Search results for: UV-Visible absorption spectroscopy (UV-Vis)

Authors: Nonhlanhla Nkosi, Kulsum Kondiah

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The toxicological manifestation of heavy metals motivates interest towards the development of a reliable, eco-friendly biosorption process. With that being said, the aim of the current study was to characterise the EPS from heavy-metal resistant bacteria isolated from acid mine decant on the West Rand, Gauteng, South Africa. To achieve this, six exopolysaccharide (EPS) producing, metal resistant strains (Pb101, Pb102, Pb103, Pb204, Co101, and Ni101) were identified as Bacillus safensis strain NBRC 100820, Bacillus proteolyticus, Micrococcus luteus, Enterobacter sp. Pb204, Bacillus wiedmannii and Bacillus zhangzhouensis, respectively with 16S rRNA sequencing. Thereafter, EPS was extracted using chemical (formaldehyde/NaOH) and physical (ultrasonification) methods followed by physicochemical characterisation of carbohydrate, DNA, and protein contents using chemical assays and spectroscopy (FTIR- Fourier transformed infrared and 3DEEM- three-dimensional excitation-emission matrix fluorescence spectroscopy). EPS treated with formaldehyde/NaOH showed better recovery of macromolecules than ultrasonification. The results of the present study showed that carbohydrates were more abundant than proteins, with carbohydrate and protein concentrations of 8.00 mg/ml and 0.22 mg/ml using chemical method in contrast to 5.00 mg/ml and 0.77 mg/ml using physical method, respectively. The FTIR spectroscopy results revealed that the extracted EPS contained hydroxyl, amide, acyl, and carboxyl groups that corresponded to the aforementioned chemical analysis results, thus asserting the presence of carbohydrates, DNA, polysaccharides, and proteins in the EPS. These findings suggest that identified functional groups of EPS form surface charges, which serve as the binding sites for suspended particles, thus possibly mediating adsorption of divalent cations and heavy metals. Using the extracted EPS in the development of a cost-effective biosorption solution for industrial wastewater treatment is attainable.

Keywords: biosorbent, exopolysaccharides, heavy metals, wastewater treatment

Procedia PDF Downloads 147

Authors: M. H. Pazandeh, M. Doudi, S. Barahimi, L. Rahimzadeh Torabi

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The use of antibiotics is essential in reducing the occurrence of adverse effects and inhibiting the emergence of antibiotic resistance in microbial populations. The necessity for a novel methodology concerning local administration of antibiotics has arisen, with particular focus on dealing with localized infections prompted by bacterial colonization of medical devices or implant materials. Bioactive glasses (BG) are extensively employed in the field of regenerative medicine, encompassing a diverse range of materials utilized for drug delivery systems. In the present investigation, various drug carriers for imipenem and tetracycline, namely single systems BG/SnO2, BG/NiO with varying proportions of metal oxide, and nanocomposite BG/SnO2/NiO, were synthesized through the sol-gel technique. The antibacterial efficacy of the synthesized samples was assessed through the utilization of the disk diffusion method with the aim of neutralizing Staphylococcus aureus as the bacterial model. The current study involved the examination of the bioactivity of two samples, namely BG10SnO2/10NiO and BG20SnO2, which were chosen based on their heightened bacterial inactivation properties. This evaluation entailed the employment of two techniques: the measurement of the pH of simulated body fluid (SBF) solution and the analysis of the sample tablets through X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy. The sample tablets were submerged in SBF for varying durations of 7, 14, and 28 days. The bioactivity of the composite bioactive glass sample was assessed through characterization of alterations in its surface morphology, structure, and chemical composition. This evaluation was performed using scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy, and X-ray diffraction spectroscopy. Subsequently, the sample was immersed in simulated liquids to simulate its behavior in biological environments. The specific body fat percentage (SBF) was assessed over a 28-day period. The confirmation of the formation of a hydroxyapatite surface layer serves as a distinct indicator of bioactivity. The infusion of antibiotics into the composite bioactive glass specimen was done separately, and then the release kinetics of tetracycline and imipenem were tested in simulated body fluid (SBF). Antimicrobial effectiveness against various bacterial strains have been proven in numerous instances using both melt and sol-gel techniques to create multiple bioactive glass compositions. An elevated concentration of calcium ions within a solution has been observed to cause an increase in the pH level. In aqueous suspensions, bioactive glass particles manifest a significant antimicrobial impact. The composite bioactive glass specimen exhibits a gradual and uninterrupted release, which is highly desirable for a drug delivery system over a span of 72 hours. The reduction in absorption, which signals the loss of a portion of the antibiotic during the loading process from the initial phosphate-buffered saline solution, indicates the successful bonding of the two antibiotics to the surfaces of the bioactive glass samples. The sample denoted as BG/10SnO2/10NiO exhibits a higher loading of particles compared to the sample designated as BG/20SnO2 in the context of bioactive glass. The enriched sample demonstrates a heightened bactericidal impact on the bacteria under investigation while concurrently preserving its antibacterial characteristics. Tailored bioactive glass that incorporates hydroxyapatite, with a regulated and efficient release of drugs targeting bacterial infections, holds promise as a potential framework for bone implant scaffolds following rigorous clinical evaluation, thereby establishing potential future biomedical uses. During the modification process, the introduction of metal oxides into bioactive glass resulted in improved antibacterial characteristics, particularly in the composite bioactive glass sample that displayed the highest level of efficiency.

Keywords: antibacterial, bioactive glasses, implant infections, multi drug resistant

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Authors: Špela Hajduk, Sean P. Berglund, Matejka Podlogar, Goran Dražić, Fatwa F. Abdi, Zorica C. Orel, Menny Shalom

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Graphitic carbon nitride materials (g-CN) have emerged as an attractive photocatalyst and electrocatalyst for photo and electrochemical water splitting reaction, due to their environmental benignity nature and suitable band gap. Many approaches were introduced to enhance the photoactivity and electronic properties of g-CN and resulted in significant changes in the electronic and catalytic properties. Here we demonstrate the synthesis of thin and homogenous g-CN layer on highly ordered ZnO nanowire (NW) substrate by growing a seeding layer of small supramolecular assemblies on the nanowires. The new synthetic approach leads to the formation of thin g-CN layer (~3 nm) without blocking all structure. Two different deposition methods of carbon nitride were investigated and will be presented. The amount of loaded carbon nitride significantly influences the PEC activity of hybrid material and all the ZnO/g-CNx electrodes show great improvement in photoactivity. The chemical structure, morphology and optical properties of the deposited g-CN were fully characterized by various techniques as X-ray powder spectroscopy (XRD), scanning electron microscopy (SEM), focused ion beam scanning electron microscopy (FIB-SEM), high-resolution scanning microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS).

