composition of F. macrocarpa fruit extract was used as a reducing and capping agent for nanoparticles’ synthesis was examined by GC-MS/MS analysis. Then, the prepared nanoparticles were confirmed by various biophysical techniques, including X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), UV-Vis Spectroscopy, and Transmission Electron Microscopy (TEM) and Energy Dispersive Spectroscopy (EDAX), and Dynamic Light Scattering (DLS). Also, the antioxidant capacity of fruit extract was determined through 2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS), Fluorescence Recovery After Photobleaching (FRAP), Superoxide Dismutase (SOD) assays. Furthermore, the cytotoxicity activities of Fe₂O₃ NPs were determined using the (3-(4, 5-dimethylthiazolyl-2)-2, 5-diphenyltetrazolium bromide) (MTT) test on MCF-7 cells. In the antibacterial assay, lethal doses of the Fe₂O₃NPs effectively inhibited the growth of gram-negative and gram-positive bacteria. The surface damage, ROS production, and protein leakage are the antibacterial mechanisms of Fe₂O₃NPs. Concerning antioxidant activity, the fruit extracts of F. macrocarpa had strong antioxidant properties, which were confirmed by DPPH, ABTS, FRAP, and SOD assays. In addition, the F. microcarpa-derived iron oxide nanomaterials greatly reduced the cell viability of (MCF-7). The GC-MS/MS analysis revealed the presence of 25 main bioactive compounds in the F. microcarpa extract. Overall, the finding of this research revealed that F. microcarpa-derived Fe₂O₃ nanoparticles could be employed as an alternative therapeutic agent to cure microbial infection and breast cancer in humans.

Keywords: ficus microcarpa, iron oxide, antibacterial activity, cytotoxicity

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Authors: Marivane Turim Koschevic, Maycon dos Santos, Marcello Lima Bertuci, Farayde Matta Fakhouri, Silvia Maria Martelli

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Natural fibers are rich raw materials in cellulose and abundant in the world, its use for the cellulose nanocrystals extraction is promising as an example cited is the cattail, macrophyte native weed in South America. This study deals with the pre-treatment cattail of crushed fibers, at six different methods of mercerization, followed by the use of bleaching. As a result, have found The positive effects of treating fibers by means of optical microscopy and spectroscopy, Fourier transform (FTIR). The sample selected for future testing of cellulose nanocrystals extraction was treated in 2.5% NaOH for 2 h, 60 °C in the first stage and 30vol H2O2, NaOH 5% in the proportion 30/70% (v/v) for 1 hour 60 °C, followed by treatment at 50/50% (v/v) 15 minutes, 50°C, with the same constituents of the solution.

Keywords: cellulose nanocrystal, chemical treatment, mercerization, natural fibers

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Authors: Reem M. Altuwirqi, Mohja S. Summan, Entesar A. Ganash, Safia H. Hamidalddin, Tamer E. Youssef, Mohammed A. Gondal

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Laser-Induced Breakdown Spectroscopy (LIBS) technique using 1064 nm Nd: YAG laser was optimized and applied for investigating the existence of radioactive elements (uranium) in twenty-six different ceramic tiles. These tiles were collected from the local Saudi market. Qualitative and quantitative analysis for trace radioactive elements like uranium in these samples was achieved using LIBS. The plasma parameters such as temperature and electron density were calculated to confirm that the plasma generated by the tile samples under laser irradiation can be related to analyte concentrations. In order to perform a quantitative analysis, calibration curves were constructed for two uranium lines (U II (424.166 nm) and U II (424.437 nm)). The Uranium activity concentration in Bq/kg for each sample was measured. Cross-validation of LIBS results with a conventional technique such as Gamma-Ray spectroscopy was also carried out for five ceramic samples. The results show that the LIBS method is an effective way of determining radioactive elements such as uranium in ceramic tiles. Moreover, the uranium concentrations of the investigated samples were below the permissible safe limit for building materials in the majority of samples. Such LIBS system could be applied to determine the presence of natural radioactive elements in ceramic tiles and their radioactivity level rapidly to ensure that they are under the safe allowed limit.

Keywords: laser-induced breakdown spectroscopy, gamma-ray spectroscopy, natural radioactivity, uranium, ceramic tiles

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Authors: Andreas Kerstan, Darren Robey, Wesam Alvan, David Troiani

