Search results for: energy-dispersive X-ray spectroscopy

Authors: Khusboo Agrawal, S. Saraf

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Quercetin, a flavonol provides a cellular protection against UV induced oxidative damages due to its excellent free radical scavenging activity and direct pro-apoptopic effect on tumor cells. However, its topical use is limited due to its unfavorable physicochemical properties. The present study was aimed to evaluate the potential of mesoporous silica nanoparticles as topical carrier system for quercetin delivery. Complexes of quercetin with mesoporous silica was prepared with different weight ratios and characterized by thermo gravimetric analysis, X-ray diffraction, high resolution TEM, FT-IR spectroscopy, zeta potential measurements and differential scanning calorimetry The protective effect of this vehicle on UV-induced degradation of the quercetin was investigated revealing a certain positive influence of the inclusion on the photostability over time. Epidermal accumulation and transdermal permeation of this molecule were ex vivo evaluated by using Franz diffusion cells. The immobilization of Quercetin in mesoporous silica nanoparticles (MSNs) increased the stability without undermining the antioxidant efficacy.

Keywords: cancer, MSNs, quercetin, topical delivery

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Authors: Tian-Fang Kang, Chao-Nan Ge, Rui Li

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An electrochemical biosensor for the determination of organophosphorus pesticides was developed based on electrochemical co-deposition of Au and Pd nanoparticles on glassy carbon electrode (GCE). Energy disperse spectroscopy (EDS) analysis was used for characterization of the surface structure. Scanning electron micrograph (SEM) demonstrates that the films are uniform and the nanoclusters are homogeneously distributed on the GCE surface. Acetylcholinesterase (AChE) was immobilized on the Au and Pd nanoparticle modified electrode (Au-Pd/GCE) by cross-linking with glutaraldehyde. The electrochemical behavior of thiocholine at the biosensor (AChE/Au-Pd/GCE) was studied. The biosensors exhibited substantial electrocatalytic effect on the oxidation of thiocholine. The peak current of linear scan voltammetry (LSV) of thiocholine at the biosensor is proportional to the concentration of acetylthiocholine chloride (ATCl) over the range of 2.5 × 10-6 to 2.5 × 10-4 M in 0.1 M phosphate buffer solution (pH 7.0). The percent inhibition of acetylcholinesterase was proportional to the logarithm of parathion concentration in the range of 4.0 × 10-9 to 1.0 × 10-6 M. The detection limit of parathion was 2.6 × 10-9 M. The proposed method exhibited high sensitivity and good reproducibility.

Keywords: acetylcholinesterase, Au-Pd nanoparticles, electrochemical biosensors, parathion

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Authors: Z. Yousefniayejahr, S. Bolognini, A. Bonini, C. Campobasso, N. Poma, F. Vivaldi, M. Di Luca, A. Tavanti, F. Di Francesco

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Pathogenic bacteria represent a threat to healthcare systems and the food industry because their rapid detection remains challenging. Electrochemical biosensors are gaining prominence as a novel technology for the detection of pathogens due to intrinsic features such as low cost, rapid response time, and portability, which make them a valuable alternative to traditional methodologies. These sensors use biorecognition elements that are crucial for the identification of specific bacteria. In this context, bacteriophages are promising tools for their inherent high selectivity towards bacterial hosts, which is of fundamental importance when detecting bacterial pathogens in complex biological samples. In this study, we present the development of a low-cost and portable sensor based on the Zeno phage for the rapid detection of Staphylococcus aureus. Screen-printed gold electrodes functionalized with the Zeno phage were used, and electrochemical impedance spectroscopy was applied to evaluate the change of the charge transfer resistance (Rct) as a result of the interaction with S. aureus MRSA ATCC 43300. The phage-based biosensor showed a linear range from 101 to 104 CFU/mL with a 20-minute response time and a limit of detection (LOD) of 1.2 CFU/mL under physiological conditions. The biosensor’s ability to recognize various strains of staphylococci was also successfully demonstrated in the presence of clinical isolates collected from different geographic areas. Assays using S. epidermidis were also carried out to verify the species-specificity of the phage sensor. We only observed a remarkable change of the Rct in the presence of the target S. aureus bacteria, while no substantial binding to S. epidermidis occurred. This confirmed that the Zeno phage sensor only targets S. aureus species within the genus Staphylococcus. In addition, the biosensor's specificity with respect to other bacterial species, including gram-positive bacteria like Enterococcus faecium and the gram-negative bacterium Pseudomonas aeruginosa, was evaluated, and a non-significant impedimetric signal was observed. Notably, the biosensor successfully identified S. aureus bacterial cells in a complex matrix such as a nasal swab, opening the possibility of its use in a real-case scenario. We diluted different concentrations of S. aureus from 108 to 100 CFU/mL with a ratio of 1:10 in the nasal swap matrices collected from healthy donors. Three different sensors were applied to measure various concentrations of bacteria. Our sensor indicated high selectivity to detect S. aureus in biological matrices compared to time-consuming traditional methods, such as enzyme-linked immunosorbent assay (ELISA), polymerase chain reaction (PCR), and radioimmunoassay (RIA), etc. With the aim to study the possibility to use this biosensor to address the challenge associated to pathogen detection, ongoing research is focused on the assessment of the biosensor’s analytical performances in different biological samples and the discovery of new phage bioreceptors.

