Search results for: electrochemical impedence spectroscopy

Authors: H. Bhuyan, S. Mändl, M. Favre, M. Cisternas, A. Henriquez, E. Wyndham, M. Walczak, D. Manova

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The 470 Li-24 Cr and 460Li-21 Cr are two alloys belonging to the next generation of super-ferritic nickel free stainless steel grades, containing titanium (Ti), niobium (Nb) and small percentage of carbon (C) and nitrogen (N). The addition of Ti and Nb improves in general the corrosion resistance while the low interstitial content of C and N assures finer precipitates and greater ductility compared to conventional ferritic grades. These grades are considered an economic alternative to AISI 316L and 304 due to comparable or superior corrosion. However, since 316L and 304 can be nitrided to improve the mechanical surface properties like hardness and wear; it is hypothesize that the tribological properties of these super-ferritic stainless steels grades can also be improved by plasma nitriding. Thus two sets of plasma immersion ion implantation experiments have been carried out, one with a high pressure capacitively coupled radio frequency plasma at PUC Chile and the other using a low pressure microwave plasma at IOM Leipzig, in order to explore further improvements in the mechanical properties of 470 Li-24 Cr and 460Li-21 Cr steel. Nitrided and unnitrided substrates have been subsequently investigated using different surface characterization techniques including secondary ion mass spectroscopy, scanning electron microscopy, energy dispersive x-ray analysis, Vickers hardness, wear resistance, as well as corrosion test. In most of the characterizations no major differences have been observed for nitrided 470 Li-24 Cr and 460Li-21 Cr. Due to the ion bombardment, an increase in the surface roughness is observed for higher treatment temperature, independent of the steel types. The formation of chromium nitride compound takes place only at a treatment temperature around 4000C-4500C, or above. However, corrosion properties deteriorate after treatment at higher temperatures. The physical characterization results show up to 25 at.% of nitrogen for a diffusion zone of 4-6 m, and a 4-5 times increase in hardness for different experimental conditions. The samples implanted with temperature higher than 400 °C presented a wear resistance around two orders of magnitude higher than the untreated substrates. The hardness is apparently affected by the different roughness of the samples and their different profile of nitrogen.

Keywords: ion implantation, plasma, RF and microwave plasma, stainless steel

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Authors: Mauricio A. Sarabia-Vallejos, Carmen M. Gonzalez-Henriquez, Adolfo Del Campo-Garcia, Aitzibier L. Cortajarena, Juan Rodriguez-Hernandez

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In this study, it was explored the formation and the morphological differences between wrinkled hydrogel patterns obtained via generation of surface instabilities. The slight variations in the polymerization conditions produce important changes in the material composition and pattern structuration. The compounds were synthesized using three main components, i.e. an amphiphilic monomer, hydroxyethyl methacrylate (HEMA), a hydrophobic monomer, trifluoroethyl methacrylate (TFMA), and a hydrophilic crosslinking agent, poly(ethylene glycol) diacrylate (PEGDA). The first part of this study was related to the formation of wrinkled surfaces using only HEMA and PEGDA and varying the amount of water added in the reaction. The second part of this study involves the gradual insertion of TFMA into the hydrophilic reaction mixture. Interestingly, the manipulation of the chemical composition of this hydrogel affects both surface morphology and physicochemical characteristics of the patterns, inducing transitions from one particular type of structure (wrinkles or ripples) to different ones (creases, folds, and crumples). Contact angle measurements show that the insertion of TFMA produces a slight decrease in surface wettability of the samples, remaining however highly hydrophilic (contact angle below 45°). More interestingly, by using confocal Raman spectroscopy, important information about the wrinkle formation mechanism is obtained. The procedure involving two consecutive thermal and photopolymerization steps lead to a “pseudo” two-layer system. Thus, upon photopolymerization, the surface is crosslinked to a higher extent than the bulk and water evaporation drives the formation of wrinkled surfaces. Finally, cellular, and bacterial proliferation studies were performed to the samples, showing that the amount of TFMA included in each sample slightly affects the proliferation of both (bacteria and cells), but in the case of bacteria, the morphology of the sample also plays an important role, importantly reducing the bacterial proliferation.

Keywords: antibiofouling properties, hydrophobic/hydrophilic balance, morphologic characterization, wrinkled hydrogel patterns

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Authors: Babak Sadeghi, Rony Snyders, Marie-Paule.Delplancke-Ogletree

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Nitrogen fixation (NF) is one of the crucial industrial processes. Many attempts have been made in order to artificially fix nitrogen, and among them, the Haber-Bosch’s (H-B) process is widely used. However, it presents two major drawbacks: huge fossil feedstock consumption and noticeable greenhouse gases emission. It is, therefore, necessary to develop alternatives. Plasma technology, as an inherent “green” technology, is considered to have a great potential for reducing the environmental impacts and improving the energy efficiency of the NF process. In this work, we have studied the catalyst assisted microwave plasma for NF application. Heterogeneous catalysts of MoO₃, with various loads 0, 5, 10, 20, and 30 wt%, supported on γ-alumina were prepared by conventional wet impregnation. Crystallinity, surface area, pore size, and microstructure were obtained by X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) adsorption isotherm, Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The XRD patterns of calcined alumina confirm the γ- phase. Characteristic picks of MoO₃ could not be observed for low loads (< 20 wt%), likely indicating a high dispersion of metal oxide over the support. The specific surface area along with pores size are decreasing with increasing calcination temperature and MoO₃ loading. The MoO₃ loading does not modify the microstructure. TEM and SEM results for loading inferior to 20 wt% are coherent with a monolayer of MoO₃ on the support as proposed elsewhere. For loading of 20 wt% and more, TEM and Electron diffraction (ED) show nanocrystalline ₃-D MoO₃ particles. The catalytic performances of these catalysts were investigated in the post-discharge of a microwave plasma for NOx formation from N₂/O₂ mixtures. The plasma is sustained by a surface wave launched in a quartz tube via a surfaguide supplied by a 2.45 GHz microwave generator in pulse mode. In-situ identification and quantification of the products were carried out by Fourier-transform infrared spectroscopy (FTIR) in the post-discharge region. FTIR analysis of the exhausted gas reveal NO and NO₂ bands in presence of catalyst while only NO band were assigned without catalyst. On the other hand, in presence of catalyst, a 10% increase of NOₓ formation and of 20% increase in energy efficiency are observed.