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Over the last 3.5 years, Quantum Cascade Lasers (QCL) technology has become increasingly important in infrared (IR) microscopy. The advantages over fourier transform infrared (FTIR) are that large areas of a few square centimeters can be measured in minutes and that the light intensive QCL makes it possible to obtain spectra with excellent S/N, even with just one scan. A firmly established solution of the laser direct infrared imaging (LDIR) 8700 is the analysis of microplastics. The presence of microplastics in the environment, drinking water, and food chains is gaining significant public interest. To study their presence, rapid and reliable characterization of microplastic particles is essential. Significant technical hurdles in microplastic analysis stem from the sheer number of particles to be analyzed in each sample. Total particle counts of several thousand are common in environmental samples, while well-treated bottled drinking water may contain relatively few. While visual microscopy has been used extensively, it is prone to operator error and bias and is limited to particles larger than 300 µm. As a result, vibrational spectroscopic techniques such as Raman and FTIR microscopy have become more popular, however, they are time-consuming. There is a demand for rapid and highly automated techniques to measure particle count size and provide high-quality polymer identification. Analysis directly on the filter that often forms the last stage in sample preparation is highly desirable as, by removing a sample preparation step it can both improve laboratory efficiency and decrease opportunities for error. Recent advances in infrared micro-spectroscopy combining a QCL with scanning optics have created a new paradigm, LDIR. It offers improved speed of analysis as well as high levels of automation. Its mode of operation, however, requires an IR reflective background, and this has, to date, limited the ability to perform direct “on-filter” analysis. This study explores the potential to combine the filter with an infrared reflective surface filter. By combining an IR reflective material or coating on a filter membrane with advanced image analysis and detection algorithms, it is demonstrated that such filters can indeed be used in this way. Vibrational spectroscopic techniques play a vital role in the investigation and understanding of microplastics in the environment and food chain. While vibrational spectroscopy is widely deployed, improvements and novel innovations in these techniques that can increase the speed of analysis and ease of use can provide pathways to higher testing rates and, hence, improved understanding of the impacts of microplastics in the environment. Due to its capability to measure large areas in minutes, its speed, degree of automation and excellent S/N, the LDIR could also implemented for various other samples like food adulteration, coatings, laminates, fabrics, textiles and tissues. This presentation will highlight a few of them and focus on the benefits of the LDIR vs classical techniques.

Keywords: QCL, automation, microplastics, tissues, infrared, speed

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Authors: Satam Alotibi, Haya A. Al-Sunaidi, Almaymunah M. AlRoibah, Zahraa H. Al-Omaran, Mohammed Alyami, Fatehia S. Alhakami, Abdellah Kaiba, Mazen Alshaaer, Talal F. Qahtan

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This research study presents a novel approach to harnessing the potential of natural geopolymer in conjunction with TiO₂ nanoparticles (TiO₂ NPs) for the development of highly efficient photocatalytic materials for water decontamination. The study begins with the formulation of a geopolymer paste derived from natural sources, which is subsequently applied as a coating on glass substrates and allowed to air-dry at room temperature. The result is a series of geopolymer-coated glass films, serving as the foundation for further experimentation. To enhance the photocatalytic capabilities of these films, a critical step involves immersing them in a suspension of TiO₂ nanoparticles (TiO₂ NPs) in water for varying durations. This immersion process yields geopolymer-loaded TiO₂ NPs films with varying concentrations, setting the stage for comprehensive characterization and analysis. A range of advanced analytical techniques, including UV-Vis spectroscopy, Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM), were meticulously employed to assess the structural, morphological, and chemical properties of the geopolymer-based TiO₂ films. These analyses provided invaluable insights into the materials' composition and surface characteristics. The culmination of this research effort sees the geopolymer-based TiO₂ films being repurposed as immobilized photocatalytic reactors for water decontamination under natural sunlight irradiation. Remarkably, the results revealed exceptional photocatalytic performance that exceeded the capabilities of conventional TiO₂-based photocatalysts. This breakthrough underscores the significant potential of natural geopolymer as a versatile and highly effective matrix for enhancing the photocatalytic efficiency of TiO₂ nanoparticles in water treatment applications. In summary, this study represents a significant advancement in the quest for sustainable and efficient photocatalytic materials for environmental remediation. By harnessing the synergistic effects of natural geopolymer and TiO₂ nanoparticles, these geopolymer-based films exhibit outstanding promise in addressing water decontamination challenges and contribute to the development of eco-friendly solutions for a cleaner and healthier environment.

Keywords: geopolymer, TiO2 nanoparticles, photocatalytic materials, water decontamination, sustainable remediation

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Authors: O. Hanita, S. A. Ainnul Hamidah, A. H. Yang Zalila, M. R. Siti Nadiah, M. H. Najihah, M. A. Hapipah

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The crude extract of the leaves of Actinodaphne sesquipedalis Hook. F. Var. Glabra (Kochummen), was taken under phytochemical investigation. The crude methanolic extract was partitioned with a different solvent system by increasing their polarities (n-hexane, dichloromethane, and methanol). The compounds were fractionated and isolated from n-hexane partition by using column chromatography with silica gel 60 or Sephadex LH-20 as a stationary phase and preparative thin layer chromatographic technique. Isolates were characterized using TLC, FTIR, UV spectrophotometer and NMR spectroscopy. The n-hexane fractionates yielded a total of four compounds namely N-methyllaurotetanine (1), dicentrine (2), β-sitosterol (3), and stigmasterol (4). The result indicates that the leaves of Actinodaphne sesquipedalis may provide a rich source of alkaloids and triterpenoids.