Keywords: electrochemical impedance spectroscopy, bacteriophage, biosensor, Staphylococcus aureus

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Authors: S. Gvazava, N. Khidasheli, V. Tediashvili, M. Donadze

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The work presented in this paper studied the of austempered ductile iron (ADI) with different combinations of structural composition (upper bainite, lower bainite, retained austenite) in rainwater. A range of structural states of the metal matrix was obtained by changing the regimes of thermal treantments of a high-strength cast iron. The specimens were austenised at 900 0C for 30, 60, 90, 120 minutes. Afterwards, isothermal quenching was performed at 280 and 400 0C for40 seconds. The study was carried out using weight-change (WC), cyclic potentiodynamic polarization (CPP), open-circuit potential (OCP), and electrochemical impedance spectroscopy (EIS) measurements and complemented by scanning electron microscopy (SEM-EDS). According to the results, corrosion resistance of the boron microallyedbainitic ADI greatly depends on the type of the bainitic matrix and the amount of the retained austenite, which is driven by diffusion permeability of interphase and intergrain boundaries.

Keywords: austempered ductile iron, corrosion behaviour, retained austenite, corrosion rate, interphase boundary, upper bainite, lower bainite

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Authors: Rami Al Jafar, Paul Elliott, Konstantinos K. Tsilidis, Abbas Dehghan

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Although Ramadan fasting is a ritual that is practiced every year by millions of Muslims, studies on Ramadan fasting are still scarce. To the best of our knowledge, none of the previous studies comprehensively explored the effect on the metabolic profile. In London Ramadan Fasting Study, blood samples were collected from 81 participants before and 10-14 days after Ramadan. Blood samples were analysed using nuclear magnetic resonance (NMR) spectroscopy which covers 249 metabolites. Mixed-effects models were used to analyse collected data and assess the effect of Ramadan fasting on the metabolic profile. Our observational study involved 85 individuals with a mean age of 45.2 years, and 53.1% of them were males. After Ramadan, forty metabolites were affected significantly by Ramadan fasting. Most of these metabolites were metabolites ratios (24), and the rest were three Glycolysis, three ketone bodies, nine Lipoprotein subclasses and one inflammation marker. This study suggests that Ramadan fasting is significantly associated with changes in the metabolic profile. However, the changes are assumed to be temporary, and the long-term effect of these changes is unknown.

Keywords: metabolic profile, Ramadan fasting, metabolites, intermittent fasting

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Authors: J. A. Sawicki, C. Ebrahimi

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The first geochemical, petrological, X-ray diffraction, Raman, Mössbauer, and oxygen isotopic analyses of very intriguing 13-kg Sooke #1 stone covered in 70% of its surface with black fusion crust, found in and recovered from Sooke Basin, near Juan de Fuca Strait, in British Columbia, were reported as poster #2775 at LPSC52 in March. Our further analyses reported in poster #6305 at 84AMMS in August and comparisons with the Mössbauer spectra of Martian meteorite MIL03346 and Martian rocks in Gusev Crater reported by Morris et al. suggest that Sooke #1 find could be a stony achondrite of Martian polymict breccia type ejected from early watery Mars. Here, the Raman spectra of a carbon-rich ~1-mm² fossil-like white area identified in this rock on a surface of polished cut have been examined in more detail. The low-intensity 532 nm and 633 nm beams of the InviaRenishaw microscope were used to avoid any destructive effects. The beam was focused through the microscope objective to a 2 m spot on a sample, and backscattered light collected through this objective was recorded with CCD detector. Raman spectra of dark areas outside fossil have shown bands of clinopyroxene at 320, 660, and 1020 cm-1 and small peaks of forsteritic olivine at 820-840 cm-1, in agreement with results of X-ray diffraction and Mössbauer analyses. Raman spectra of the white area showed the broad band D at ~1310 cm-1 consisting of main mode A1g at 1305 cm⁻¹, E2g mode at 1245 cm⁻¹, and E1g mode at 1355 cm⁻¹ due to stretching diamond-like sp3 bonds in diamond polytype lonsdaleite, as in Ovsyuk et al. study. The band near 1600 cm-1 mostly consists of D2 band at 1620 cm-1 and not of the narrower G band at 1583 cm⁻¹ due to E2g stretching in planar sp2 bonds that are fundamental building blocks of carbon allotropes graphite and graphene. In addition, the broad second-order Raman bands were observed with 532 nm beam at 2150, ~2340, ~2500, 2650, 2800, 2970, 3140, and ~3300 cm⁻¹ shifts. Second-order bands in diamond and other carbon structures are ascribed to the combinations of bands observed in the first-order region: here 2650 cm⁻¹ as 2D, 2970 cm⁻¹ as D+G, and 3140 cm⁻¹ as 2G ones. Nanodiamonds are abundant in the Universe, found in meteorites, interplanetary dust particles, comets, and carbon-rich stars. The diamonds in meteorites are presently intensely investigated using Raman spectroscopy. Such particles can be formed by CVD process and during major impact shocks at ~1000-2300 K and ~30-40 GPa. It cannot be excluded that the fossil discovered in Sooke #1 could be a remnant of an alien carbon organism that transformed under shock impact to nanodiamonds. We trust that for the benefit of research in astro-bio-geology of meteorites, asteroids, Martian rocks, and soil, this find deserves further, more thorough investigations. If possible, the Raman SHERLOCK spectrometer operating on the Perseverance Rover should also search for such objects in the Martian rocks.

Keywords: achondrite, nanodiamonds, lonsdaleite, raman spectra

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Authors: Abdelrahman Zkria, Tsuyoshi Yoshitake

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Diamond is one of the most interesting semiconducting carbon materials owing to its unique physical and chemical properties, yet its application in electronic devices is limited due to the difficulty of realizing n-type conduction by nitrogen doping. In contrast Ultrananocrystalline diamond with diamond grains of about 3–5 nm in diameter have attracted much attention for device-oriented applications because they may enable the realization of n-type doping with nitrogen. In this study, nitrogen-doped Ultra-Nanocrystalline diamond films were prepared by coaxial arc plasma deposition (CAPD) method, the nitrogen content was estimated by X-ray photoemission spectroscopy (XPS). The electrical conductivity increased with increasing nitrogen contents. Heterojunction diodes with p-type Si were fabricated and evaluated based on current–voltage (I–V) and capacitance–voltage (C–V) characteristics measured in dark at room temperature.