Keywords: carbon nitride, photoanode, solar water splitting, zinc oxide

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Authors: Syahidah N. Zulkifli, Herlina A. Rahim, Nurul A. M. Subha

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Sustaining water quality is critical in order to avoid any harmful health consequences for end-user consumers. The detection of microbial impurities at the household level is the foundation of water security. Water quality is now monitored only at water utilities or infrastructure, such as water treatment facilities or reservoirs. This research provides a first-hand scientific understanding of microbial composition presence in Malaysia’s household point-of-use (POUs) water supply influenced by seasonal fluctuations, standstill periods, and flow dynamics by using the NIR-Raman spectroscopic technique. According to the findings, 20% of water samples were contaminated by pathogenic bacteria, which are Legionella and Salmonella cells. A comparison of the spectra reveals significant signature peaks (420 cm⁻¹ to 1800 cm⁻¹), including species-specific bands. This demonstrates the importance of regularly monitoring POUs water quality to provide a safe and clean water supply to homeowners. Conventional Raman spectroscopy, up-to-date, is no longer suited for real-time monitoring. Therefore, this study introduced an alternative micro-spectrometer to give a rapid and sustainable way of monitoring POUs water quality. Assessing microbiological threats in water supply becomes more reliable and efficient by leveraging IoT protocol.

Keywords: microbial contaminants, water quality, water monitoring, Raman spectroscopy

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Authors: Lucija Pustahija, Christine Bandl, Wolfgang Kern, Christian Mitterer

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Concerning today´s ecological demands, producing reliable materials from sustainable resources is a continuously developing topic. Such an example is the production of carbon materials via pyrolysis of natural gases or biomass. The amazing properties of pyrolytic carbon are utilized in various fields, where in particular the application in building industry is a promising way towards the utilization of pyrolytic carbon and composites based on pyrolytic carbon. For many applications, surface modification of carbon is an important step in tailoring its properties. Therefore, in this paper, an investigation of different oxidation methods was performed to prepare the carbon surface before functionalizing it with organosilanes, which act as coupling agents for epoxy and polyurethane resins. Made in such a way, a building material based on carbon composites could be used as a lightweight, durable material that can be applied where water or air filtration / purification is needed. In this work, both wet and dry oxidation were investigated. Wet oxidation was first performed in solutions of nitric acid (at 120 °C and 150 °C) followed by oxidation in hydrogen peroxide (80 °C) for 3 and 6 h. Moreover, a hydrothermal method (under oxygen gas) in autoclaves was investigated. Dry oxidation was performed under plasma and corona discharges, using different power values to elaborate optimum conditions. Selected samples were then (in preliminary experiments) subjected to a silanization of the surface with amino and glycidoxy organosilanes. The functionalized surfaces were examined by X-ray photon spectroscopy and Fourier transform infrared spectroscopy spectroscopy, and by scanning electron microscopy. The results of wet and dry oxidation methods indicated that the creation of functionalities was influenced by temperature, the concentration of the reagents (and gases) and the duration of the treatment. Sequential oxidation in aq. HNO₃ and H₂O₂ results in a higher content of oxygen functionalities at lower concentrations of oxidizing agents, when compared to oxidizing the carbon with concentrated nitric acid. Plasma oxidation results in non-permanent functionalization on the carbon surface, by which it´s necessary to find adequate parameters of oxidation treatments that could enable longer stability of functionalities. Results of the functionalization of the carbon surfaces with organosilanes will be presented as well.

Keywords: building materials, dry oxidation, organosilanes, pyrolytic carbon, resins, surface functionalization, wet oxidation

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Authors: P. Joshna, Souvik Kundu

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Detection of ultraviolet (UV) radiation is very important as it has exhibited a profound influence on humankind and other existences, including military equipment. In this work, a self-powered UV photodetector was reported based on oxides heterojunctions. The thin films of p-type nickel oxide (NiO) and n-type reduced graphene oxide (rGO) were used for the formation of p-n heterojunction. Low-Cost and low-temperature chemical synthesis was utilized to prepare the oxides, and the spin coating technique was employed to deposit those onto indium doped tin oxide (ITO) coated glass substrates. The top electrode platinum was deposited utilizing physical vapor evaporation technique. NiO offers strong UV absorption with high hole mobility, and rGO prevents the recombination rate by separating electrons out from the photogenerated carriers. Several structural characterizations such as x-ray diffraction, atomic force microscope, scanning electron microscope were used to study the materials crystallinity, microstructures, and surface roughness. On one side, the oxides were found to be polycrystalline in nature, and no secondary phases were present. On the other side, surface roughness was found to be low with no pit holes, which depicts the formation of high-quality oxides thin films. Whereas, x-ray photoelectron spectroscopy was employed to study the chemical compositions and oxidation structures. The electrical characterizations such as current-voltage and current response were also performed on the device to determine the responsivity, detectivity, and external quantum efficiency under dark and UV illumination. This p-n heterojunction device offered faster photoresponse and high on-off ratio under 365 nm UV light illumination of zero bias. The device based on the proposed architecture shows the efficacy of the oxides heterojunction for efficient UV photodetection under zero bias, which opens up a new path towards the development of self-powered photodetector for environment and health monitoring sector.