Keywords: actinodaphne sesquipedalis, alkaloids, phytochemical investigation, triterpenoids

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Authors: Ayla Roberta Galaco, Juliana Fonseca De Lima, Osvaldo Antonio Serra

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Coordination polymers, also known as metal-organic frameworks (MOFs) or lanthanoide organic frameworks (LOFs) have been reported due of their promising applications in gas storage, separation, catalysis, luminescence, magnetism, drug delivery, and so on. As a type of organic–inorganic hybrid materials, the properties of coordination polymers could be chosen by deliberately selecting the organic and inorganic components. LOFs have received considerable attention because of their properties such as porosity, luminescence, and magnetism. Methods such as solvothermal synthesis are important as a strategy to control the structural and morphological properties as well as the composition of the target compounds. In this work the first solvothermal synthesis was employed to obtain the compound [Y0.4,Yb0.4,Er0.2(dmf)(for)(H2O)(tft)], by using terephthalic acid (tft) and oxalic acid, decomposed in formate (for), as ligands; Yttrium, Ytterbium and, Erbium as metal centers, in DMF and water for 4 days under 160 °C. The semi-rigid terephthalic acid (dicarboxylic) coordinates with Ln3+ ions and also is possible to form a polyfunctional bridge. On the other hand, oxalate anion has no high-energy vibrational groups, which benefits the excitation of Yb3+ in upconversion process. It was observed that the compounds with water molecules in the coordination sphere of the lanthanoide ions cause lower crystalline properties and change the structure of the LOF (1D, 2D, 3D). In the FTIR, the bands at 1589 and 1500 cm-1 correspond to the asymmetric stretching vibration of –COO. The band at 1383 cm-1 is assigned to the symmetric stretching vibration of –COO. Single crystal X-ray diffraction study reveals an infinite 3D coordination framework that crystalizes in space group P21/c. The other three products, [TR(chel)(ofd)0,5(H2O)2], where TR= Eu3+, Y3, and Yb3+/Er3+ were obtained by using 1, 2-phenylenedioxydiacetic acid (ofd) and chelidonic acid (chel) as organic ligands. Thermal analysis shows that the lanthanoide organic frameworks do not collapse at temperatures below 250 °C. By the polycrystalline X-ray diffraction patterns (PXRD) it was observed that the compounds with Eu3+, Y3+, and Yb3+/Er3+ ions are isostructural. From PXRD patterns, high crystallinity can be noticed for the complexes. The final products were characterized by single X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), energy dispersive spectroscopy (EDS) and thermogravimetric analysis (TGA). The X-ray diffraction (XRD) is an effective method to investigate crystalline properties of synthesized materials. The solid crystal obtained in the synthesis show peaks at 2θ < 10°, indicating the MOF formation. The chemical composition of LOFs was also confirmed by EDS.

Keywords: isostructural, lanthanoids, lanthanoids organic frameworks (LOFs), metal organic frameworks (MOFs), thermogravimetry, X-Ray diffraction

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Authors: Jahangir Ahmad Rather, Emad A. Khudaish, Ahsanulhaq Qurashi, Palanisamy Kannan

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Chemical modification and assembling of fullerenes are fundamentally important for the application of fullerenes as functional molecules and in molecular devices and organic electronic devices. We have synthesized fullerene nanorods C60NRs conjugate via liquid-liquid interface and the synthesized C60NRs was characterized by FTIR spectroscopy, field emission electron microscopy (FESEM) and X-ray diffraction techniques. The C60NRs were immobilized on glassy carbon electrode via surface bound diazonium salts as an impact strategy. This method involves electrografting of p–nitrophenyl to give GCE–Ph–NO2 and then the terminal nitro-group was chemically reduced to GCE–Ph–NH2 in a presence of sodium borohydride/gold–polyaniline nanocomposite (NaBH4/Au–PANI). The Au–PANI composite was synthesized and characterized by FTIR, UV-vis, SEM and EDX techniques. The C60NRs were immobilized on GCE–Ph–NH2 via amination reaction which involves N-H addition across a π-bond on [60] fullerene. The immobilized C60NRs/GCE was subjected to electrochemical reduction in 1.0 M KOH to yield ERC60NRs/GCE sensor. The developed sensor shows high electrocatalytic activity for the detection of ethylparaben (EP) over a concentration range from 0.01 to 0.52 µM with a detection limit (LOD) 3.8 nM. The amount of EP present in the nourishing repair cream (OlAY®) was determined by standard addition method at the developed ERC60NRs/GCE sensor. The total concentration of EP was found to be 0.011 µM (0.1%) and is within the permissible limit of 0.19 % EP in cosmetics according to the European scientific committee (SCCS) on consumer safety on 22 March 2011 (SCCS/1348/11).