Keywords: heterojunction diodes, hopping conduction mechanism, nitrogen-doping, ultra-nanocrystalline diamond

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Authors: Albert Mufundirwa, Satoru Yoshioka, K. Ogi, Takeharu Sugiyama, George F. Harrington, Bretislav Smid, Benjamin Cunning, Kazunari Sasaki, Akari Hayashi, Stephen M. Lyth

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Polymer electrolyte membrane fuel cells (PEMFCs) are electrochemical energy conversion devices used for portable, residential and vehicular applications due to their low emissions, high efficiency, and quick start-up characteristics. However, PEMFCs generally use expensive, Pt-based electrocatalysts as electrode catalysts. Due to the high cost and limited availability of platinum, research and development to either drastically reduce platinum loading, or replace platinum with alternative catalysts is of paramount importance. A combination of high surface area supports and nano-structured active sites is essential for effective operation of catalysts. We synthesize carbon foam supports by thermal decomposition of sodium ethoxide, using a template-free, gram scale, cheap, and scalable pyrolysis method. This carbon foam has a high surface area, highly porous, three-dimensional framework which is ideal for electrochemical applications. These carbon foams can have surface area larger than 2500 m²/g, and electron microscopy reveals that they have micron-scale cells, separated by few-layer graphene-like carbon walls. We applied this carbon foam as a platinum catalyst support, resulting in the improved electrochemical surface area and mass activity for the oxygen reduction reaction (ORR), compared to carbon black. Similarly, silver-decorated carbon foams showed higher activity and efficiency for electrochemical carbon dioxide conversion than silver-decorated carbon black. A promising alternative to Pt-catalysts for the ORR is iron-impregnated nitrogen-doped carbon catalysts (Fe-N-C). Doping carbon with nitrogen alters the chemical structure and modulates the electronic properties, allowing a degree of control over the catalytic properties. We have adapted our synthesis method to produce nitrogen-doped carbon foams with large surface area, using triethanolamine as a nitrogen feedstock, in a novel bottom-up protocol. These foams are then infiltrated with iron acetate (FeAc) and pyrolysed to form Fe-N-C foams. The resulting Fe-N-C foam catalysts have high initial activity (half-wave potential of 0.68 VRHE), comparable to that of commercially available Pt-free catalysts (e.g., NPC-2000, Pajarito Powder) in acid solution. In alkaline solution, the Fe-N-C carbon foam catalysts have a half-wave potential of 0.89 VRHE, which is higher than that of NPC-2000 by almost 10 mVRHE, and far out-performing platinum. However, the durability is still a problem at present. The lessons learned from X-ray absorption spectroscopy (XAS), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and electrochemical measurements will be used to carefully design Fe-N-C catalysts for higher performance PEMFCs.

Keywords: carbon-foam, polymer electrolyte membrane fuel cells, platinum, Pt-free, Fe-N-C, ORR

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Authors: S. Totong, P. Daorattanachai, N. Laosiripojana

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Lignin depolymerization into phenolic-based chemicals is an interesting process for utilizing and upgrading a benefit and value of lignin. In this study, the depolymerization reaction was performed to convert alkaline lignin into smaller molecule compounds. Fumed SiO₂ was used as a catalyst to improve catalytic activity in lignin decomposition. The important parameters in depolymerization process (i.e., reaction temperature, reaction time, etc.) were also investigated. In addition, gas chromatography with mass spectrometry (GC-MS), flame-ironized detector (GC-FID), and Fourier transform infrared spectroscopy (FT-IR) were used to analyze and characterize the lignin products. It was found that fumed SiO₂ catalyst led the good catalytic activity in lignin depolymerization. The main products from catalytic depolymerization were guaiacol, syringol, vanillin, and phenols. Additionally, metal supported on fumed SiO₂ such as Cu/SiO₂ and Ni/SiO₂ increased the catalyst activity in terms of phenolic products yield.

Keywords: alkaline lignin, catalytic, depolymerization, fumed SiO₂, phenolic-based chemicals

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Authors: N. Perini, M. C. Thaller, F. Mercuri, S. Orlanducci, A. Rubechini, L. Migliore

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The preservation of cultural heritage is one of the major challenges of today’s society, because of the fundamental right of future generations to inherit it as the continuity with their historical and cultural identity. Parchments, consisting of a semi-solid matrix of collagen produced from animal skin (i.e., sheep or goats), are a significant part of the cultural heritage, being used as writing material for many centuries. Due to their animal origin, parchments easily undergo biodeterioration. The most common biological damage is characterized by isolated or coalescent purple spots that often leads to the detachment of the superficial layer and the loss of the written historical content of the document. Although many parchments with the same biodegradative features were analyzed, no common causative agent has been found so far. Very recently, a study was performed on a purple-damaged parchment roll dated back 1244 A.D, the A.A. Arm. I-XVIII 3328, belonging to the oldest collection of the Vatican Secret Archive (Fondo 'Archivum Arcis'), by comparing uncolored undamaged and purple damaged areas of the same document. As a whole, the study gave interesting results to hypothesize a model of biodeterioration, consisting of a microbial succession acting in two main phases: the first one, common to all the damaged parchments, is characterized by halophilic and halotolerant bacteria fostered by the salty environment within the parchment maybe induced by bringing of the hides; the second one, changing with the individual history of each parchment, determines the identity of its colonizers. The design of this model was pivotal to this study, performed by different labs of the Tor Vergata University (Rome, Italy), in collaboration with the Vatican Secret Archive. Three documents, belonging to a collection of dramatically damaged parchments archived as 'Faldone Patrizi A 19' (dated back XVII century A.D.), were analyzed through a multidisciplinary approach, including three updated technologies: (i) Next Generation Sequencing (NGS, Illumina) to describe the microbial communities colonizing the damaged and undamaged areas, (ii) RAMAN spectroscopy to analyze the purple pigments, (iii) Light Transmitted Analysis (LTA) to evaluate the kind and entity of the damage to native collagen. The metagenomic analysis obtained from NGS revealed DNA sequences belonging to Halobacterium salinarum mainly in the undamaged areas. RAMAN spectroscopy detected pigments within the purple spots, mainly bacteriorhodopsine/rhodopsin-like pigments, a purple transmembrane protein containing retinal and present in Halobacteria. The LTA technique revealed extremely damaged collagen structures in both damaged and undamaged areas of the parchments. In the light of these data, the study represents a first confirmation of the microbial succession model described above. The demonstration of this model is pivotal to start any possible new restoration strategy to bring back historical parchments to their original beauty, but also to open opportunities for intervention on a huge amount of documents.