Keywords: γ-Al2O₃-MoO₃, µ-waveplasma, N2 fixation, Plasma-catalysis, Plasma diagnostic

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Authors: A. Schander, T. Tessmann, H. Stemmann, S. Strokov, A. Kreiter, W. Lang

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For the chronic application of neural prostheses and other brain-computer interfaces, long-term stable microelectrodes for electrical stimulation are essential. In recent years many developments were done to investigate different appropriate materials for these electrodes. One of these materials is the electrical conductive polymer poly(3,4-ethylenedioxythiophene) (PEDOT), which has lower impedance and higher charge injection capacity compared to noble metals like gold and platinum. However the long-term stability of this polymer is still unclear. Thus this paper reports on the in-vitro evaluation of the long-term stability of PEDOT coated gold microelectrodes. For this purpose a highly flexible electrocorticography (ECoG) electrode array, based on the polymer polyimide, is used. This array consists of circular gold electrodes with a diameter of 560 µm (0.25 mm2). In total 25 electrodes of this array were coated simultaneously with the polymer PEDOT:PSS in a cleanroom environment using a galvanostatic electropolymerization process. After the coating the array is additionally sterilized using a steam sterilization process (121°C, 1 bar, 20.5 min) to simulate autoclaving prior to the implantation of such an electrode array. The long-term measurements were performed in phosphate-buffered saline solution (PBS, pH 7.4) at the constant body temperature of 37°C. For the in-vitro electrical stimulation a one channel bipolar current stimulator is used. The stimulation protocol consists of a bipolar current amplitude of 5 mA (cathodal phase first), a pulse duration of 100 µs per phase, a pulse pause of 50 µs and a frequency of 1 kHz. A PEDOT:PSS coated gold electrode with an area of 1 cm2 serves as the counter electrode. The electrical stimulation is performed continuously with a total amount of 86.4 million bipolar current pulses per day. The condition of the PEDOT coated electrodes is monitored in between with electrical impedance spectroscopy measurements. The results of this study demonstrate that the PEDOT coated electrodes are stable for more than 3.6 billion bipolar current pulses. Also the unstimulated electrodes show currently no degradation after the time period of 5 months. These results indicate an appropriate long-term stability of this electrode coating for chronic recording and electrical stimulation. The long-term measurements are still continuing to investigate the life limit of this electrode coating.

Keywords: chronic recording, electrical stimulation, long-term stability, microelectrodes, PEDOT

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Authors: David Adade-Boateng, Benard Fei Baffoe, Colin A. Booth, Michael A. Fullen

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Remediation of diesel fuel, oil and grease in contaminated soils obtained from a mine site in Ghana are explored using rhizoremediation technology with different levels of nutrient amendments (i.e. N (nitrogen) in Compost (0.2, 0.5 and 0.8%), Urea (0.2, 0.5 and 0.8%) and Topsoil (0.2, 0.5 and 0.8%)) for a native species. A Ghanaian native grass species, Paspalum spp. from the Poaceae family, indicative across Sub-Saharan Africa, was selected following the development of essential and desirable growth criteria. Vegetative parts of the species were subjected to ten treatments in a Randomized Complete Block Design (RCBD) in three replicates. The plant-associated microbial community was examined in Paspalum spp. An assessment of the influence of Paspalum spp on the abundance and activity of micro-organisms in the rhizosphere revealed a build-up of microbial communities over a three month period. This was assessed using the MPN method, which showed rhizospheric samples from the treatments were significantly different (P <0.05). Multiple comparisons showed how microbial populations built-up in the rhizosphere for the different treatments. Treatments G (0.2% compost), H (0.5% compost) and I (0.8% compost) performed significantly better done other treatments, while treatments D (0.2% topsoil) and F (0.8% topsoil) were insignificant. Furthermore, treatment A (0.2% urea), B (0.5% urea), C (0.8% urea) and E (0.5% topsoil) also performed the same. Residual diesel and oil concentrations (as total petroleum hydrocarbons, TPH and oil and grease) were measured using infra-red spectroscopy and gravimetric methods, respectively. The presence of single species successfully enhanced the removal of hydrocarbons from soil. Paspalum spp. subjected to compost levels (0.5% and 0.8%) and topsoil levels (0.5% and 0.8%) showed significantly lower residual hydrocarbon concentrations compared to those treated with Urea. A strong relationship (p<0.001) between the abundance of hydrocarbon degrading micro-organisms in the rhizosphere and hydrocarbon biodegradation was demonstrated for rhizospheric samples with treatment G (0.2% compost), H (0.5% compost) and I (0.8% compost) (P <0.001). The same level of amendment with 0.8% compost (N-level) can improve the application effectiveness. These findings have wide-reaching implications for the environmental management of soils contaminated by hydrocarbons in Sub-Saharan Africa. However, it is necessary to further investigate the in situ rhizoremediation potential of Paspalum spp. at the field scale.

Keywords: rhizoremediation, microbial population, rhizospheric sample, treatments

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Authors: Mohamed H. Sorour, Hayam F. Shaalan, Heba A. Hani, Eman S. Sayed

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Ion exchange adsorption has a long standing history of success for seawater softening and selective ion removal from saline sources. Strong, weak and mixed types ion exchange systems could be designed and optimized for target separation. In this paper, different types of adsorbents comprising zeolite 13X and kaolin, in addition to, poly acrylate/zeolite (AZ), poly acrylate/kaolin (AK) and stand-alone poly acrylate (A) hydrogel types were prepared via microwave (M) and ultrasonic (U) irradiation techniques. They were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The developed adsorbents were evaluated on bench scale level and based on assessment results, a composite bed has been formulated for performance evaluation in pilot scale column investigations. Owing to the hydrogel nature of the partially crosslinked poly acrylate, the developed adsorbents manifested a swelling capacity of about 50 g/g. The pilot trials have been carried out using magnesium enriched Red Seawater to simulate Red Seawater desalination brine. Batch studies indicated varying uptake efficiencies, where Mg adsorption decreases according to the following prepared hydrogel types AU>AM>AKM>AKU>AZM>AZU, being 108, 107, 78, 69, 66 and 63 mg/g, respectively. Composite bed adsorbent tested in the up-flow mode column studies indicated good performance for Mg uptake. For an operating cycle of 12 h, the maximum uptake during the loading cycle approached 92.5-100 mg/g, which is comparable to the performance of some commercial resins. Different regenerants have been explored to maximize regeneration and minimize the quantity of regenerants including 15% NaCl, 0.1 M HCl and sodium carbonate. Best results were obtained by acidified sodium chloride solution. In conclusion, developed cation exchange adsorbents comprising clay or zeolite support indicated adequate performance for Mg recovery under saline environment. Column design operated at the up-flow mode (approaching expanded bed) is appropriate for such type of separation. Preliminary cost indicators for Mg recovery via ion exchange have been developed and analyzed.