Keywords: diazonium salt reduction, ethylparaben (EP), endocrine disruptor, fullerene nanorods (C60NRs), gold–polyaniline nanocomposite (Au–PANI)

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Authors: Mahmoud H. Abu Elella, Riham R. Mohamed, Magdy W. Sabaa

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Introduction: Microbial pollution is global problem threatening the human health. It is resulted by pathogenic microorganisms such as Escherichia coli (E. coli), Staphylococcus aureus (S. aureus) and other pathogenic strains. They cause a dangerous effect on human health, so great efforts have been exerted to produce new and effective antimicrobial agents. Nowadays, natural polysaccharides, such as chitosan and its derivatives are used as antimicrobial agents. The aim of our work is to synthesize of a biodegradable polymer such as N-quaternized chitosan (NQC) then Characterization of NQC by using different analysis techniques such as Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM) and using it as an antibacterial agent against different pathogenic bacteria. Methods: Synthesis of NQC using dimethylsulphate. Results: FTIR technique exhibited absorption peaks of NQC, SEM images illustrated that surface of NQC was smooth and antibacterial results showed that NQC had a high antibacterial effect. Discussion: NQC was prepared and it was proved by FTIR technique and SEM images antibacterial results exhibited that NQC was an antibacterial agent.

Keywords: antimicrobial agent, N-quaternized chitosan chloride, silver nanocomposites, sodium polyacrylate

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Authors: Mehrzad Mohabbi Yadollahi, Pouneh Abdollahifard, Behzad Mokhtare, Majid Atashafrazeh

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Geopolymers are believed to provide good fire resistance. The effects of elevated temperatures on mechanical and microstructural properties of pumice-based geopolymer were investigated in this study. Pumice based geopolymer was exposed to elevated temperatures of 200, 400, 600, and 800 ºC for 3 hours. The residual strength of these specimens was determined after cooling at room temperature and microstructures of these samples were investigated by FTIR and SEM analyses. Specimens which were initially grey turned reddish accompanied by the appearance of cracks as temperatures increased to 600 and 800 ºC.

Keywords: geopolymer, pumice, elevated temperature, SEM, FTIR

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Authors: Miyeon Yoo, Sewon Kim, Changyeop Lee

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It is important to measure the internal temperature or temperature distribution precisely in combustion system to increase energy efficiency and reduce the pollutants. Especially in case of large combustion systems such as power plant boiler and reheating furnace of steel making process, it is very difficult to measure those physical properties in detail. Tunable diode laser absorption spectroscopy measurement and analysis can be attractive method to overcome the difficulty. In this paper, TDLAS methods are used to measure the oxygen concentration and temperature distribution in various experimental conditions.

Keywords: tunable diode laser absorption Spectroscopy, temperature distribution, gas concentration

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Authors: A. N. Kurbanova, G. K. Sugurbekova, N. K. Akhmetov

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The asphaltenes are heavy fraction of crude oil. Asphaltenes on oilfield is known for its ability to plug wells, surface equipment and pores of the geologic formations. The present research is devoted to the deasphalting of crude oil as the initial stage refining oil. Solvent deasphalting was conducted by extraction with organic solvents (cyclohexane, carbon tetrachloride, chloroform). Analysis of availability of metals was conducted by ICP-MS and spectral feature at deasphalting was achieved by FTIR. High contents of asphaltenes in crude oil reduce the efficiency of refining processes. Moreover, high distribution heteroatoms (e.g., S, N) were also suggested in asphaltenes cause some problems: environmental pollution, corrosion and poisoning of the catalyst. The main objective of this work is to study the effect of deasphalting process crude oil to improve its properties and improving the efficiency of recycling processes. Experiments of solvent extraction are using organic solvents held in the crude oil JSC “Pavlodar Oil Chemistry Refinery. Experimental results show that deasphalting process also leads to decrease Ni, V in the composition of the oil. One solution to the problem of cleaning oils from metals, hydrogen sulfide and mercaptan is absorption with chemical reagents directly in oil residue and production due to the fact that asphalt and resinous substance degrade operational properties of oils and reduce the effectiveness of selective refining of oils. Deasphalting of crude oil is necessary to separate the light fraction from heavy metallic asphaltenes part of crude oil. For this oil is pretreated deasphalting, because asphaltenes tend to form coke or consume large quantities of hydrogen. Removing asphaltenes leads to partly demetallization, i.e. for removal of asphaltenes V/Ni and organic compounds with heteroatoms. Intramolecular complexes are relatively well researched on the example of porphyinous complex (VO2) and nickel (Ni). As a result of studies of V/Ni by ICP MS method were determined the effect of different solvents-deasphalting – on the process of extracting metals on deasphalting stage and select the best organic solvent. Thus, as the best DAO proved cyclohexane (C6H12), which as a result of ICP MS retrieves V-51.2%, Ni-66.4%? Also in this paper presents the results of a study of physical and chemical properties and spectral characteristics of oil on FTIR with a view to establishing its hydrocarbon composition. Obtained by using IR-spectroscopy method information about the specifics of the whole oil give provisional physical, chemical characteristics. They can be useful in the consideration of issues of origin and geochemical conditions of accumulation of oil, as well as some technological challenges. Systematic analysis carried out in this study; improve our understanding of the stability mechanism of asphaltenes. The role of deasphalted crude oil fractions on the stability asphaltene is described.