Keywords: biodeterioration, parchments, purple spots, ecological succession

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Authors: Muhammad Tariq, Muhammad Waseem, Muhammad Hidayat Rasool

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Isolation and characterization of chromium tolerant Staphylococcus aureus from industrial wastewater and their potential use to bioremediate environmental chromium. Objectives: Chromium with its great economic importance in industrial use is major metal pollutant of the environment. Chromium are used in different industries for various applications such as textile, dyeing and pigmentation, wood preservation, manufacturing pulp and paper, chrome plating, steel and tanning. The release of untreated chromium in industrial effluents causes serious threat to environment and human health, therefore, the current study designed to isolate chromium tolerant Staphylococcus aureus for removal of chromium prior to their final discharge into the environment due to its cost effective and beneficial advantage over physical and chemical methods. Methods: Wastewater samples were collected from discharge point of different industries. Heavy metal analysis by atomic absorption spectrophotometer and microbiological analysis such as total viable count, total coliform, fecal coliform and Escherichia coli were conducted. Staphylococcus aureus was identified through gram’s staining, biomeriux vitek 2 microbial identification system and 16S rRNA gene amplification by polymerase chain reaction. Optimum growth conditions with respect to temperature, pH, salt concentrations and effect of chromium on the growth of bacteria, resistance to other heavy metal ions, minimum inhibitory concentration and chromium uptake ability of Staphylococcus aureus strain K1 was determined by spectrophotometer. Antibiotic sensitivity pattern was also determined by disc diffusion method. Furthermore, chromium uptake ability was confirmed by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscope equipped with Oxford Energy Dipersive X-ray (EDX) micro analysis system. Results: The results presented that optimum temperature was 35ᵒC, pH was 8.0 and salt concentration was 0.5% for growth of Staphylococcus aureus K1. The maximum uptake ability of chromium by bacteria was 20mM than other heavy metal ions. The antibiotic sensitivity pattern revealed that Staphylococcus aureus was vancomycin and methicillin sensitive. Non hemolytic activity on blood agar and negative coagulase reaction showed that it was non-pathogenic. Furthermore, the growth of bacteria decreases in the presence of chromium and maximum chromium uptake by bacteria observed at optimum growth conditions. Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and Energy dispersive X-ray (EDX) analysis confirmed the presence of chromium uptake by Staphylococcus aureus K1. Conclusion: The study revealed that Staphylococcus aureus K1 have the potential to bio-remediate chromium toxicity from wastewater. Gradually, this biological treatment becomes more important due to its advantage over physical and chemical methods to protect environment and human health.

Keywords: wastewater, staphylococcus, chromium, bioremediation

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Authors: Dibyendu Adak, Saroj Mandal

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The fly ash based geopolymer concrete generally requires heat activation after casting, which has been considered as an important limitation for its practical application. Such limitation can be overcome by a modification in the process at the time of mixing of ingredients (fly and activator fluid) for geopolymer concrete so that curing can be made at ambient temperature. This process modified geopolymer concrete shows an appreciable improvement in structural performance compared to conventional heat cured geopolymer concrete and control cement concrete. The improved durability performance based on water absorption, sulphate test, and RCPT is also noted. The microstructural properties analyzed through Field Emission Scanning Electron Microscope (FESEM) with Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD) techniques show the better interaction of fly ash and activator solution at early ages for the process modified geopolymer concrete. This accelerates the transformation of the amorphous phase of fly ash to the crystalline phase.

Keywords: fly ash, geopolymer concrete, process modification, structural properties, durability, micro-structures

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Authors: O. Çomaklı, M. Yazıcı, T. Yetim, A. F. Yetim, A. Çelik

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In this work, TiO₂ films were deposited on Cp-Ti substrates by thermal oxidation, DC plasma oxidation, and by the sol-gel method. Microstructures of uncoated and TiO₂ film coated samples were examined by X-ray diffraction and SEM. Thin oxide film consisting of anatase (A) and rutile (R) TiO₂ structures was observed on the surface of CP-Ti by under three different treatments. Also, the more intense anatase and rutile peaks appeared at samples plasma oxidized at 700˚C. The thicknesses of films were about 1.8 μm at the TiO₂ film coated samples by sol-gel and about 2.7 μm at thermal oxidated samples, while it was measured as 3.9 μm at the plasma oxidated samples. Electrochemical corrosion behaviour of uncoated and coated specimens was mainly carried out by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) in simulated body fluid (SBF) solution. Results showed that at the plasma oxidated samples exhibited a better resistance property to corrosion than that of other treatments.