Keywords: batch and dynamic magnesium separation, seawater, polyacrylate hydrogel, cost evaluation

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Authors: Roman Matejka, Vaclav Prochazka, Tibor Izak, Jana Stepanovska, Martina Travnickova, Alexander Kromka

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Cell-based impedance spectroscopy is suitable method for electrical monitoring of cell activity especially on substrates that cannot be easily inspected by optical microscope (without fluorescent markers) like decellularized tissues, nano-fibrous scaffold etc. Special sensor for this measurement was developed. This sensor consists of corning glass substrate with gold interdigitated electrodes covered with diamond layer. This diamond layer provides biocompatible non-conductive surface for cells. Also, a special PPFC flow cultivation chamber was developed. This chamber is able to fix sensor in place. The spring contacts are connecting sensor pads with external measuring device. Construction allows real-time live cell imaging. Combining with perfusion system allows medium circulation and generating shear stress stimulation. Experimental evaluation consist of several setups, including pure sensor without any coating and also collagen and fibrin coating was done. The Adipose derived stem cells (ASC) and Human umbilical vein endothelial cells (HUVEC) were seeded onto sensor in cultivation chamber. Then the chamber was installed into microscope system for live-cell imaging. The impedance measurement was utilized by vector impedance analyzer. The measured range was from 10 Hz to 40 kHz. These impedance measurements were correlated with live-cell microscopic imaging and immunofluorescent staining. Data analysis of measured signals showed response to cell adhesion of substrates, their proliferation and also change after shear stress stimulation which are important parameters during cultivation. Further experiments plan to use decellularized tissue as scaffold fixed on sensor. This kind of impedance sensor can provide feedback about cell culture conditions on opaque surfaces and scaffolds that can be used in tissue engineering in development artificial prostheses. This work was supported by the Ministry of Health, grants No. 15-29153A and 15-33018A.

Keywords: bio-impedance measuring, bioreactor, cell cultivation, diamond layer, gold interdigitated electrodes, tissue engineering

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Authors: Josline Salib, Sayed El-Toumy, Abeer Salama, Enayat Omara, Emad Hassan

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Diabetic nephropathy is an important cause of morbidity and mortality and is now among the most common causes of end-stage renal failure (ESRF) in developed countries. Thus, the aim of the present study was to investigate the phenolic compounds content of Cichorium intybus aerial parts extracts as well as the therapeutic effects on diabetic nephropathy, oxidative stress, and anti-inflammatory by characterizing biochemical, histopathological changes and immunohistochemistry in an experimental diabetic rat model as compared with Amaryl. Ten known compounds of flavonoids, coumarins and phenolic acid derivatives were isolated from the C. intybus aqueous methanolic extract. Structures of the isolated compounds were established by chromatography, UV and 1D⁄2D 1H⁄ 13C spectroscopy. The aqueous methanol extract of C. intybus aerial parts was administered to Streptozotocin diabetes rats at doses (100 and 200 mg/kg) for 21 days. After treatment, blood glucose, serum insulin, urea, creatinine, and TNF-α were evaluated. Enzymatic scavengers including catalase (CAT), glutathione (GSH), malondialdehyde (MDA) and nitric oxide (NO) were determined to evaluate the oxidative status in the renal tissue. Diabetic rats treated with C. intybus extract showed a dose-dependent reduction of fasting blood glucose and kidney antioxidant status in comparison to the diabetic control group. The extract was able to enhance the antioxidant defenses of the kidney by increasing the reduced GSH and CAT content and decreasing MDA content in addition to significantly decreasing kidney nitric oxide content compared to diabetic control rats. Furthermore, the histopathological findings in C. intybus extract administered rats were observed at markedly lesser extent than the diabetic control group. Also, inducible nitric oxide synthase (iNOS) levels were decreased significantly after the administration of high-dose C. intybus extract in diabetic rats. Showing significant antihyperglycemic and antioxidant properties of C. intybus aerial parts extract, which is attributed to its polyphenolic content, may offer a potential source for the treatment of diabetes.

Keywords: antioxidant activity, anti-diabetic nephropathy, cichorium intybus aerial parts, phenolic compounds

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Authors: Mohamed Moustafa, Medhat Abdallah, Ramy Magdy, Ahmed Abdrabou, Mohamed Badr

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The scribe box under study dates back to the old kingdom. It was excavated by the Italian expedition in Qena (1935-1937). The box consists of 2pieces, the lid and the body. The inner side of the lid is decorated with ancient Egyptian inscriptions written with a black pigment. The box was made using several panels assembled together by wooden dowels and secured with plant ropes. The entire box is covered with a red pigment. This study aims to use analytical techniques in order to identify and have deep understanding for the box components. Moreover, the authors were significantly interested in using infrared reflectance transmission imaging (RTI-IR) to improve the hidden inscriptions on the lid. The identification of wood species included in this study. The visual observation and assessment were done to understand the condition of this box. 3Ddimensions and 2D programs were used to illustrate wood joints techniques. Optical microscopy (OM), X-ray diffraction (XRD), X-ray fluorescence portable (XRF) and Fourier Transform Infrared spectroscopy (FTIR) were used in this study in order to identify wood species, remains of insects bodies, red pigment, fibers plant and previous conservation adhesives, also RTI-IR technique was very effective to improve hidden inscriptions. The analysis results proved that wooden panels and dowels were identified as Acacia nilotica, wooden rail was Salix sp. the insects were identified as Lasioderma serricorne and Gibbium psylloids, the red pigment was Hematite, while the fiber plants were linen, previous adhesive was identified as cellulose nitrates. The historical study for the inscriptions proved that it’s a Hieratic writings of a funerary Text. After its transportation from the Egyptian museum storage to the wood conservation laboratory of the Grand Egyptian museum –conservation center (GEM-CC), conservation techniques were applied with high accuracy in order to restore the object including cleaning , consolidating of friable pigments and writings, removal of previous adhesive and reassembly, finally the conservation process that were applied were extremely effective for this box which became ready for display or storage in the grand Egyptian museum.