Keywords: chemical synthesis, oxides, photodetectors, spin coating

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Authors: Ogundele Lasun Tunde, Ayeku Oluwagbemiga Patrick

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Heavy metals are released into the sediments in aquatic environment from both natural and anthropogenic sources and they are considered as worldwide issue due to their deleterious ecological risks and food chain disruption. In this study, sediments samples were collected at three major sites (Awoye, Abereke and Ayetoro) along Ondo coastal area using VanVeen grab sampler. The concentrations of As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, V and Zn were determined by employing Atomic Absorption Spectroscopy (AAS). The combined concentrations data were subjected to Positive Matrix Factorization (PMF) receptor approach for source identification and apportionment. The probable risks that might be posed by heavy metals in the sediment were estimated by potential and integrated ecological risks indices. Among the measured heavy metals, Fe had the average concentrations of 20.38 ± 2.86, 23.56 ± 4.16 and 25.32 ± 4.83 lg/g at Abereke, Awoye and Ayetoro sites, respectively. The PMF resulted in identification of four sources of heavy metals in the sediments. The resolved sources and their percentage contributions were oil exploration (39%), industrial waste/sludge (35%), detrital process (18%) and Mn-sources (8%). Oil exploration activities and industrial wastes are the major sources that contribute heavy metals into the coastal sediments. The major pollutants that posed ecological risks to the local aquatic ecosystem are As, Pb, Cr and Cd (40 B Ei ≤ 80) classifying the sites as moderate risk. The integrate risks values of Awoye, Abereke and Ayetoro are 231.2, 234.0 and 236.4, respectively suggesting that the study areas had a moderate ecological risk. The study showed the suitability of PMF receptor model for source identification of heavy metals in the sediments. Also, the intensive anthropogenic activities and natural sources could largely discharge heavy metals into the study area, which may increase the heavy metal contents of the sediments and further contribute to the associated ecological risk, thus affecting the local aquatic ecosystem.

Keywords: positive matrix factorization, sediments, heavy metals, sources, ecological risks

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Authors: Ghada Ben Hamad, Zohir Younsi, Hassane Naji, Noureddine Lebaz, Naoual Belouaggadia

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This study deals with a bifunctional micro-encapsulated phase change (MCP) material, capric-stearic acid/graphene oxide-TiO2, which has been successfully developed by in situ hydrolysis and polycondensation of tetrabutyl titanate and modification of graphene oxide (GO) on the TiO2 doped shell. The use of graphene and doped TiO2 is a promising approach to provide photocatalytic activity under visible light and improve the microcapsules physicochemical properties. The morphology and chemical structure of the resulting microcapsule samples were determined by using Fourier transform infrared (FT-IR) spectroscopy, scanning electronic microscope (SEM), and X-ray diffractometer (XRD) methods. The ultraviolet, visible spectrophotometer (UV–vis), the differential scanning calorimeter (DSC) and the thermogravimetric analyzer (TGA) were used to investigate the absorption of visible and ultraviolet (UV), the thermal properties, and thermal stabilities of the microcapsules. Note that, the visible light photocatalytic activity was assessed for the toluene and benzene gaseous removal in a suitable test room. The microcapsules exhibit an interesting spherical morphology and an average diameter of 15 to 25 μm. The addition of graphene can enhance the rigidity of the shell and improve the microcapsules thermal reliability. At the same time, the thermal analysis tests showed that the synthesized microcapsules had a high solar thermal energy-storage and better thermal stability. In addition, the capric-stearic acid microcapsules exhibited high solar photocatalytic activity with respect to atmospheric pollutants under natural sunlight. The fatty acid samples obtained with the GO/TiO2 shell showed great potential for applications of solar energy storage, solar photocatalytic degradation of air pollutants and buildings energy conservation.

Keywords: thermal energy storage, microencapsulation, titanium dioxide, photocatalysis, graphene oxide

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Authors: A. Burakowska, M. Piotrowski, M. Kubicki, H. Trzaskowska, R. Sosnowiec, B. Myslek-Laurikainen

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The most important source of atmospheric radioactivity are radionuclides generated as a result of the impact of primary and secondary cosmic radiation, with the nuclei of nitrogen oxygen and carbon in the upper troposphere and lower stratosphere. This creates about thirty radioisotopes of more than twenty elements. For organisms, the four of them are most important: ³H, ⁷Be, ²²Na, ¹⁴C. The natural radionuclides, which are present in Earth crust, also settle on dust and particles of water vapor. By this means, the derivatives of uranium and thorium, and long-life 40K get into the air. ¹³⁷Cs is the most widespread isotope, that is implemented by humans into the environment. To determine the concentration of radionuclides in the atmosphere, high volume air samplers were used, where the aerosol collection took place on a special filter fabric (Petrianov filter tissue FPP-15-1.5). In 2002 the high volume air sampler AZA-1000 was installed at the Polish Polar Observatory of the Polish Academy of Science in Hornsund, Spitsbergen (77°00’N, 15°33’E), designed to operate in all weather conditions of the cold polar region. Since 1991 (with short breaks) the ASS-500 air sampler has been working, which is located in Swider at the Kalinowski Geophysical Observatory of Geophysics Institute of the Polish Academy of Science (52°07’N, 21°15’E). The following results of radionuclides concentrations were obtained from both stations using gamma spectroscopy analysis: ⁷Be, ¹³⁷Cs, ¹³⁴Cs, ²¹⁰Pb, ⁴⁰K. For gamma spectroscopy analysis HPGe (High Purity Germanium) detector were used. These data were compared with each other. The preliminary results gave evidence that radioactivity measured in aerosols is not proportional to the amount of dust for both studied regions. Furthermore, the results indicate annual variability (seasonal fluctuations) as well as a decrease in the average activity of ⁷Be with increasing latitude. The content of ⁷Be in surface air also indicates the relationship with solar activity cycles.

Keywords: aerosols, air filters, atmospheric beryllium, environmental radionuclides, gamma spectroscopy, mid-latitude regions radionuclides, polar regions radionuclides, solar cycles

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Authors: Coline Bretz, Andrea Vaccaro, Dario Leumann

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The food, personal care, and cosmetic industries are seeing increased consumer demand for more sustainable and innovative ingredients. When developing new formulations incorporating such ingredients, stability is one of the first criteria that must be assessed, and it is thus of great importance to have a method that can detect instabilities early and quickly. Diffusing Wave Spectroscopy (DWS) is a light scattering technique that probes the motion,i.e., the mean square displacement (MSD), of colloids, such as nanoparticles in a suspension or droplets in emulsions. From the MSD, the rheological properties of the surrounding medium can be determined via the so-called microrheology approach. In the case of purely viscous media, it is also possible to obtain information about particle size. DWS can thus be used to monitor the size evolution of particles, droplets, or bubbles in aging dispersions, emulsions, or foams. In the context of early instability detection in emulsions, DWS offers considerable advantages, as the samples are measured in a contact-free manner, using only small quantities of samples loaded in a sealable cuvette. The sensitivity and rapidity of the technique are key to detecting and following the ageing of emulsions reliably. We present applications of DWS focused on the characterization of emulsions. In particular, we demonstrate the ability to record very subtle changes in the structural properties early on. We also discuss the various mechanisms at play in the destabilization of emulsions, such as coalescence or Ostwald ripening, and how to identify them through this technique.