Keywords: TiO₂, CP-Ti, corrosion properties, thermal oxidation, plasma oxidation, sol-gel

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Authors: Samar Aoujia, Théo Guérineaub, Rayan Zaitera, Evelyne Fargina, Younès Messaddeqb, Thierry Cardinala

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Two barium gallo-germanate glass series were elaborated to investigate the effect of the yttrium introduction on the glass physicochemical properties and crystallization behavior. One to twenty mol% of YO3/2 were either added into the glass matrix or substituted for gallium oxide. The glass structure was studied by Raman spectroscopy, and the thermal, optical, thermo-mechanical and physical properties are examined. The introduction of yttrium ions in both glass series increases the glass transition temperature, crystallization temperature, softening temperature, coefficient of linear thermal expansion and density. Through differential scanning calorimetry and X-ray diffraction analyses, it was found that competition occurs between the gallo-germanate zeolite-type phase and the yttrium-containing phase. From 13 mol% of YO3/2, the yttrium introduction impedes the formation of surface crystallization in these glasses.

Keywords: photonic, heavy-metal oxide, glass, crystallization

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Authors: Esther Lorrayne M. Pereira, Adriana S. M. Batista, Fabíola A. S. Ribeiro, Adelina P. Santos, Luiz O. Faria

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In this work we have prepared nanocomposites made by mixing Poli (vinilidene fluoride) (PVDF), zirconium oxide (ZrO₂) and multi–walled carbon nanotubes (MWCNTs) aiming to find dosimetric properties for applications in high dose dosimetry. The samples were irradiated with a Co-60 source at constant dose rate (16.7 kGy/h), with doses ranging from 100 to 2750 kGy. The UV-Vis and FTIR spectrophotometry have been used to monitor the appearing of C=C conjugated bonds and radio-oxidation of carbon (C=O). FTIR spectrometry has that the absorbance intensities at 1715 cm⁻¹ and 1730 cm⁻¹ can be used for high dosimetry purposes for gamma doses ranging from 500 to 2750 kGy. In this range, it is possible to observe a linear relationship between Abs & Dose. Fading of signal was evaluated for one month and reproducibility in 2000 kGy dose. Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) was used for evaluated the dispersion ZrO₂ and MWCNT in the matrix of the PVDF.

Keywords: polymer, composite, high dose dosimetry, PVDF/ZrO₂/MWCNT

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Authors: Burcu Kiren, Alattin CAkan, Nezihe Ayas

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Hydrogen will be arguably the best fuel in the future as it is the most abundant element in the universe. Hydrogen, as a fuel, is notably environmentally benign, sustainable and has high energy content compared to other sources of energy. It can be generated from both conventional and renewable sources. The hydrolysis reaction of metal hydrides provides an option for hydrogen production in the presence of a catalyst. In this study, Ni/dolomite catalyst was synthesized by the wet impregnation method for hydrogen production by hydrolysis reaction of sodium borohydride (NaBH4). Besides, the synthesized catalysts characterizations were examined by means of thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer –Emmett – Teller (BET) and scanning electron microscopy (SEM). The influence of reaction temperature (25-75 °C), reaction time (15-60 min.), amount of catalyst (50-250 mg) and active metal loading ratio (20,30,40 wt.%) were investigated. The catalyst prepared with 30 wt.% Ni was noted as the most suitable catalyst, achieving of 35.18% H₂ and hydrogen production rate of 19.23 mL/gcat.min at 25 °C at reaction conditions of 5 mL of 0.25 M NaOH and 100 mg NaBH₄, 100 mg Ni/dolomite.

Keywords: sodium borohydride, hydrolysis, catalyst, Ni/dolomite, hydrogen

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Authors: Ayodele Odularu, Peter Ajibade, Albert Bolhuis

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This study aimed at assessing the antibacterial activities of four zinc (II) complexes. Zinc (II) complexes of nitrogen, oxygen and sulfur coordination modes were synthesized using direct substitution reaction. The characterization techniques involved physicochemical properties (molar conductivity) and spectroscopic techniques. The molar conductivity gave the non-electrolytic nature of zinc (II) complexes. The spectral studies of zinc (II) complexes were done using electronic spectra (UV-Vis) and Fourier Transform Infra-red Spectroscopy (FT-IR). Spectral data from the spectroscopic studies confirmed the coordination of the mixed ligands with zinc (II) ion. The antibacterial activities of zinc(II) complexes of were all in supportive of Overtone’s concept and Tweedy’s theory of chelation for bacterial strains of S. aureus MRSA252 and E coli MC4100 because the zones of inhibition were greater than the corresponding ligands. In summary, all zinc (II) complexes of ZEPY, ZE1PH, ZE1PY and ZE135PY all have potentials for antibacterial activities.

Keywords: antibacterial activities, spectral studies, syntheses, zinc(II) complexes

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Authors: Manel Hannachi, Mustapha Nechiche, Said Azem

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This study focuses on biodegradable materials made from Poly-lactic acid (PLA) and vegetal reinforcements. Three materials are developed from PLA, as a matrix, and : (i) olive kernels (OK); (ii) alfa (α) short fibers and (iii) OK+ α mixture, as reinforcements. After processing of PLA pellets and olive kernels in powder and alfa stems in short fibers, three mixtures, namely PLA-OK, PLA-α, and PLA-OK-α are prepared and homogenized in Turbula®. These mixtures are then compacted at 180°C under 10 MPa during 15 mn. Scanning Electron Microscopy (SEM) examinations show that PLA matrix adheres at surface of all reinforcements and the dispersion of these ones in matrix is good. X-ray diffraction (XRD) analyses highlight an increase of PLA inter-reticular distances, especially for the PLA-OK case. These results are explained by the dissociation of some molecules derived from reinforcements followed by diffusion of the released atoms in the structure of PLA. This is consistent with Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) analysis results.