Keywords: asphaltenes, deasphalting, extraction, vanadium, nickel, metalloporphyrins, ICP-MS, IR spectroscopy

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Authors: Eva Slaninova, Diana Cernayova, Zuzana Sedrlova, Katerina Mrazova, Petr Sedlacek, Jana Nebesarova, Stanislav Obruca

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Cyanobacteria are gram-negative prokaryotes belonging to a group of photosynthetic bacteria. In comparison with heterotrophic microorganisms, cyanobacteria utilize atmospheric nitrogen and carbon dioxide without any additional substrates. This ability of these microorganisms could be employed in biotechnology for the production of bioplastics, concretely polyhydroxyalkanoates (PHAs) which are primarily accumulated as a storage material in cells in the form of intracellular granules. In this study, there two cyanobacterial cultures from genera Synechocystis were used, namely Synechocystic sp. PCC 6803 and Synechocystis salina CCALA 192. There were optimized and used several various approaches, including microscopic techniques such as cryo-scanning electron microscopy (Cryo-SEM) and transmission electron microscopy (TEM), and fluorescence lifetime imaging microscopy using Nile red as a fluorescent probe (FLIM). Due to these instrumental techniques, the morphology of intracellular space and surface of cells were characterized. The next group of methods which were employed was spectroscopic techniques such as UV-Vis spectroscopy measured in two modes (turbidimetry and integration sphere) and Fourier transform infrared spectroscopy (FTIR). All these diverse techniques were used for the detection and characterization of pigments (chlorophylls, carotenoids, phycocyanin, etc.) and PHAs, in our case poly (3-hydroxybutyrate) (P3HB). To verify results, gas chromatography (GC) was employed concretely for the determination of the amount of P3HB in biomass. Cyanobacteria were also characterized as polyhydroxybutyrate producers by flow cytometer, which could count cells and at the same time distinguish cells including P3HB and without due to fluorescent probe called BODIPY and live/dead fluorescent probe SYTO Blue. Based on results, P3HB content in cyanobacteria cells was determined, as also the overall fitness of the cells. Acknowledgment: Funding: This study was partly funded by the projectGA19-29651L of the Czech Science Foundation (GACR) and partly funded by the Austrian Science Fund (FWF), project I 4082-B25.

Keywords: cyanobacteria, fluorescent probe, microscopic techniques, poly(3hydroxybutyrate), spectroscopy, chromatography

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Authors: Suheyla Kocaman, Gulnare Ahmetli

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In this study, acrylated soybean oil (AESO) was used as modifying agent for DGEBF-type epoxy resin (ER). AESO was used as a co-matrix in 50 wt % with ER. Composites with eco-friendly natural fillers-banana bark and seashell were prepared. MNA was used as a hardener. Effect of banana peel (BP) and seashell (SSh) fillers on mechanical properties, such as tensile strength, elongation at break, and hardness of M-ERs were investigated. The structure epoxy resins (M-ERs) cured with MNA and sebacic acid (SAc) hardeners were characterized by Fourier transform infrared spectroscopy (FTIR). Tensile test results show that Young’s (elastic) modulus, tensile strength and hardness of SSh particles reinforced with M-ERs were higher than the M-ERs reinforced with banana bark.

Keywords: biobased composite, epoxy resin, mechanical properties, natural fillers

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Authors: G. S. Sudha, Smita Mohanty, S. K. Nayak

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Epoxidized oils can replace petroleum derived materials in numerous industrial applications, because of their respectable oxirane oxygen content and high reactivity of oxirane ring. Epoxidized castor oil (ECO) has synthesized in the presence of a sulphonated polystyrene type cation exchange resin. The formation of the oxirane ring was confirmed by Fourier Transform Infrared Spectroscopy (FTIR) analysis. The epoxidation reaction was evaluated by Nuclear Magnetic Resonance (NMR) studies. ECO is used as a toughening phase to increase the toughness of petroleum-based epoxy resin.

Keywords: epoxy resin, epoxidized castor oil, sulphonated polystyrene type cation exchange resin, petroleum derived materials

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Authors: C.W. Kan

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This paper investigates the use of atmospheric pressure plasma for improving the surface hydrophobicity of polyurethane synthetic leather with tetramethylsilane (TMS). The atmospheric pressure plasma treatment with TMS is a single-step process to enhance the hydrophobicity of polyurethane synthetic leather. The hydrophobicity of the treated surface was examined by contact angle measurement. The physical and chemical surface changes were evaluated by scanning electron microscopy (SEM) and infrared spectroscopy (FTIR). The purpose of this paper is to provide learning materials for understanding how to use atmospheric pressure plasma in the textile finishing process to transform a hydrophilic surface to hydrophobic.

Keywords: Learning materials, atmospheric pressure plasma treatment, hydrophobic, hydrophilic, surface

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Authors: Ali Garba Danjani, Abdulrasheed Halliru Usman

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Due to the rapidly increasing biological applications and antibacterial properties of versatile chitosan composites, the effects of chitosan/polyvinyl chloride composites film were investigated. Chitosan/polyvinyl chloride films were prepared by a casting method. Polyethylene glycol (PEG) was used as a plasticizer in the blending stage of film preparation. Characterizations of films were done by Scanning Electron microscopy (SEM), Fourier transforms infrared spectroscopy (FTIR), and thermogravimetric analyzer (TGA). Chitosan composites incorporation enhanced the antibacterial activity of chitosan films against Escherichia coli and Staphylococcus aureus. The composite film produced is proposed as packaging or coating material because of its flexibility, antibacterial efficacy, and good mechanical strength.