Keywords: instrumentation, emulsions, stability, DWS

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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: M. Lehtihet, S. Rosado, C. Pradère, J. Leng

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Poly(3,4-ethylene dioxythiophene) polystyrene sulfonate (PEDOT: PSS), is a polymer mixture well-known for its semiconducting properties and is widely used in the coating industry for its visible transparency and high electronic conductivity (up to 4600 S/cm) as a transparent non-metallic electrode and in organic light-emitting diodes (OLED). It also possesses strong absorption properties in the Near Infra-Red (NIR) range (λ ranging between 900 nm to 2.5 µm). In the present work, we take advantage of this absorption to explore its potential use as a transparent light-to-heat converter. PEDOT: PSS aqueous dispersions are deposited onto a glass substrate using a blade-coating technique in order to produce uniform coatings with controlled thicknesses ranging in ≈ 400 nm to 2 µm. Blade-coating technique allows us good control of the deposit thickness and uniformity by the tuning of several experimental conditions (blade velocity, evaporation rate, temperature, etc…). This liquid coating technique is a well-known, non-expensive technique to realize thin film coatings on various substrates. For coatings on glass substrates destined to solar insulation applications, the ideal coating would be made of a material able to transmit all the visible range while reflecting the NIR range perfectly, but materials possessing similar properties still have unsatisfactory opacity in the visible too (for example, titanium dioxide nanoparticles). NIR absorbing thin films is a more realistic alternative for such an application. Under solar illumination, PEDOT: PSS thin films heat up due to absorption of NIR light and thus act as planar heaters while maintaining good transparency in the visible range. Whereas they screen some NIR radiation, they also generate heat which is then conducted into the substrate that re-emits this energy by thermal emission in every direction. In order to quantify the heating power of these coatings, a sample (coating on glass) is placed in a black enclosure and illuminated with a solar simulator, a lamp emitting a calibrated radiation very similar to the solar spectrum. The temperature of the rear face of the substrate is measured in real-time using thermocouples and a black-painted Peltier sensor measures the total entering flux (sum of transmitted and re-emitted fluxes). The heating power density of the thin films is estimated from a model of the thin film/glass substrate describing the system, and we estimate the Solar Heat Gain Coefficient (SHGC) to quantify the light-to-heat conversion efficiency of such systems. Eventually, the effect of additives such as dimethyl sulfoxide (DMSO) or optical scatterers (particles) on the performances are also studied, as the first one can alter the IR absorption properties of PEDOT: PSS drastically and the second one can increase the apparent optical path of light within the thin film material.

Keywords: PEDOT: PSS, blade-coating, heat, thin-film, Solar spectrum

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Authors: Rhea Patel, Madhuri Vinchurkar, Rajul Patkar, Gopal Pranjale, Maryam Shojaei Baghini

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One of the major limitations on food resources worldwide is the deterioration of plant products due to pathogenic infections. Early screening of plants for pathogenic infections can serve as a boon in the Agricultural sector. The standard microbiology techniques has not kept pace with the rapid enumeration and automated methods for bacteria detection. Electrochemical Impedance Spectroscopy (EIS) serves as a label free bio sensing technique to monitor pathogens in real time. The changes in the electrical impedance of a growing bacterial culture can be monitored to detect activity of microorganisms. In this study, we demonstrate development of a gold interdigitated electrode (gold IDE) based impedance biosensor to detect bacterial cells in real on-field crop samples. To calibrate our impedance measurement system, nutrient broth suspended Escherichia coli cells were used. We extended this calibrated protocol to identify the agricultural pathogens in real potato tuber samples. Distinct difference was seen in the impedance recorded for the healthy and infected potato samples. Our results support the potential application of this Impedance based biosensor in Agricultural pathogen detection.

Keywords: agriculture, biosensor, electrochemical impedance spectroscopy, microelectrode, pathogen detection

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Authors: Eman Alzahrani

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Magnetic nanoparticles (MNPs) were fabricated using the chemical co-precipitation method followed by coating the surface of magnetic Fe3O4 nanoparticles with gum arabic (GA). The fabricated magnetic nanoparticles were characterised using transmission electron microscopy (TEM) which showed that the Fe3O4 nanoparticles and GA-MNPs nanoparticles had a mean diameter of 33 nm, and 38 nm, respectively. Scanning electron microscopy (SEM) images showed that the MNPs modified with GA had homogeneous structure and agglomerated. The energy dispersive X-ray spectroscopy (EDAX) spectrum showed strong peaks of Fe and O. X-ray diffraction patterns (XRD) indicated that the naked magnetic nanoparticles were pure Fe3O4 with a spinel structure and the covering of GA did not result in a phase change. The covering of GA on the magnetic nanoparticles was also studied by BET analysis, and Fourier transform infrared spectroscopy. Moreover, the present study reports a fast and simple method for removal and recovery of methylene blue dye (MB) from aqueous solutions by using the synthesised magnetic nanoparticles modified with gum arabic as adsorbent. The experimental results show that the adsorption process attains equilibrium within five minutes. The data fit the Langmuir isotherm equation and the maximum adsorption capacities were 8.77 mg mg-1 and 14.3 mg mg-1 for MNPs and GA-MNPs, respectively. The results indicated that the homemade magnetic nanoparticles were quite efficient for removing MB and will be a promising adsorbent for the removal of harmful dyes from waste-water.