Keywords: alfa short fibers, biodegradable composite, olive kernels, poly-lactic acid

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Authors: M. S. M. Yusof, R. Ramli, S. K. C. Soh, N. Ismail, N. Ngah

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This study presents the synthesis of a series of methoxybenzoylthiourea amino acid derivatives. The compounds were obtained from the reactions between 2/3/4-methoxybenzoyl isothiocyanate with threonine. All of the compounds were characterized via mass spectrometry, ¹H and ¹³C NMR spectrometry, UV-Vis spectrophotometer and FT-IR spectroscopy. Mass spectra for all of the compounds showed the presence of molecular ion [M]⁺ peaks at m/z 312, which are in agreement to the calculated molecular weight. For ¹H NMR spectra, the presence of OCH₃, C=S-NH and C=O-NH protons were observed within range of δ_H 3.8-4.0 ppm, 11.1-11.5 ppm and 10.0-11.5 ppm, respectively. ¹³C NMR spectra in all compounds displayed the presence of OCH₃, C=O-NH, C=O-OH and C=S carbon resonances within range of δ_C 55.0-57.0 ppm, 165.0-168.0 ppm, 170.0-171.0 ppm and 180.0-182.0 ppm, respectively. In UV spectra, two absorption bands have been observed and both were assigned to the n-π* and π-π* transitions. Six vibrational modes of v(N-H), v(O-H), v(C=O-OH), v(C=O-NH), v(C=C) aromatic and v(C=S) appeared in the FT-IR spectra within the range of 3241-3467 cm^-1, 2976-3302 cm^-1, 1720-1768 cm^-1, 1655-1672 cm^-1, 1519-1525 cm^-1 and 754-763 cm^-1, respectively. The antibacterial activity for all of the compounds was screened against Staphylococcus aureus, Staphylococcus epidermidis, Salmonella typhimurium and Escherichia coli. However, no activity was observed.

Keywords: methoxybenzoyl isothiocyanate, amino acid, threonine, antibacterial

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Authors: R. Benakcha, M. Omari

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Powders of La1-xMgxAlO3 (0 ≤ x ≤ 5) oxides, with large surface areas were synthesized by sol-gel process, utilizing citric acid. Heating of a mixed solution of CA, EtOH, and nitrates of lanthanum, aluminium and magnesium at 70°C gave transparent gel without any precipitation. The formation of pure perovskite La1-xMgxAlO3, occurred when the precursor was heat-treated at 800°C for 6 h. No X-ray diffraction evidence for the presence of crystalline impurities was obtained. The La1-xMgxAlO3 powders prepared by the sol-gel method have a considerably large surface area in the range of 12.9–20 m^2.g^-1 when compared with 0.3 m^2.g^-1 for the conventional solid-state reaction of LaAlO3. The structural characteristics were examined by means of conventional techniques namely X-ray diffraction, infrared spectroscopy, thermogravimetry and differential thermal (TG-DTA) and specific surface SBET. Pore diameters and crystallite sizes are in the 8.8-11.28 nm and 25.4-30.5 nm ranges, respectively. The sol-gel method is a simple technique that has several advantages. In addition to that of not requiring high temperatures, it has the potential to synthesize many kinds of mixed oxides and obtain other materials homogeneous and large purities. It also allows formatting a variety of materials: very fine powders, fibers and films.

Keywords: aluminate, lanthan, perovskite, sol-gel

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Authors: Memet Vezir Kahraman, Ferhat Sen

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This study aimed to develop polyelectrolyte structured antimicrobial food packaging materials that do not contain any antimicrobial agents. Cationic hydroxyethyl cellulose was synthesized and characterized by Fourier Transform Infrared, carbon and proton Nuclear Magnetic Resonance spectroscopy. Its nitrogen content was determined by the Kjeldahl method. Polyelectrolyte structured antimicrobial food packaging materials were prepared using hydroxyethyl cellulose, cationic hydroxyethyl cellulose, and sodium alginate. Antimicrobial activity of materials was defined by inhibition zone method (disc diffusion method). Thermal stability of samples was evaluated by thermal gravimetric analysis and differential scanning calorimetry. Surface morphology of samples was investigated by scanning electron microscope. The obtained results prove that produced food packaging materials have good thermal and antimicrobial properties, and they can be used as food packaging material in many industries.

Keywords: antimicrobial food packaging, cationic hydroxyethyl cellulose, polyelectrolyte, sodium alginate

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Authors: Jafar Khan Kasi, Ajab Khan Kasi, Muzamil Bokhari

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Carbon nanotube is one of the most attractive materials for the potential applications of nanotechnology due to its excellent mechanical, thermal, electrical and optical properties. In this paper we report a supercapacitor made of nickel foil electrodes, coated with multiwall carbon nanotubes (MWCNTs) thin film using electrophoretic deposition (EPD) method. Chemical vapor deposition method was used for the growth of MWCNTs and ethanol was used as a hydrocarbon source. High graphitic multiwall carbon nanotube was found at 750 C analyzing by Raman spectroscopy. We observed the electrochemical performance of supercapacitor by cyclic voltammetry. The electrodes of supercapacitor fabricated from MWCNTs exhibit considerably small equivalent series resistance (ESR), and a high specific power density. Electrophoretic deposition is an easy method in fabricating MWCNT electrodes for high performance supercapacitor.