Keywords: scribe box, hieratic, 3D program, Acacia nilotica, XRD, cellulose nitrate, conservation

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Authors: Mohamed H. Sorour, Hayam F. Shaalan, Heba A. Hani, Eman S. Sayed, Amany A. El-Mansoup

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Heavy metals (HMs) present an increasing threat to aquatic and soil environment. Thus, techniques should be developed for the removal and/or recovery of those HMs from point sources in the generating industries. This paper reports our endeavors concerning the development of in-house developed weak cation exchange polyacrylate hydrogel kaolin composites for heavy metals removal. This type of composite enables desirable characteristics and functions including mechanical strength, bed porosity and cost advantages. This paper emphasizes the effect of varying crosslinker (methylenebis(acrylamide)) concentration. The prepared cation exchanger has been subjected to intensive characterization using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray fluorescence (XRF) and Brunauer Emmett and Teller (BET) method. Moreover, the performance was investigated using synthetic and real wastewater for an industrial complex east of Cairo. Simulated and real wastewater compositions addressed; Cr, Co, Ni, and Pb are in the range of (92-115), (91-103), (86-88) and (99-125), respectively. Adsorption experiments have been conducted in both batch and column modes. In general, batch tests revealed enhanced cation exchange capacities of 70, 72, 78.2 and 99.9 mg/g from single synthetic wastes while, removal efficiencies of 82.2, 86.4, 44.4 and 96% were obtained for Cr, Co, Ni and Pb, respectively from mixed synthetic wastes. It is concluded that the mixed synthetic and real wastewaters have lower adsorption capacities than single solutions. It is worth mentioned that Pb attained higher adsorption capacities with comparable results in all tested concentrations of synthetic and real wastewaters. Pilot scale experiments were also conducted for mixed synthetic waste in a fluidized bed column for 48 hour cycle time which revealed 86.4%, 58.5%, 66.8% and 96.9% removal efficiency for Cr, Co, Ni, and Pb, respectively with maximum regeneration was also conducted using saline and acid regenerants. Maximum regeneration efficiencies for the column studies higher than the batch ones about by about 30% to 60%. Studies are currently under way to enhance the regeneration efficiency to enable successful scaling up of the adsorption column.

Keywords: polyacrylate hydrogel kaolin, ultrasonic irradiation, heavy metals, adsorption and regeneration

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Authors: F. Pires, V. Geraldo, O. N. Oliveira Jr., M. Raposo

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Catechins are powerful antioxidants which have attractive properties useful for tumor therapy. Considering their antioxidant activity, these molecules can act as a scavenger of the reactive oxygen species (ROS), alleviating the damage of cell membrane induced by oxidative stress. The complexity and dynamic nature of the cell membrane compromise the analysis of the biophysical interactions between drug and cell membrane and restricts the transport or uptake of the drug by intracellular targets. To avoid the cell membrane complexity, we used biomimetic systems as liposomes and Langmuir monolayers to study the interaction between catechin and membranes at the molecular level. Liposomes were formed after the dispersion of anionic 1,2-dipalmitoyl-sn-glycero-3-[phospho-rac-(1-glycerol)(sodium salt) (DPPG) phospholipids in an aqueous solution, which mimic the arrangement of lipids in natural cell membranes and allows the entrapment of catechins. Langmuir monolayers were formed after dropping amphiphilic molecules, DPPG phospholipids, dissolved in an organic solvent onto the water surface. In this work, we mixed epigallocatechin-3-gallate (EGCG) with DPPG liposomes and exposed them to ultra-violet radiation in order to evaluate the antioxidant potential of these molecules against oxidative stress induced by radiation. The presence of EGCG in the mixture decreased the rate of lipid peroxidation, proving that EGCG protects membranes through the quenching of the reactive oxygen species. Considering the high amount of hydroxyl groups (OH groups) on structure of EGCG, a possible mechanism to these molecules interact with membrane is through hydrogen bonding. We also investigated the effect of EGCG at various concentrations on DPPG Langmuir monolayers. The surface pressure isotherms and infrared reflection-absorption spectroscopy (PM-IRRAS) results corroborate with absorbance results preformed on liposome-model, showing that EGCG interacts with polar heads of the monolayers. This study elucidates the physiological action of EGCG which can be incorporated in lipid membrane. These results are also relevant for the improvement of the current protocols used to incorporate catechins in drug delivery systems.

Keywords: catechins, lipid membrane, anticancer agent, molecular interactions

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Authors: Bertalan Jillek, Péter Szabó, Judit Kopniczky, István Szabó, Balázs Patczai, Kinga Turzó

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Hip and knee prostheses are one of the most frequently used medical implants, that can significantly improve patients’ quality of life. Long term success and biointegration of these prostheses depend on several factors, like bulk and surface characteristics, construction and biocompatibility of the material. The applied surgical technique, the general health condition and life-quality of the patient are also determinant factors. Medical devices used in orthopedic surgeries have different surfaces depending on their function inside the human body. Surface roughness of these implants determines the interaction with the surrounding tissues. Numerous modifications have been applied in the recent decades to improve a specific property of an implant. Our goal was to compare the surface characteristics of typical implant materials used in orthopedic surgery and traumatology. Morphological and chemical structure of Vortex plate anodized titanium, cemented THR (total hip replacement) stem high nitrogen REX steel (SS), uncemented THR stem and cup titanium (Ti) alloy with titanium plasma spray coating (TPS), cemented cup and uncemented acetabular liner HXL and UHMWPE and TKR (total knee replacement) femoral component CoCrMo alloy (Sanatmetal Ltd, Hungary) discs were examined. Visualization and elemental analysis were made by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Surface roughness was determined by atomic force microscopy (AFM) and profilometry. SEM and AFM revealed the morphological and roughness features of the examined materials. TPS Ti presented the highest Ra value (25 ± 2 μm, followed by CoCrMo alloy (535 ± 19 nm), Ti (227 ± 15 nm) and stainless steel (170 ± 11 nm). The roughness of the HXL and UHMWPE surfaces was in the same range, 147 ± 13 nm and 144 ± 15 nm, respectively. EDS confirmed typical elements on the investigated prosthesis materials: Vortex plate Ti (Ti, O, P); TPS Ti (Ti, O, Al); SS (Fe, Cr, Ni, C) CoCrMo (Co, Cr, Mo), HXL (C, Al, Ni) and UHMWPE (C, Al). The results indicate that the surface of prosthesis materials have significantly different features and the applied investigation methods are suitable for their characterization. Contact angle measurements and in vitro cell culture testing are further planned to test their surface energy characteristics and biocompatibility.