Keywords: Fe3O4 magnetic nanoparticles, gum arabic, co-precipitation, adsorption dye, methylene blue, adsorption isotherm

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Authors: Maged Syed Ahamd, Manal Mohamed Yasser, Essam Sholkamy

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In this paper, we reported that selenium (Se) nanoparticles were firstly biosynthesized with a simple and eco-friendly biological method. Their shape, size, FTIR (Fourier Transform Infrared spectroscopy), UV–vis spectra, TEM (Transmission Electron Microscopy) images and EDS (Energy Dispersive Spectroscopy) pattern have been analyzed. TEM analyses of the samples obtained at different stages indicated that the formation of these Se nanostructures was governed by an incubation time (12- 24- 48 hours). The Se nanoparticles were initially generated and then would transform into crystal seeds for the subsequent growth of nanowires; however obtaining stable Se nanowire with a diameter of about 15-100 nm. EDS shows that Se nanoparticles are entirely pure. The IR spectra showed the peaks at 550 cm-1, 1635 cm-1, 1994 cm-1 and 3430 cm-1 correspond to the presence of Se-O bending and stretching vibrations. The concentrations of Se-NPs (0, 1, 2, 5 µg/ml) did not give significantly effect on both two cell lines while the highest concentrations (10- 100 µg/ml gave significantly effects on them. The lethal dose (ID50%) of Se-NPs on Hep2 G and MCF-7 cells was obtained at 75.96 and 61.86 µg/ml, respectively. Results showed that Se nanoparticles as anticancer agent against MCF-7 cells were more effective than Hep2 G cells. Our results suggest that Se-NPs may be a candidate for further evaluation as a chemotherapeutic agent for breast and liver cancers.

Keywords: selenium nanoparticle, Streptomyces bikiniensis, nanowires, chemotherapeutic agent

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Authors: Strahinja Kovačević, Lidija Jevrić, Miloš Kuzmanović, Sanja Podunavac-Kuzmanović

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In this paper, various derivatives of benzimidazole have been evaluated against Gram-negative bacteria Escherichia coli. For all investigated compounds the minimum inhibitory concentration (MIC) was determined. Quantitative structure-activity relationships (QSAR) attempts to find consistent relationships between the variations in the values of molecular properties and the biological activity for a series of compounds so that these rules can be used to evaluate new chemical entities. The correlation between MIC and some absorption, distribution, metabolism and excretion (ADME) parameters was investigated, and the mathematical models for predicting the antibacterial activity of this class of compounds were developed. The quality of the multiple linear regression (MLR) models was validated by the leave-one-out (LOO) technique, as well as by the calculation of the statistical parameters for the developed models and the results are discussed on the basis of the statistical data. The results of this study indicate that ADME parameters have a significant effect on the antibacterial activity of this class of compounds. Principal component analysis (PCA) and agglomerative hierarchical clustering algorithms (HCA) confirmed that the investigated molecules can be classified into groups on the basis of the ADME parameters: Madin-Darby Canine Kidney cell permeability (MDCK), Plasma protein binding (PPB%), human intestinal absorption (HIA%) and human colon carcinoma cell permeability (Caco-2).

Keywords: benzimidazoles, QSAR, ADME, in silico

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Authors: Hagen Stosnach

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The analytical demands on modern instruments for element analysis in food samples include the analysis of major, trace and ultra-trace essential elements as well as potentially toxic trace elements. In this study total reflection, X-ray fluorescence analysis (TXRF) is presented as an analytical technique, which meets the requirements, defined by the Association of Official Agricultural Chemists (AOAC) regarding the limit of quantification, repeatability, reproducibility and recovery for most of the target elements. The advantages of TXRF are the small sample mass required, the broad linear range from µg/kg up to wt.-% values, no consumption of gases or cooling water, and the flexible and easy sample preparation. Liquid samples like alcoholic or non-alcoholic beverages can be analyzed without any preparation. For solid food samples, the most common sample pre-treatment methods are mineralization, direct deposition of the sample onto the reflector without/with minimal treatment, mainly as solid suspensions or after extraction. The main disadvantages are due to the possible peaks overlapping, which may lower the accuracy of quantitative analysis and the limit in the element identification. This analytical technique will be presented by several application examples, covering a broad range of liquid and solid food types.

Keywords: essential elements, toxic metals, XRF, spectroscopy

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Authors: Uchenna Sydney Mbamara, Bolu Olofinjana, Ezekiel Oladele B. Ajayi

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Elaborate surface metrology of undoped ZnO thin films, deposited by organometallic chemical vapour deposition (OMCVD) technique at different precursor flow rates, was carried out. Dicarbomethyl-zinc precursor was used. The films were deposited on AISI304L steel and soda-lime glass substrates. Ultraviolet-visible-near-infrared (UV-Vis-NIR) spectroscopy showed that all the thin films were over 80% transparent, with an average bandgap of 3.39 eV, X-ray diffraction (XRD) results showed that the thin films were crystalline with a hexagonal structure, while Rutherford backscattering spectroscopy (RBS) results identified the elements present in each thin film as zinc and oxygen in the ratio of 1:1. Microscope and contactless profilometer results gave images with characteristic colours. The profilometer also gave the surface roughness data in both 2D and 3D. The asperity distribution of the thin film surfaces was Gaussian, while the average fractal dimension Da was in the range of 2.5 ≤ Da. The metrology proved the surfaces good for ‘touch electronics’ and coating mechanical parts for low friction.

Keywords: undoped ZnO, precursor flow rate, OMCVD, thin films, surface texture, tribology

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Authors: Sayed M. Ahmed, Sawsan S. Darwish, Mahmoud A. Adam, Nagib A. Elmarzugi, Mohammad A. Al-Dosari, Nadia A. Al-Mouallimi

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Historical stone surfaces and architectural heritage especially which located in open areas may undergo unwanted changes due to the exposure to many physical and chemical deterioration factors, air pollution, soluble salts, Rh/temperature, and biodeterioration are the main causes of decay of stone building materials. The development and application of self-cleaning treatments on historical and architectural stone surfaces could be a significant improvement in conservation, protection, and maintenance of cultural heritage. In this paper, nanometric titanium dioxide has become a promising photocatalytic material owing to its ability to catalyze the complete degradation of many organic contaminants and represent an appealing way to create self-cleaning surfaces, thus limiting maintenance costs, and to promote the degradation of polluting agents. The obtained nano-TiO2 coatings were applied on travertine (Marble and limestone often used in historical and monumental buildings). The efficacy of the treatments has been evaluated after coating and artificial thermal aging, through capillary water absorption, Ultraviolet-light exposure to evaluate photo-induced and the hydrophobic effects of the coated surface, while the surface morphology before and after treatment was examined by scanning electron microscopy (SEM). The changes of molecular structure occurring in treated samples were spectroscopy studied by FTIR-ATR, and Colorimetric measurements have been performed to evaluate the optical appearance. All the results get together with the apparent effect that coated TiO2 nanoparticles is an innovative method, which enhanced the durability of stone surfaces toward UV aging, improved their resistance to relative humidity and temperature, self-cleaning photo-induced effects are well evident, and no alteration of the original features.