Keywords: carbon nanotube, chemical vapor deposition, catalyst, charge, cyclic voltammetry

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Authors: Roman J. Jedrzejczyk, Damian K. Chlebda, Anna Dziedzicka, Rafal Wazny, Agnieszka Domka, Maciej Sitarz, Przemyslaw J. Jodlowski

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The aim of this study was to obtain antimicrobial material based on thin zirconium dioxide coatings on structured reactors doped with metal nanoparticles using the sonochemical sol-gel method. As a result, dense, uniform zirconium dioxide films were obtained on the kanthal sheets which can be used as support materials in antimicrobial converters with sophisticated shapes. The material was characterised by physicochemical methods, such as AFM, SEM, EDX, XRF, XRD, XPS and in situ Raman and DRIFT spectroscopy. In terms of antimicrobial activity, the material was tested by ATP/AMP method using model microbes isolated from the real systems. The results show that the material can be potentially used in the market as a good candidate for active package and as active bulkheads of climatic systems. The mechanical tests showed that the developed method is an efficient way to obtain durable converters with high antimicrobial activity against fungi and bacteria.

Keywords: antimicrobial properties, kanthal steel, nanocomposite, zirconium oxide

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Authors: Hua Jin, Il Kim

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The biocompatible tadpole-shaped polypeptides with one cyclic polypeptides ring and two alkyl chain tails were synthesized by N-heterocyclic carbine (NHC)-mediated ring-opening polymerization (ROP) of α-amino acid N-carboxyanhydrides (NCAs). First, the NHC precursor, denoted as [NHC(H)][HCO₃], with two alkyl chains at the nitrogen was prepared by a simple anion metathesis of imidazole(in)ium chlorides with KHCO₃. Then NHC releasing from the [NHC(H)][HCO₃] directly initiated the ROP of NCA to produce the cyclic polypeptides. Finally, the tadpole-shaped polypeptides with two regulable tails were obtained. The target polypeptides were characterized by nuclear magnetic resonance spectrum (1H NMR), Fourier transform infrared spectroscopy (FT-IR), gel permeation chromatography (GPC) and matrix-assisted laser desorption ionization-time of flight mass spectra (MALDI-TOF MS). This pioneering approach simplifies the synthesis procedures of tadpole-shaped polypeptides compared to other methods, which usually requires specific intramolecular ring-closure reaction.

Keywords: cyclic polypeptides, α-amino acid N-carboxyanhydrides, N-heterocyclic carbene, ring-opening polymerization, tadpole-shaped

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Authors: Dina M. Abd El-Aty, D. Aman, E. G. Zaki, Heba M. Salem

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A friendly environmental source of energy as hydrogen was produced by photo-hydrolysis of hydrogen storage material as sodium borohydride (NaBH4), which is non-toxic and stores a high percentage of hydrogen. The photoreaction was produced under visible light and nano-alumina as a catalyst. In this study, we use more economical and friendly environmental oil as a template to produce a nano-catalyst. The prepared catalyst was characterized by X-Ray diffraction, N2-adsorption-desorption, Fourier Transforms Infrared, Scanning Electron microscope and X-Ray Photoelectron Spectroscopy. Different parameters such as catalyst weight, NaBH4 weight and time of irradiation were studied to obtain a highly efficient photo-hydrolysis reaction. The reaction is pseudo-first order and the hydrogen production rate was determined as 1500 ml min-1 g-1 at the optimum conditions.

Keywords: photo-reaction, nano-alumina, hydrogen production, sodium borohydride, visible light

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Authors: Ali N. Siyal, Saima Q. Memon, Latif Elçi, Aydan Elçi

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Polystyrene (PS) was extracted from Styrofoam (expanded polystyrene foam) waste, so called white pollutant. The PS was functionalized with N, N- Bis(2-aminobenzylidene)benzene-1,2-diamine (ABA) ligand through an azo spacer. The resin was characterized by FT-IR spectroscopy and elemental analysis. The PS-N=N-ABA resin was used for the enrichment and speciation of Cr(III)/Cr(VI) ions and total Cr determination in aqueous samples by Flame Atomic Absorption Spectrometry (FAAS). The separation of Cr(III)/Cr(VI) ions was achieved at pH 2. The recovery of Cr(VI) ions was achieved ≥ 95.0% at optimum parameters: pH 2; resin amount 300 mg; flow rates 2.0 mL min-1 of solution and 2.0 mL min-1 of eluent (2.0 mol L-1 HNO3). Total Cr was determined by oxidation of Cr(III) to Cr(VI) ions using H2O2. The limit of detection (LOD) and quantification (LOQ) of Cr(VI) were found to be 0.40 and 1.20 μg L-1, respectively with preconcentration factor of 250. Total saturation and breakthrough capacitates of the resin for Cr(IV) ions were found to be 0.181 and 0.531 mmol g-1, respectively. The proposed method was successfully applied for the preconcentration/speciation of Cr(III)/Cr(VI) ions and determination of total Cr in industrial effluents.

Keywords: styrofoam waste, polymeric resin, preconcentration, speciation, Cr(III)/Cr(VI) ions, FAAS

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Authors: S. M. AL-Shomar, N. B. Ibrahim, Sahrim Hj. Ahmad

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ZnO thin films with various Gd doping concentration (0, 0.01, 0.03 and 0.05 mol/L) have been synthesized by sol–gel method on quartz substrates at annealing temperature of 600 ºC. X-ray analysis reveals that ZnO(Gd) films have hexagonal wurtzite structure. No peaks that correspond to Gd metal clusters or gadolinium acetylacetonate are detected in the patterns. The position of the main peak (101) shifts to higher angles after doping. The surface morphologies studied using a field emission scanning electron microscope (FESEM) showed that the grain size and the films thickness reduced gradually with the increment of Gd concentration. The roughness of ZnO film investigated by an atomic force microscopy (AFM) showed that the films are smooth and high dense grain. The roughness of doped films decreased from 6.05 to 4.84 rms with the increment of dopant concentration.The optical measurements using a UV-Vis-NIR spectroscopy showed that the Gd doped ZnO thin films have high transmittance (above 80%) in the visible range and the optical band gap increase with doping concentration from 3.13 to 3.39 eV. The doped films show low electrical resistivity 2.6 × 10-3Ω.cm.at high doping concentration.