Keywords: chitosan, polymeric nanocomposites, antibacterial activity, polymer blend

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Authors: C. Girometta, S. Babbini, R. M. Baiguera, D. S. Branciforti, M. Cartabia, D. Dondi, M. Pellegrini, A. M. Picco, E. Savino

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Interest on wood decay fungi (WDF) has been increasing in the last year's thanks to the potentiality of this kind of fungi; research on new WDF strains has increased as well thus pointing out the key role of the culture collections. One of the most recent biotechnological application of WDF is the development of novel materials from natural or recycled resources. Based on different combinations of fungal species, substrate, and processing treatment involved (e.g. heat pressing), it is possible to achieve a wide variety of materials with different features useful for many industrial applications: from packaging to thermal and acoustic insulation. In comparison with the conventional ones, these materials represent a 100% natural and compostable alternative involving low amounts of energy in the production process. The purpose of the present work was to isolate and select WDF strains able to colonize and degrade different plant wastes thus producing a fungal biomass shapeable to achieve bio-composite materials. Strains were selected within the mycological culture collection of Pavia University (MicUNIPV, over 300 strains of WDF). The selected strains have been investigated with regards their ability to colonize and degrade plant residues from the local major cultivations (e.g. poplar, alfalfa, maize, rice, and wheat) and produce the fungal biomass. The degradation of the substrate was assessed by Thermogravimetric analysis (TGA) and Fourier Transform Infrared Spectroscopy (FTIR). Chemical characterization confirmed that TGA and FTIR are complementary techniques able to provide quality-quantitative information on compositional and structural variation that occurs during the transformation from the substrate to the bio-composite material. This pilot study provides a fundamental step to tune further applications in fungus-residues composite biomaterials.

Keywords: bio-composite material, lignocellulosic residues, sustainable materials, wood decay fungi

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Authors: J. V. Gonzalez Fernandez, T. Mozume, S. Gozu, A. Lastras Martinez, L. F. Lastras Martinez, J. Ortega Gallegos, R. E. Balderas Navarro

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We report on a theoretical-experimental study of photoreflectance anisotropy (PRA) spectroscopy of coupled double quantum wells. By probing the in-plane interfacial optical anisotropies, we demonstrate that PRA spectroscopy has the capacity to detect and distinguish layers with quantum dimensions. In order to account for the experimental PRA spectra, we have used a theoretical model at k=0 based on a linear electro-optic effect through a piezoelectric shear strain.

Keywords: coupled double quantum well (CDQW), linear electro-optic (LEO) effect, photoreflectance anisotropy (PRA), piezoelectric shear strain

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Authors: Ali Naeemy, Mir Ghasem Hoseini

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In this study, for the first time, an analytical method developed and validated by combining electrochemical impedance spectroscopy and electromembrane extraction (EIS-EME) by Vulcan/poly pyrrole nanocomposite modified screen-printed electrode (PPY–VU/SPE) for accurately quantifying zolpidem. EME parameters optimized, including solvent composition, voltage, pH adjustments and extraction time. Zolpidem was transferred from a donor solution (pH 5) to an acceptor solution (pH 13) using a hollow fiber in 1-octanol as a membrane, driven by a 60 V voltage for 25 minutes, ensuring precise and selective extraction. In comparison with SPE, VU/SPE and PPY/SPE, the PPY–VU/SPE was much more efficient for ZP oxidation. Calibration curves with good linearity were obtained in the concentration range of 2-75 µmol L-1 using the EIS-EME with the detection limit of 0.5 µmol L-1 . Finally, the EIS-EME by using the PPY– VU/SPE was successfully used to determine ZP in tablet dosage form, urine and plasma samples. Keywords: Electrochemical impedance spectroscopy, Electromembrane extraction, Zolpidem, Vulcan, poly pyrrole, Screen printed electrode

Keywords: electrochemical impedance spectroscopy, electromembrane extraction, screen printed electrode, zolpidem

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Authors: Ke Lin, Steve Wu Qing Yang, Zhang Nan

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The medicine and drugs has in the past been manufactured to the final products and then used laboratory analysis to verify their quality. However the industry needs crucially a monitoring technique for the final batch to batch quality check. The introduction of process analytical technology (PAT) provides an incentive to obtain real-time information about drugs on the production line, with the following optical techniques being considered: near-infrared (NIR) spectroscopy, Raman spectroscopy and imaging, mid-infrared spectroscopy with the use of chemometric techniques to quantify the final product. However, presents problems in that the spectra obtained will consist of many combination and overtone bands of the fundamental vibrations observed, making analysis difficult. In this work, we describe a non-destructive system and method for capsule and liquid medicine identification, more particularly, using terahertz time-domain spectroscopy and/or designed terahertz portable system for identifying different types of medicine in the package of capsule or in liquid medicine bottles. The target medicine can be detected directly, non-destructively and non-invasively.