Keywords: architectural calcareous stone monuments, coating, photocatalysis TiO2, self-cleaning, thermal aging

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Authors: Hasan Yalcin, Tugba Dursun Capar

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Deep-fat frying causes desirable as well as undesirable changes in oil and potato, and changes the quality of the oil by hydrolysis, oxidation, and polymerization. The main objective of the present study was to investigate the pre-drying effects on the quality of both frying oil and potatoes. Prior to frying, potato slices (10 mm x10 mm x 30 mm) were air- dried at 60°C for 15, 30, 45, 60, 90, and 120 mins., respectively. Potato slices without the pre-drying treatment were considered as the control variable. Potato slices were fried in sunflower oil at 180°C for 5, 10, and 13 mins. The deep-frying experiments were repeated five times using the new potato slices in the same oil without oil replenishment. Samples of the fresh oil, together with those sampled at the end of successive frying operations (1th, 3th and 5th) were removed and analysed. Moisture content, colour and oil intake of the potato and colour, peroxide value (PV), free fatty acid (FFA), fatty acid composition and viscosity of the used oil were evaluated. The effect of frying time was also examined. Results show that pre-drying treatment had a significant effect on physicochemical properties and colour parameters of potato slices and frying oil. Pre-drying considerably decreased the oil absorption. The lowest oil absorption was found for the treatment that was pre-dried for 120, and fried for 5 min. The FFA levels decreased permanently for each pre-treatment throughout the frying period. All the pre-drying treatments had reached their maximum levels of FFA by the end of the frying procedures. The PV of the control and 60 min pre-dried sample decreased after the third frying. However, the PV of other samples increased constantly throughout the frying periods. Lastly, pre-drying did not affect the fatty acid composition of frying oil considerably when compared against previously unused oil.

Keywords: air-drying, deep-fat frying, moisture content oil uptake, quality

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Authors: Thilini Kananke

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Culinary herbs have long been considered as significant dietary sources of many potential health-promoting compounds. The present research focused on analysis of antimicrobial, antioxidant and physicochemical properties in selected four culinary herbs namely Murraya koenigii (Curry leaves), Pandanus amaryllifolius (Pandan leaves), Cymbopogon citrates (Lemon grass leaves), and Mentha Piperita (Minchi leaves) obtained from several market sites in Ratnapura District, Sri Lanka. The antimicrobial activity of ethanolic, chloroform and distilled water extracts of culinary herbs were evaluated against the strains of Staphylococcus aureus, Salmonella typhi and Shigella spp. Total phenolic content and the radical scavenging activity (using DPPH assay) of culinary herbs were determined. Four heavy metals (Cu, Cd, Pb and Fe) were analyzed in the selected culinary herbs using the atomic absorption spectroscopy (AAS). Proximate compositions of the selected herbs were analyzed using AOAC official methods. Antimicrobial activity of all selected culinary herbs showed relativity high inhibition zones against S. aureus. Pandan leaves showed the least antimicrobial activity against selected bacterial strains compared with other culinary herbs. Both the highest radical scavenging activity (lower IC50 value) and the total phenolic content (25.57 ±3.54µg GAE/100g) were reported in Mentha piperita extract. The highest concentrations of Cu, Fe and Cd were reported in Curry leaves (29.15 mg/kg), Lemon grass leaves (257.98 mg/kg) and Pandan leaves (6.05 mg/kg) respectively. The heavy metal contents detected in all culinary herbs were below the permitted limits set by WHO/FAO, except Cd. The highest moisture (85.00±0.00%) and fiber (10.66± 2.00%) contents were found in Pandan leaves, while the highest protein (8.94±0.29%), fat (12.3± 2.52%) and ash (3.50± 0.17%) contents were reported in curry leaves. The information obtained from this study highlights the importance of further investigation of other antioxidant, antimicrobial and health promoting compounds of culinary herbs available in Sri Lanka for a detailed comparison.

Keywords: antimicrobial, antioxidant, culinary herbs, proximate analysis

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Authors: SeyedMohammad Hosseini, Amirhossein Moghanian

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The main purpose of this research was to design a biomimetic system by freeze-drying method for evaluating the effect of adding 5 and 10 mol. % of zinc (Zn)in 58S bioactive glass and gelatin (5ZnBG/G and 10ZnBG/G) in terms of structural and biological changes. The structural analyses of samples were performed by X-Ray Diffraction (XRD), scanning electron microscopy (SEM), and Fourier-transform infrared spectroscopy (FTIR). Also, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazoliumbromide(MTT) and alkaline phosphate (ALP) activity test were carried out for investigation of MC3T3-E1cell behaviors. The SEM results demonstrated the spherical shape of the formed hydroxyapatite (HA) phases, and also HA characteristic peaks were detected by X-ray diffraction spectroscopy (XRD)after 3 days of immersion in the simulated body fluid (SBF) solution. Meanwhile, FTIR spectra proved that the intensity of P–O peaks for 5ZnBG/G was more than 10ZnBG/G and control samples. Moreover, the results of alkaline phosphatase activity (ALP) test illustrated that the optimal amount of Zn (5ZnBG/G) caused a considerable enhancement in bone cell growth. Taken together, the scaffold with 5 mol.% Zn was introduced as an optimal sample because of its higher biocompatibility, in vitro bioactivity, and growth of MC3T3-E1cellsin in comparison with other samples in bone tissue engineering.