Keywords: morphology, PE, roughness, titanium

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Authors: Norica Godja, Andreas Schindel, Luka Payrits, Zsolt Pasztor, Bálint Hegedüs, Petr Homola, Jan Horňas, Jiří Běhal, Roman Ruzek, Martin Holzleitner, Sascha Senck

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In order to reduce fuel consumption and CO₂ emissions in the aviation sector, innovative solutions are being sought to reduce the weight of aircraft, including additive manufacturing (AM). Of particular importance are the excellent mechanical properties that are required for aircraft structures. Ti6Al4V alloys, with their high mechanical properties in relation to weight, can reduce the weight of aircraft structures compared to structures made of steel and aluminium. Currently, conventional processes such as casting and CNC machining are used to obtain the desired structures, resulting in high raw material removal, which in turn leads to higher costs and impacts the environment. Additive manufacturing (AM) offers advantages in terms of weight, lead time, design, and functionality and enables the realisation of alternative geometric shapes with high mechanical properties. However, there are currently technological shortcomings that have led to AM not being approved for structural components with high safety requirements. An assessment of damage tolerance for AM parts is required, and quality control needs to be improved. Pores and other defects cannot be completely avoided at present, but they should be kept to a minimum during manufacture. The mechanical properties of the manufactured parts can be further improved by various treatments. The influence of different treatment methods (heat treatment, CNC milling, electropolishing, chemical polishing) and operating parameters were investigated by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray diffraction (XRD), electron backscatter diffraction (EBSD) and measurements with a focused ion beam (FIB), taking into account surface roughness, possible anomalies in the chemical composition of the surface and possible cracks. The results of the characterisation of the constructed and treated samples are discussed and presented in this paper. These results were generated within the framework of the 3TANIUM project, which is financed by EU with the contract number 101007830.

Keywords: Ti6Al4V alloys, laser powder bed fusion, damage tolerance, heat treatment, electropolishing, potential cracking

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Authors: Fatma A. Mohamed, Hend M. Ahmed

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This research explores the antimicrobial effects of dielectric barrier discharge (DBD) oxygen plasma treatment combined with ZnO NPs on the cotton fabric, focusing on various treatment durations (5, 10, 15, 20, and 30 minutes) and discharge powers (15.5–17.35 watts) at flow rate 0.5 l/min. After treatment with oxygen plasma and ZnO NPs, the fabric was printed with green tea (Camellia sinensis) at five different concentrations. The study evaluated the treatment's effectiveness by analyzing surface wettability, specifically through wet-out time and hydrophilicity, as well as measuring contact angles. To investigate the chemical changes on the fabric's surface, attenuated total reflectance–Fourier transform infrared (ATR-FTIR) spectroscopy was employed to identify the functional groups formed as a result of the plasma treatment. This comprehensive approach aims to understand how DBD oxygen plasma treatment and ZnO nanoparticles change cotton fabric properties and enhance its antimicrobial potential, paving the way for innovative applications in textiles. In addition to the chemical analysis, the surface morphology of the O₂ plasma/ZnO NPs-treated cotton fabric was examined using scanning electron microscopy (SEM). FTIR analysis revealed an increase in polar functional groups (-COOH, -OH, and -C≡O) on the fabric's surface, contributing to enhanced hydrophilicity and functionality. The antimicrobial properties were evaluated using qualitative and quantitative methods, including agar plate assays and modified Hoenstein tests against Staphylococcus aureus and Escherichia coli. The results indicated a significant improvement in antimicrobial effectiveness for the cotton fabric treated with plasma and coated with natural extracts, maintaining this efficacy even after four washing cycles. This research demonstrates that utilizing oxygen DBD plasma/ZnO NPs treatment, combined with the absorption of tea and tulsi leaf extracts, presents a promising strategy for developing natural antimicrobial textiles. This approach is particularly relevant given the increasing medical and healthcare demands for effective antimicrobial materials. Overall, the method not only enhances the absorption of plant extracts but also significantly boosts antimicrobial efficacy, offering valuable insights for future textile applications.

Keywords: cotton, ZnO NPs, green tea leaf, antimicrobial avtivity, DBD oxygen plasma

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Authors: Joel F. Campbell, Bing Lin, Michael Obland, Susan Kooi, Tai-Fang Fan, Byron Meadows, Edward Browell, Wayne Erxleben, Doug McGregor, Jeremy Dobler, Sandip Pal, Christopher O'Dell, Ken Davis

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The Active Sensing of CO₂ Emissions over Nights, Days, and Seasons (ASCENDS) CarbonHawk Experiment Simulator (ACES) is a NASA Langley Research Center instrument funded by NASA’s Science Mission Directorate that seeks to advance technologies critical to measuring atmospheric column carbon dioxide (CO₂ ) mixing ratios in support of the NASA ASCENDS mission. The ACES instrument, an Intensity-Modulated Continuous-Wave (IM-CW) lidar, was designed for high-altitude aircraft operations and can be directly applied to space instrumentation to meet the ASCENDS mission requirements. The ACES design demonstrates advanced technologies critical for developing an airborne simulator and spaceborne instrument with lower platform consumption of size, mass, and power, and with improved performance. The Atmospheric Carbon and Transport – America (ACT-America) is an Earth Venture Suborbital -2 (EVS-2) mission sponsored by the Earth Science Division of NASA’s Science Mission Directorate. A major objective is to enhance knowledge of the sources/sinks and transport of atmospheric CO₂ through the application of remote and in situ airborne measurements of CO₂ and other atmospheric properties on spatial and temporal scales. ACT-America consists of five campaigns to measure regional carbon and evaluate transport under various meteorological conditions in three regional areas of the Continental United States. Regional CO₂ distributions of the lower atmosphere were observed from the C-130 aircraft by the Harris Corp. Multi-Frequency Fiber Laser Lidar (MFLL) and the ACES lidar. The airborne lidars provide unique data that complement the more traditional in situ sensors. This presentation shows the applications of CO₂ lidars in support of these science needs.