Keywords: terahertz, non-destructive, non-invasive, chemical identification

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Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, L. Kalina, M. Hajdúchová, V. Enev, J. Wasserbauer

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In this work, copper ferrite CuFe2O4 spinel ferrite nanoparticles with different particle size at different annealing temperature were synthesized using the starch-assisted sol-gel auto-combustion method. The synthesized nanoparticles were characterized by conventional powder X-ray diffraction (XRD) spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, Field-Emission Scanning Electron Microscopy, X-ray Photoelectron Spectroscopy, and Vibrating Sample Magnetometer. The XRD patterns confirmed the formation of CuFe2O4 spinel ferrite nanoparticles. Field-Emission Scanning Electron Microscopy revealed that particles are of spherical morphology with particle size 5-20 nm at lower annealing temperature. An infrared spectroscopy study showed the presence of two principal absorption bands in the frequency range around 530 cm-1 (ν1) and around 360 cm-1 (ν2); which indicate the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Raman spectroscopy study also indicated the change in octahedral and tetrahedral site related Raman modes in copper ferrite nanoparticles with change of particle size. This change in magnetic behavior with change of particle size of CuFe2O4 nanoparticles was also observed. The change in magnetic properties with change of particle size is due to cation redistribution, which was confirmed by X-Ray photoelectron study.

Keywords: copper ferrite, nanoparticles, magnetic property, CuFe2O4

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Authors: Tasnuva Tamanna, Aimin Yu

Abstract:

Application of nanoscience in biomedical field has come across as a new era. This study involves the synthesis of nano drug carrier with antibiotic loading. Based on the founding that polydopamine (PDA) nanoparticles could be formed via self-polymerization of dopamine at alkaline pH, one-step synthesis of rifampicin coupled polydopamine (PDA-R) nanoparticles was achieved by adding rifampicin into the dopamine solution. The successful yield of PDA nanoparticles with or without the presence of rifampicin during the polymerization process was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. Drug loading was monitored by UV-vis spectroscopy and the loading efficiency of rifampicin was calculated to be 76%. Such highly capacious nano-reservoir was found very stable with little drug leakage at pH 3.

Keywords: drug loading, nanoparticles, polydopamine, rifampicin

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Authors: Shaeel A. Al Thabaiti, Sulaiman N. Basahel, Salem M. Bawaked, Mohamed Mokhtar

Abstract:

Nanosheets for cobalt-layered double hydroxide (Co-Al-LDH)/GO were successfully synthesized with different Co:M g:Al ratios (0:3:1, 1.5:1.5:1, and 3:0:1). The layered double hydroxide structure and morphology were determined using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). Temperature prgrammed reduction (TPR) of Co-Al-LDH showed reduction peaks at lower temperature which indicates the ease reducibility of this particular sample. The thermal behaviour was studied using thermal graviemetric technique (TG), and the BET-surface area was determined using N2 physisorption at -196°C. The C-C coupling reaction was carried out over all the investigated catalysts. The Mg–Al LDH catalyst without Co ions is inactive, but the isomorphic substitution of Mg by Co ions (Co:Mg:Al = 1.5:1.5:1) in the cationic sheet resulted in 88% conversion of iodobenzene under reflux. LDH/GO hybrid is up to 2 times higher activity than for the unsupported LDH.

Keywords: adsorption, co-precipitation, graphene oxide, layer double hydroxide

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Authors: Eliane G. Tótoli, Hérida Regina N. Salgado

Abstract:

Daptomycin is an important antimicrobial agent used in clinical practice nowadays, since it is very active against some Gram-positive bacteria that are particularly challenges for the medicine, such as methicillin-resistant Staphylococcus aureus (MRSA) and vancomycin-resistant Enterococci (VRE). The importance of environmental preservation has receiving special attention since last years. Considering the evident need to protect the natural environment and the introduction of strict quality requirements regarding analytical procedures used in pharmaceutical analysis, the industries must seek environmentally friendly alternatives in relation to the analytical methods and other processes that they follow in their routine. In view of these factors, green analytical chemistry is prevalent and encouraged nowadays. In this context, infrared spectroscopy stands out. This is a method that does not use organic solvents and, although it is formally accepted for the identification of individual compounds, also allows the quantitation of substances. Considering that there are few green analytical methods described in literature for the analysis of daptomycin, the aim of this work was the development and validation of a green analytical method for the quantification of this drug in lyophilized powder for injectable solution, by Fourier-transform infrared spectroscopy (FT-IR). Method: Translucent potassium bromide pellets containing predetermined amounts of the drug were prepared and subjected to spectrophotometric analysis in the mid-infrared region. After obtaining the infrared spectrum and with the assistance of the IR Solution software, quantitative analysis was carried out in the spectral region between 1575 and 1700 cm-1, related to a carbonyl band of the daptomycin molecule, and this band had its height analyzed in terms of absorbance. The method was validated according to ICH guidelines regarding linearity, precision (repeatability and intermediate precision), accuracy and robustness. Results and discussion: The method showed to be linear (r = 0.9999), precise (RSD% < 2.0), accurate and robust, over a concentration range from 0.2 to 0.6 mg/pellet. In addition, this technique does not use organic solvents, which is one great advantage over the most common analytical methods. This fact contributes to minimize the generation of organic solvent waste by the industry and thereby reduces the impact of its activities on the environment. Conclusion: The validated method proved to be adequate to quantify daptomycin in lyophilized powder for injectable solution and can be used for its routine analysis in quality control. In addition, the proposed method is environmentally friendly, which is in line with the global trend.