Keywords: scaffold, gelatin, modified bioactive glass, alp, bone tissue engineering

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Authors: Vishal Kumar, Soumitra Satapathi

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Föster Resonance Energy Transfer (FRET) is a powerful technique used to probe close-range molecular interactions. Physically, the FRET phenomenon manifests as a dipole–dipole interaction between closely juxtaposed fluorescent molecules (10–100 Å). Our effort is to employ this FRET technique to make a prototype device for highly sensitive detection of environment pollutant. Among the most common environmental pollutants, nitroaromatic compounds (NACs) are of particular interest because of their durability and toxicity. That’s why, sensitive and selective detection of small amounts of nitroaromatic explosives, in particular, 2,4,6-trinitrophenol (TNP), 2,4-dinitrotoluene (DNT) and 2,4,6-trinitrotoluene (TNT) has been a critical challenge due to the increasing threat of explosive-based terrorism and the need of environmental monitoring of drinking and waste water. In addition, the excessive utilization of TNP in several other areas such as burn ointment, pesticides, glass and the leather industry resulted in environmental accumulation, and is eventually contaminating the soil and aquatic systems. To the date, high number of elegant methods, including fluorimetry, gas chromatography, mass, ion-mobility and Raman spectrometry have been successfully applied for explosive detection. Among these efforts, fluorescence-quenching methods based on the mechanism of FRET show good assembly flexibility, high selectivity and sensitivity. Here, we report a FRET-based sensor system for the highly selective detection of NACs, such as TNP, DNT and TNT. The sensor system is composed of a copolymer Poly [(N,N-dimethylacrylamide)-co-(Boc-Trp-EMA)] (RP) bearing tryptophan derivative in the side chain as donor and dansyl tagged copolymer P(MMA-co-Dansyl-Ala-HEMA) (DCP) as an acceptor. Initially, the inherent fluorescence of RP copolymer is quenched by non-radiative energy transfer to DCP which only happens once the two molecules are within Förster critical distance (R0). The excellent spectral overlap (Jλ= 6.08×10¹⁴ nm⁴M⁻¹cm⁻¹) between donors’ (RP) emission profile and acceptors’ (DCP) absorption profile makes them an exciting and efficient FRET pair i.e. further confirmed by the high rate of energy transfer from RP to DCP i.e. 0.87 ns⁻¹ and lifetime measurement by time correlated single photon counting (TCSPC) to validate the 64% FRET efficiency. This FRET pair exhibited a specific fluorescence response to NACs such as DNT, TNT and TNP with 5.4, 2.3 and 0.4 µM LODs, respectively. The detection of NACs occurs with high sensitivity by photoluminescence quenching of FRET signal induced by photo-induced electron transfer (PET) from electron-rich FRET pair to electron-deficient NAC molecules. The estimated stern-volmer constant (KSV) values for DNT, TNT and TNP are 6.9 × 10³, 7.0 × 10³ and 1.6 × 104 M⁻¹, respectively. The mechanistic details of molecular interactions are established by time-resolved fluorescence, steady-state fluorescence and absorption spectroscopy confirmed that the sensing process is of mixed type, i.e. both dynamic and static quenching as lifetime of FRET system (0.73 ns) is reduced to 0.55, 0.57 and 0.61 ns DNT, TNT and TNP, respectively. In summary, the simplicity and sensitivity of this novel FRET sensor opens up the possibility of designing optical sensor of various NACs in one single platform for developing multimodal sensor for environmental monitoring and future field based study.

Keywords: FRET, nitroaromatic, stern-Volmer constant, tryptophan and dansyl tagged copolymer

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Authors: Sharmin Akhter, M. Salahuddin, Sukalyan Kumar Kundu, Mohammad Fahim Kadir

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Relatively insoluble candidate drug like carbamazepine (CBZ) often exhibit incomplete or erratic absorption; and hence wide consideration is given to improve aqueous solubility of such compound. Solid dispersions were formulated with an aim of improving aqueous solubility, oral bioavailability and the rate of dissolution of Carbamazepine using different hydrophyllic polymer like Polyethylene Glycol (PEG) 6000, Polyethylene Glycol (PEG) 4000, kollidon 30, HPMC 6 cps, poloxamer 407 and povidone k 30. Solid dispersions were prepared with different drug to polymer weight ratio by the solvent evaporation method where methanol was used as solvent. Drug-polymer physical mixtures were also prepared to compare the rate of dissolution. Effects of different polymer were studied for solid dispersion formulation as well as physical mixtures. These formulations were characterized in the solid state by Fourier Transform Infrared (FTIR) spectroscopy and Scanning Electron Microscopy (SEM). Solid state characterization indicated CBZ was present as fine particles and entrapped in carrier matrix of PEG 6000 and PVP K30 solid dispersions. Fourier Transform Infrared (FTIR) spectroscopic studies showed the stability of CBZ and absence of well-defined drug-polymer interactions. In contrast to the very slow dissolution rate of pure CBZ, dispersions of drug in polymers considerably improved the dissolution rate. This can be attributed to increased wettability and dispersibility, as well as decreased crystallinity and increase in amorphous fraction of drug. Solid dispersion formulations containing PEG 6000 and Povidone K 30 showed maximum drug release within one hour at the ratio of 1:1:1. Even physical mixtures of CBZ prepared with both carriers also showed better dissolution profiles than those of pure CBZ. In conclusions, solid dispersions could be a promising delivery of CBZ with improved oral bioavailability and immediate release profiles.

Keywords: carbamazepine, FTIR, kollidon 30, HPMC 6 CPS, PEG 6000, PEG 4000, poloxamer 407, water solubility, povidone k 30, SEM, solid dispersion

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Authors: Rashad Al-Gaashani

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The physicochemical activation method was used to produce high-quality activated carbon (AC) with a large surface area of about 2000 m2/g from low-cost and abundant biomass wastes in Qatar, namely date seeds. X-Ray diffraction (XRD), scanning electron spectroscopy (SEM), energy dispersive X-Ray spectroscopy (EDS), and Brunauer-Emmett-Teller (BET) surface area analysis was used to evaluate the AC samples. AC produced from date seeds has a wide range of pores available, including micro- and nano-pores. This type of AC with a well-developed pore structure may be very attractive for different applications, including air and water purification from micro and nano pollutants. Heavy metals iron (III) and copper (II) ions were removed from wastewater using the AC produced using a batch adsorption technique. The AC produced from date seeds biomass wastes shows high removal of heavy metals such as iron (III) ions (100%) and copper (II) ions (97.25%). The highest removal of copper (II) ions (100%) with AC produced from date seeds was found at pH 8, whereas the lowest removal (22.63%) occurred at pH 2. The effect of adsorption time, adsorbent dose, and pH on the removal of heavy metals was studied.