Keywords: CO₂ measurement, IMCW, CW lidar, laser spectroscopy

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Authors: Lotanna Ezeonu, Jason P. Robbins, Ziyu Tang, Xiaofang Yang, Bruce E. Koel, Simon G. Podkolzin

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The interaction of organic molecules with metal surfaces is of interest in numerous technological applications, such as catalysis, bone replacement, and biosensors. Acetic acid is one of the main products of bio-oils produced from the pyrolysis of hemicellulosic feedstocks. However, their high oxygen content makes them unsuitable for use as fuels. Hydrodeoxygenation is a proven technique for catalytic deoxygenation of bio-oils. An understanding of the energetics and control of the bond-breaking sequences of biomass-derived oxygenates on metal surfaces will enable a guided optimization of existing catalysts and the development of more active/selective processes for biomass transformations to fuels. Such investigations have been carried out with the aid of ultrahigh vacuum and its concomitant techniques. The high catalytic activity of platinum in biomass-derived oxygenate transformations has sparked a lot of interest. We herein exploit infrared reflection absorption spectroscopy(IRAS), temperature-programmed desorption(TPD), and density functional theory(DFT) to study the adsorption and decomposition of acetic acid on a Pt(111) surface, which was then compared with Ni(111), a model non-noble metal. We found that acetic acid adsorbs molecularly on the Pt(111) surface, interacting through the lone pair of electrons of one oxygen atomat 90 K. At 140 K, the molecular form is still predominant, with some dissociative adsorption (in the form of acetate and hydrogen). Annealing to 193 K led to complete dehydrogenation of molecular acetic acid species leaving adsorbed acetate. At 440 K, decomposition of the acetate species occurs via decarbonylation and decarboxylation as evidenced by desorption peaks for H₂,CO, CO₂ and CHX fragments (x=1, 2) in theTPD.The assignments for the experimental IR peaks were made using visualization of the DFT-calculated vibrational modes. The results showed that acetate adsorbs in a bridged bidentate (μ²η²(O,O)) configuration. The coexistence of linear and bridge bonded CO was also predicted by the DFT results. Similar molecular acid adsorption energy was predicted in the case of Ni(111) whereas a significant difference was found for acetate adsorption.

Keywords: acetic acid, platinum, nickel, infared-absorption spectrocopy, temperature programmed desorption, density functional theory

Procedia PDF Downloads 105

Authors: Mannar R. Maurya, Bithika Sarkar, Fernando Avecilla

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Peroxidase activity is possibly successfully used for different industrial processes in medicine, chemical industry, food processing and agriculture. However, they bear some intrinsic drawback associated with denaturation by proteases, their special storage requisite and cost factor also. Now a day’s artificial enzyme mimics are becoming a research interest because of their significant applications over conventional organic enzymes for ease of their preparation, low price and good stability in activity and overcome the drawbacks of natural enzymes e.g serine proteases. At present, a large number of artificial enzymes have been synthesized by assimilating a catalytic center into a variety of schiff base complexes, ligand-anchoring, supramolecular complexes, hematin, porphyrin, nanoparticles to mimic natural enzymes. Although in recent years a several number of vanadium complexes have been reported by a continuing increase in interest in bioinorganic chemistry. To our best of knowledge, the investigation of artificial enzyme mimics of vanadium complexes is very less explored. Recently, our group has reported synthetic vanadium schiff base complexes capable of mimicking peroxidases. Herein, we have synthesized monoidovanadium(IV) and dioxidovanadium(V) complexes of pyrazoleone derivateis ( extensively studied on account of their broad range of pharmacological appication). All these complexes are characterized by various spectroscopic techniques like FT-IR, UV-Visible, NMR (1H, 13C and 51V), Elemental analysis, thermal studies and single crystal analysis. The peroxidase mimic activity has been studied towards oxidation of pyrogallol to purpurogallin with hydrogen peroxide at pH 7 followed by measuring kinetic parameters. The Michaelis-Menten behavior shows an excellent catalytic activity over its natural counterparts, e.g. V-HPO and HRP. The obtained kinetic parameters (Vmax, Kcat) were also compared with peroxidase and haloperoxidase enzymes making it a promising mimic of peroxidase catalyst. Also, the catalytic activity has been studied towards the oxidation of 1-phenylethanol in presence of H2O2 as an oxidant. Various parameters such as amount of catalyst and oxidant, reaction time, reaction temperature and solvent have been taken into consideration to get maximum oxidative products of 1-phenylethanol.

Keywords: oxovanadium(IV)/dioxidovanadium(V) complexes, NMR spectroscopy, Crystal structure, peroxidase mimic activity towards oxidation of pyrogallol, Oxidation of 1-phenylethanol

Procedia PDF Downloads 339

Authors: Alan Luo, Hunter N. B. Moseley

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Many macromolecular structure entries in the Protein Data Bank (PDB) have a range of regional (localized) quality issues, be it derived from x-ray crystallography, Nuclear Magnetic Resonance (NMR) spectroscopy, or other experimental approaches. However, most PDB entries are judged by global quality metrics like R-factor, R-free, and resolution for x-ray crystallography or backbone phi-psi distribution statistics and average restraint violations for NMR. Regional quality is often ignored when PDB entries are re-used for a variety of structurally based analyses. The binding of ligands, especially ligands involved in energy metabolism, is of particular interest in many structurally focused protein studies. Using a regional quality metric that provides chemically interpretable information from electron density maps, a significant number of outliers in regional structural quality was detected across x-ray crystallographic PDB entries for proteins bound to biochemically critical ligands. In this study, a series of analyses was performed to evaluate both specific and general potential factors that could promote these outliers. In particular, these potential factors were the minimum distance to a metal ion, the minimum distance to a crystal contact, and the isotropic atomic b-factor. To evaluate these potential factors, Fisher’s exact tests were performed, using regional quality criteria of outlier (top 1%, 2.5%, 5%, or 10%) versus non-outlier compared to a potential factor metric above versus below a certain outlier cutoff. The results revealed a consistent general effect from region-specific normalized b-factors but no specific effect from metal ion contact distances and only a very weak effect from crystal contact distance as compared to the b-factor results. These findings indicate that no single specific potential factor explains a majority of the outlier ligand-bound regions, implying that human error is likely as important as these other factors. Thus, all factors, including human error, should be considered when regions of low structural quality are detected. Also, the downstream re-use of protein structures for studying ligand-bound conformations should screen the regional quality of the binding sites. Doing so prevents misinterpretation due to the presence of structural uncertainty or flaws in regions of interest.