Keywords: daptomycin, Fourier-transform infrared spectroscopy, green analytical chemistry, quality control, spectrometry in IR region

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Authors: Charles Klein O. Gorit, Mark Tristan J. Quimque Jr., M. Cecilia V. Almeda, Concepcion M. Salvana

Abstract:

Chitosan is a promising biopolymer commonly found in crustacean shells that has plausible effects in water purification and wastewater treatment. It is a primary derivative of chitin and considered second of the most abundant biopolymer prior to cellulose. Morphological analysis had been done using Scanning Electron Microscopy with Energy Dispersive Microscopy (SEM/EDS), and due to its porous nature, it showcases a certain degree of porosity, hence, larger adsorption site of heavy metal. The Energy Dispersive Spectroscopy of the chitosan and ‘lead-bound’ chitosan, shows a relative increase of percent abundance of lead cation from 1.44% to 2.08% hence, adsorption occurs. Chitosan, as a nitrogenous polysaccharide, subjected to Fourier transform infrared spectroscopy (FTIR) analysis shows amide bands ranging from 1635.36 cm⁻¹ for amide 1 band and 1558.40 cm-1 for amide 2 band with NH stretching. For ‘lead-bound’ chitosan, the FT-IR analysis shows a change in peaks upon adsorption of Pb(II) cation. The spectrum shows broadening of OH and NH stretching band. Such observation can be attributed to the probability that the attachment of Pb(II) ions is in these functional groups. A column filter was devised with lead-bound chitosan to determine the zero point charge (pHzpc) of the biopolymer. The results show that at pH 8.34, below than the zpc level of literatures cited for lead which ranges from pH 4 to 7, favors the adsorption site of chitosan and its capability to adsorb traces amount of aqueous lead.

Keywords: chitosan, biopolymer, FT-IR, SEM, zero-point charge, heavy metal, lead ions

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Authors: Yaseen Elhebshi, Abdulkareem Hamid, Nureddin Bin Issa, Xiaonong Chen

Abstract:

A convenient method of preparing ultrafine polystyrene latex nano-particles with amino groups on the surface is developed. Polystyrene latexes in the size range 50–400 nm were prepared via emulsion polymerization, using sodium dodecyl sulfate (SDS) as surfactant. Polystyrene with amino groups on the surface will be fine to use as organic filler to modify rubber. Transmission electron microscopy (TEM) was used to observe the morphology of silicon dioxide and functionalized polystyrene nano-particles. The nature of bonding between the polymer and the reactive groups on the filler surfaces was analyzed using Fourier transform infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) was employed to examine the filler surface.

Keywords: reactive filler, emulsion polymerization, particle size, polystyrene nanoparticles

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Authors: Mahmoud H. Abu Elella, Riham R. Mohamed, Magdy W. Sabaa

Abstract:

Firstly, synthesis of N-Quaternized Chitosan (NQC), then it was proven by FTIR and 1H-NMR analysis. The degree of quaternization(DQ 35% ) was determined by equation. Secondly, synthesis of cross-linked hydrogels composed of NQC and poly (vinyl alcohol) (PVA) in different weight ratios in presence of glutaraldehyde (GA) as cross-linking agent. Characterization of the prepared hydrogels was done using FTIR, SEM, XRD,and TGA. Swellability in simulated body fluid (SBF) solutions applied on NQC / PVA hydrogels and swelling rate(Wt%) and metal ions uptake was done on it.

Keywords: hydrogel, metal ions uptake, N-quaternized chitosan, poly (vinyl alcohol), swellability

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Authors: Touka Nassim, Tabli Dalila

Abstract:

In this study, CuO thin films synthesized via simple sol-gel method, have been deposited on glass substrates by the spin coating technique and annealed at various temperatures. Samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier-transform infrared (FT-IR) and Raman spectroscopy, and UV-visible spectroscopy. The structural characterization by XRD reveals that the as prepared films were tenorite phase and have a high level of purity and crystallinity. The crystallite size of the CuO films was affected by the annealing temperature and was estimated in the range 20-31.5 nm. SEM images show a homogeneous distribution of spherical nanoparticles over the surface of the annealed films at 350 and 450 °C. Vibrational Spectroscopy revealed vibration modes specific to CuO with monolithic structure on the Raman spectra at 289 cm−1 and on FT-IR spectra around 430-580 cm−1. Electronic investigation performed by UV–Visible spectroscopy showed that the films have high absorbance in the visible region and their optical band gap increases from 2.40 to 2.66 eV (blue shift) with increasing annealing temperature from 350 to 550 °C.

Keywords: Sol-gel, Spin coating method, Copper oxide, Thin films

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