Keywords: activated carbon, date seeds, biomass, heavy metals removal, water treatment

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Authors: S. Girish, N. Ajay

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Permeation properties have been widely used to quantify durability characteristics of concrete for assessing long term performance and sustainability. The processes of deterioration in concrete are mediated largely by water. There is a strong interest in finding a better way of assessing the material properties of concrete in terms of durability. Water sorptivity is a useful single material property which can be one of the measures of durability useful in service life planning and prediction, especially in severe environmental conditions. This paper presents the results of the comparative study of sorptivity of Self-Compacting Concrete (SCC) with conventionally vibrated concrete. SCC is a new, special type of concrete mixture, characterized by high resistance to segregation that can flow through intricate geometrical configuration in the presence of reinforcement, under its own mass, without vibration and compaction. SCC mixes were developed for the paste contents of 0.38, 0.41 and 0.43 with fly ash as the filler for different cement contents ranging from 300 to 450 kg/m3. The study shows better performance by SCC in terms of capillary absorption. The sorptivity value decreased as the volume of paste increased. The use of higher paste content in SCC can make the concrete robust with better densification of the micro-structure, improving the durability and making the concrete more sustainable with improved long term performance. The sorptivity based on secondary absorption can be effectively used as a durability index to predict the time duration required for the ingress of water to penetrate the concrete, which has practical significance.

Keywords: self-compacting concrete, service life prediction, sorptivity, volume of paste

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Authors: Muhamad Azuddin Hassan, Siti Shafura Karim, Ambri Mohamed, Iskandar Yahya

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Human serum albumin plays a significant part in the physiological functions of the human body system (HSA).HSA level monitoring is critical for early detection of HSA-related illnesses. The goal of this study is to show that a field effect transistor (FET)-based immunosensor can assess HSA using high aspect ratio carbon nanotubes network (CNT) as a transducer. The CNT network were deposited using air brush technique, and the FET device was made using a shadow mask process. Field emission scanning electron microscopy and a current-voltage measurement system were used to examine the morphology and electrical properties of the CNT network, respectively. X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy were used to confirm the surface alteration of the CNT. The detection process is based on covalent binding interactions between an antibody and an HSA target, which resulted in a change in the manufactured biosensor's drain current (Id).In a linear range between 1 ng/ml and 10zg/ml, the biosensor has a high sensitivity of 0.826 mA (g/ml)-1 and a LOD value of 1.9zg/ml.HSA was also identified in a genuine serum despite interference from other biomolecules, demonstrating the CNT-FET immunosensor's ability to quantify HSA in a complex biological environment.

Keywords: carbon nanotubes network, biosensor, human serum albumin

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy

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Authors: H. Boucheloukh, S. Rouissa, N. Aoun, M. Beloucifa, T. Sehili, F. Parrino, V. Loddo

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To optimize water purification and wastewater treatment by heterogeneous photocatalysis, we used NiFe₂O₄ as a catalyst and solar irradiation as a source of energy. In this concept, an organic substance present in many industrial effluents was chosen: naproxen ((S)-6-methoxy-α-methyl-2-naphthaleneacetic acid or 2-(6-methoxynaphthalenyl) propanoic), a non-steroidal anti-inflammatory drug. The main objective of this study is to degrade naproxen by an iron and nickel catalyst, the degradation of this organic pollutant by nickel ferrite has been studied in a heterogeneous aqueous medium, with the study of the various factors influencing photocatalysis such as the concentration of matter and the acidity of the medium. The photocatalytic activity was followed by HPLC-UV andUV-Vis spectroscopy. A first-order kinetic model appropriately fitted the experimental data. The degradation of naproxen was also studied in the presence of H₂O₂ as well as in an aqueous solution. The new hetero-system NiFe₂O₄/oxalic acid is also discussed. The fastest naproxen degradation was obtained with NiFe₂O₄/H₂O₂. In a first-place, we detailed the characteristics of the material NiFe₂O₄, which was synthesized by the sol-gel methods, using various analytical techniques: visible UV spectrophotometry, X-ray diffraction, FTIR, cyclic voltammetry, luminescent discharge optical emission spectroscopy.

Keywords: naproxen, nickelate, photocatalysis, oxalic acid

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Authors: Mohsin Ejaz, Shiao-Wei Kuo

Abstract:

The growing production and exploitation of fossil fuels have placed human society in serious environmental issues. As a result, it's critical to design efficient and eco-friendly energy production and storage techniques. Porous organic polymers (POPs) are multi-dimensional porous network materials developed through the formation of covalent bonds between different organic building blocks that possess distinct geometries and topologies. POPs have tunable porosities and high surface area making them a good candidate for an effective electrode material in energy storage applications. Herein, we prepared a fully benzoxazine-based porous organic polymers (TPA–DHTP–BZ POP) through sonogashira coupling of dihydroxyterephthalaldehyde (DHPT) and triphenylamine (TPA) containing benzoxazine (BZ) monomers. Firstly, both BZ monomers (TPA-BZ-Br and DHTP-BZ-Ea) were synthesized by three steps, including Schiff base, reduction, and mannich condensation reaction. Finally, the TPA–DHTP–BZ POP was prepared through the sonogashira coupling reaction of brominated monomer (TPA-BZ-Br) and ethynyl monomer (DHTP-BZ-Ea). Fourier transform infrared (FTIR) and solid-state nuclear magnetic resonance (NMR) spectroscopy confirmed the successful synthesis of monomers as well as POP. The porosity of TPA–DHTP–BZ POP was investigated by the N₂ absorption technique and showed a Brunauer–Emmett–Teller (BET) surface area of 196 m² g−¹, pore size 2.13 nm and pore volume of 0.54 cm³ g−¹, respectively. The TPA–DHTP–BZ POP experienced thermal ring-opening polymerization, resulting in poly (TPA–DHTP–BZ) POP having strong inter and intramolecular hydrogen bonds formed by phenolic groups and Mannich bridges, thereby enhancing CO₂ capture and supercapacitive performance. The poly(TPA–DHTP–BZ) POP demonstrated a remarkable CO₂ capture of 3.28 mmol g−¹ and a specific capacitance of 67 F g−¹ at 0.5 A g−¹. Thus, poly(TPA–DHTP–BZ) POP could potentially be used for energy storage and CO₂ capture applications.

Keywords: porous organic polymer, benzoxazine, sonogashira coupling, CO₂, supercapacitor

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