Keywords: biomacromolecular structure, coenzyme, electron density discrepancy analysis, x-ray crystallography

Procedia PDF Downloads 128

Authors: Erwin San Juan Martinez, Miguel Angel Aguilar Mendez, Manuel Sandoval Villa, Libia Iris Trejo Tellez

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Some nanomaterials may improve the vegetal growth in certain concentration intervals, and could be used as nanofertilizers in order to increase crops yield, and decreasing the environmental pollution due to non-controlled use of conventional fertilizers, therefore the present investigation’s objective was to synthetize and characterize gelatin nanoparticles loaded with calcium generated through pulverization technique and be used as nanofertilizers. To obtain these materials, a fractional factorial design 27-4 was used in order to evaluate the largest number of factors (concentration of Ca2+, temperature and agitation time of the solution and calcium concentration, drying temperature, and % spray) with a possible effect on the size, distribution and morphology of nanoparticles. For the formation of nanoparticles, a Nano Spray-Dryer B - 90® (Buchi, Flawil, Switzerland), equipped with a spray cap of 4 µm was used. Size and morphology of the obtained nanoparticles were evaluated using a scanning electron microscope (JOEL JSM-6390LV model; Tokyo, Japan) equipped with an energy dispersive x-ray X (EDS) detector. The total quantification of Ca2+ as well as its release by the nanoparticles was carried out in an equipment of induction atomic emission spectroscopy coupled plasma (ICP-ES 725, Agilent, Mulgrave, Australia). Of the seven factors evaluated, only the concentration of fertilizer, % spray and concentration of polymer presented a statistically significant effect on particle size. Micrographs of SEM from six of the eight conditions evaluated in this research showed particles separated and with a good degree of sphericity, while in the other two particles had amorphous morphology and aggregation. In all treatments, most of the particles showed smooth surfaces. The average size of smallest particle obtained was 492 nm, while EDS results showed an even distribution of Ca2+ in the polymer matrix. The largest concentration of Ca2+ in ICP was 10.5%, which agrees with the theoretical value calculated, while the release kinetics showed an upward trend within 24 h. Using the technique employed in this research, it was possible to obtain nanoparticles loaded with calcium, of good size, sphericity and with release controlled properties. The characteristics of nanoparticles resulted from manipulation of the conditions of synthesis which allow control of the size and shape of the particles, and provides the means to adapt the properties of the materials to an specific application.

Keywords: calcium, controlled release, gelatin, nano spraydryer, nanofertilizer

Procedia PDF Downloads 178

Authors: Danilo A. F. Fontes, Magaly A. M.Lyra, Maria L. C. Moura, Leslie R. M. Ferraz, Salvana P. M. Costa, Amanda C. Q. M. Vieira, Larissa A. Rolim, Giovanna C. R. M. Schver, Ping I. Lee, Severino Alves-Júnior, José L. Soares-Sobrinho, Pedro J. Rolim-Neto

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Efavirenz (EFV) is a first-choice drug in antiretroviral therapy with high efficacy in the treatment of infection by Human Immunodeficiency Virus, which causes Acquired Immune Deficiency Syndrome (AIDS). EFV has low solubility in water resulting in a decrease in the dissolution rate and, consequently, in its bioavailability. Among the technological alternatives to increase solubility, the Lamellar Double Hydroxides (LDH) have been applied in the development of systems with poorly water-soluble drugs. The use of analytical techniques such as X-Ray Diffraction (XRD), Infrared Spectroscopy (IR) and Differential Scanning Calorimetry (DSC) allowed the elucidation of drug interaction with the lamellar compounds. The objective of this work was to characterize and develop the binary systems with EFV and LDH in order to increase the solubility of the drug. The LDH-CaAl was synthesized by the method of co-precipitation from salt solutions of calcium nitrate and aluminum nitrate in basic medium. The systems EFV-LDH and their physical mixtures (PM) were obtained at different concentrations (5-60% of EFV) using the solvent technique described by Takahashi & Yamaguchi (1991). The characterization of the systems and the PM’s was performed by XRD techniques, IR, DSC and dissolution test under non-sink conditions. The results showed improvements in the solubility of EFV when associated with LDH, due to a possible change in its crystal structure and formation of an amorphous material. From the DSC results, one could see that the endothermic peak at 173°C, temperature that correspond to the melting process of EFZ in the crystal form, was present in the PM results. For the EFZ-LDH systems (with 5, 10 and 30% of drug loading), this peak was not observed. XRD profiles of the PM showed well-defined peaks for EFV. Analyzing the XRD patterns of the systems, it was found that the XRD profiles of all the systems showed complete attenuation of the characteristic peaks of the crystalline form of EFZ. The IR technique showed that, in the results of the PM, there was the appearance of one band and overlap of other bands, while the IR results of the systems with 5, 10 and 30% drug loading showed the disappearance of bands and a few others with reduced intensity. The dissolution test under non-sink conditions showed that systems with 5, 10 and 30% drug loading promoted a great increase in the solubility of EFV, but the system with 10% of drug loading was the only one that could keep substantial amount of drug in solution at different pHs.

Keywords: Efavirenz, Lamellar Double Hydroxides, Pharmaceutical Techonology, Solubility