Keywords: Gd doped ZnO, electric, optics, microstructure

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Authors: Galina Mamardashvili, Nugzar Mamardashvili, Win Dehaen

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The processes of complexation of the Zn-tetraarylporphyrins with eight 4-(4-(3,6-bis(t-butyl)carbazol-9-yl-phenyl)-1,2,3-triazole (ZnP1) and eight 4-(4-(3,6-di-tert-butyl-9-H-carbazol-9-yl)phenoxy)methyl)-2,4,6-trimethylphenyl (ZnP2)with the 1,10-diaza-4,7,13,18tetraoxabicyclo[8.5.5]eicosane (L1),1,10-diaza-4,7,13,16,21,24-hexaoxabicyclo[8.8.8]hexacosane (L2)and 1,10-diaza-5,6,14,15-dibenzo-4,7,13,16,21,24 hexaoxabicyclo[8.8.8] hexacosane (L3) were investigated by the method of spectrophotometric titration and ¹H NMR-spectroscopy. We determined the structures of the host-guest complexes, and their stability constants in toluene were calculated. It was found out that the ZnP1 interacts with the guest molecules L1, L2 with the formation of stable "nest" type complexes and does not form similar complexes with the L3 (presumably due to the fact that the L3 does not match the size of the porphyrin ZnP(1) cavity). On the other hand, the porphyrin ZnP2 binds all of the ligands L1-L3, however complexes thus formed are less stable than complexes ZnP1-L1, ZnP1-L2. In the report, we will also discuss the influence of the alkali cations additives on the stability of the complexes between the porphyrin ZnP1, ZnP2 hosts and guest molecules of the ligands L1-L3.

Keywords: porphyrin, cryptand, cation, complex guest-host

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Authors: Rajinder Kaur, Atul Khanna

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Transparent glass-ceramic and crystalline samples of the system: xSrO-(100-x)TeO2; x = 7.5 and 8.5 mol% were prepared by quenching the melts in the temperature range of 700 to 950oC. A very interesting effect of the temperature on the glass-forming ability (GFA) of strontium tellurite melts is observed,and it is found that the melts produce transparent glass-ceramics when it is solidified from lower temperatures in the range of 700-750oC, however, when the melts are cooled from higher temperatures in the range of 850-950oC, the GFA is significantly reduced andanti-glass and/or crystalline phases are produced on solidification.The effect of temperature on GFA of strontium tellurite melts is attributed to short-range structural transformations: TeO₄TeO₃ which procceds towards the right side with an increrase in temperature. This isomerization reaction lowers the melt viscosity and enhances the crystallization tedendency. It is concluded that the high-temperature strontium tellurite meltsfreeze faster into crystalline phases as compared to the melts at a lower temperature; the latter supercooland solidify into glassy phases.

Keywords: anti-glasss, ceramic, supercool liquid, raman spectroscopy

Procedia PDF Downloads 83

Authors: Sunitha Sampathi, Pankaj Kumar Tiriya, Sonia Gera, Sravanthi Reddy Pailla, V. Likhitha, A. J. Maruthi

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Surgical site infections (SSIs) are the most common nosocomial infections localized at the incision site. With an estimated 27 million surgical procedures each year in USA, approximately 2-5% rate of SSIs are predicted to occur annually. SSIs are treated with antibiotic medication. Current trend suggest that the direct drug delivery from the suture to the scared tissue can improve patient comfort and wound recovery. For that reason coating the surface of the medical device such as suture and catguts with broad spectrum antibiotics can prevent the formation of bactierial colonies with out comprimising the mechanical properties of the sutures.Hence, the present study was aimed to develop and evaluate a surgical suture coated with an antibiotic Ciprofloxacin hydrochloride loaded on gold nanoparticles. Gold nanoparticles were synthesized by chemical reduction method and conjugated with ciprofloxacin using Polyvinylpyrolidone as stabilizer and gold as carrier. Ciprofloxacin conjugated gold nanoparticles were coated over an absorbable surgical suture made of Polyglactan using sodium alginate as an immobilising agent by slurry dipping technique. The average particle size and Polydispersity Index of drug conjugated gold NPs were found to be 129±2.35 nm and 0.243±0.36 respectively. Gold nanoparticles are characterized by UV-Vis absorption spectroscopy, Fourier Transform Infrared Spectroscopy (FT-IR), Scanning electron microscopy and Transmission electron microscopy. FT-IR revealed that there is no chemical interaction between drug and polymer. Antimicrobial activity for coated sutures was evaluated by disc diffusion method on culture plates of both gram negative (E-coli) and gram positive bacteria (Staphylococcus aureus) and results found to be satisfactory. In vivo studies for coated sutures was performed on Swiss albino mice and histological evaluation of intestinal wound healing parameters such as wound edges in mucosa, muscularis, presence of necrosis, exudates, granulation tissue, granulocytes, macrophages, restoration, and repair of mucosal epithelium and muscularis propria on day 7 after surgery were studied. The control animal group, sutured with plain suture (uncoated suture) showed signs of restoration and repair, but presence of necrosis, heamorraghic infiltration and granulation tissue was still noticed. Whereas the animal group treated with ciprofloxacin and ciprofloxacin gold nanoparticle coated sutures has shown promising decrease in terms of haemorraghic infiltration, granulation tissue, necrosis and better repaired muscularis layers on comparision with plain coated sutures indicating faster rate of repair and less chance of sepsis. Hence coating of sutures with broad spectrum antibiotics can be an alternate technique to reduce SSIs.

Keywords: ciprofloxacin hydrochloride, gold nanoparticles, surgical site infections, sutures

Procedia PDF Downloads 256