Procedia PDF Downloads 581

Authors: Yodai Ashikubo, Toshiaki Suzuki, Satoshi Kouya, Mitsuya Motohashi

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Functional microstructures such as wires, fins, needles, and rolls are currently being applied to variety of high-performance devices. Under these conditions, a roll structure (silicon micro-nanoroll) was formed on the surface of the silicon substrate via fine bubbles during anodization using an extremely diluted hydrofluoric acid (HF + H₂O). The as-formed roll had a microscale length and width of approximately 1 µm. The number of rolls was 3-10 times and the thickness of the film forming the rolls was about 10 nm. Thus, it is promising for applications as a distinct device material. These rolls functioned as capsules and/or pipelines. To date, number of rolls and roll length have been controlled by anodization conditions. In general, controlling the position and roll winding state is required for device applications. However, it has not been discussed. Grooves formed on silicon surface before anodization might be useful control the bubbles. In this study, we investigated the effect of the grooves on the position and shape of the roll. The surfaces of the silicon wafers were anodized. The starting material was p-type (100) single-crystalline silicon wafers. The resistivity of the wafer is 5-20 ∙ cm. Grooves were formed on the surface of the substrate before anodization using sandpaper and diamond pen. The average width and depth of the grooves were approximately 1 µm and 0.1 µm, respectively. The HF concentration {HF/ (HF + C₂H5OH + H₂O)} was 0.001 % by volume. The C2H5OH concentration {C₂H5OH/ (HF + C₂H5OH + H₂O)} was 70 %. A vertical single-tank cell and Pt cathode were used for anodization. The silicon roll was observed by field-emission scanning electron microscopy (FE-SEM; JSM-7100, JEOL). The atomic bonding state of the rolls was evaluated using X-ray photoelectron spectroscopy (XPS; ESCA-3400, Shimadzu). For straight groove, the rolls were formed along the groove. This indicates that the orientation of the rolls can be controlled by the grooves. For lattice-like groove, the rolls formed inside the lattice and along the long sides. In other words, the aspect ratio of the lattice is very important for the roll formation. In addition, many rolls were formed and winding states were not uniform when the lattice size is too large. On the other hand, no rolls were formed for small lattice. These results indicate that there is the optimal size of lattice for roll formation. In the future, we are planning on formation of rolls using groove formed by lithography technique instead of sandpaper and the pen. Furthermore, the rolls included nanoparticles will be formed for nanodevices.

Keywords: silicon roll, anodization, fine bubble, microstructure

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Authors: Saad Mohamed Elsaid Onaizah

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One of the reasons for the intensive use of pesticides is to protect agricultural crops and orchards from pests or agricultural worms. The period of time that pesticides stay inside the soil is estimated at about (2) to (12) weeks. Perhaps the most important reason that led to groundwater pollution is the easy leakage of these harmful pesticides from the soil into the aquifers. This research aims to find the best ways to use trated activated charcoal with gold nitrate solution; For the purpose of removing the deadly pesticides from the aqueous solution by adsorption phenomenon. The most used pesticides in Egypt were selected, such as Malathion, Methomyl Abamectin and, Thiamethoxam. Activated charcoal doped with gold ions was prepared by applying chemical and thermal treatments to activated charcoal using gold nitrate solution. Adsorption of studied pesticide onto activated carbon /Au was mainly by chemical adsorption forming complex with the gold metal immobilised on activated carbon surfaces. Also, gold atom was considered as a catalyst to cracking the pesticide molecule. Gold activated charcoal is a low cost material due to the use of very low concentrations of gold nitrate solution. its notice the great ability of activated charcoal in removing selected pesticides due to the presence of the positive charge of the gold ion, in addition to other active groups such as functional oxygen and lignin cellulose. The presence of pores of different sizes on the surface of activated charcoal is the driving force for the good adsorption efficiency for the removal of the pesticides under study The surface area of the prepared char as well as the active groups were determined using infrared spectroscopy and scanning electron microscopy. Some factors affecting the ability of activated charcoal were applied in order to reach the highest adsorption capacity of activated charcoal, such as the weight of the charcoal, the concentration of the pesticide solution, the time of the experiment, and the pH. Experiments showed that the maximum limit revealed by the batch adsorption study for the adsorption of selected insecticides was in contact time (80) minutes at pH (7.70). These promising results were confirmed, and by establishing the practical application of the developed system, the effect of various operating factors with equilibrium, kinetic and thermodynamic studies is evident, using the Langmuir application on the effectiveness of the absorbent material with absorption capacities higher than most other adsorbents.

Keywords: waste water, pesticides pollution, adsorption, activated carbon

Procedia PDF Downloads 78

Authors: Davoud Dorranian, Hajar Sadeghi, Elmira Solati

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Carbon nanostructures in various forms were synthesized using pulsed laser ablation of a graphite target in different liquid environment. The beam of a Q-switched Nd:YAG laser of 1064-nm wavelength at 7-ns pulse width is employed to irradiate the solid target in water, acetone, alcohol, and cetyltrimethylammonium bromide (CTAB). Then the effect of the liquid environment on the characteristic of carbon nanostructures produced by laser ablation was investigated. The optical properties of the carbon nanostructures were examined at room temperature by UV–Vis-NIR spectrophotometer. The crystalline structure of the carbon nanostructures was analyzed by X-ray diffraction (XRD). The morphology of samples was investigated by field emission scanning electron microscope (FE-SEM). Transmission electron microscope (TEM) was employed to investigate the form of carbon nanostructures. Raman spectroscopy was used to determine the quality of carbon nanostructures. Results show that different carbon nanostructures such as nanoparticles and few-layer graphene were formed in various liquid environments. The UV-Vis-NIR absorption spectra of samples reveal that the intensity of absorption peak of nanoparticles in alcohol is higher than the other liquid environments due to the larger number of nanoparticles in this environment. The red shift of the absorption peak of the sample in acetone confirms that produced carbon nanoparticles in this liquid are averagely larger than the other medium. The difference in the intensity and shape of the absorption peak indicated the effect of the liquid environment in producing the nanoparticles. The XRD pattern of the sample in water indicates an amorphous structure due to existence the graphene sheets. X-ray diffraction pattern shows that the degree of crystallinity of sample produced in CTAB is higher than the other liquid environments. Transmission electron microscopy images reveal that the generated carbon materials in water are graphene sheet and in the other liquid environments are graphene sheet and spherical nanostructures. According to the TEM images, we have the larger amount of carbon nanoparticles in the alcohol environment. FE-SEM micrographs indicate that in this liquids sheet like structures are formed however in acetone, produced sheets are adhered and these layers overlap with each other. According to the FE-SEM micrographs, the surface morphology of the sample in CTAB was coarser than that without surfactant. From Raman spectra, it can be concluded the distinct shape, width, and position of the graphene peaks and corresponding graphite source.

Keywords: carbon nanostructures, graphene, pulsed laser ablation, graphite

Procedia PDF Downloads 312

Authors: Bruno Baptista, Andreia S. R. Oliveira, Patricia V. Mendonca, Jorge F. J. Coelho, Fani Sousa

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Drug delivery systems are designed to allow adequate protection and controlled delivery of drugs to specific locations. These systems aim to reduce side effects and control the biodistribution profile of drugs, thus improving therapeutic efficacy. This study involved the synthesis of polymeric nanoparticles, based on amphiphilic diblock copolymers, comprising a biocompatible, poly (oligo (ethylene oxide) methyl ether methacrylate (POEOMA) as hydrophilic segment and a pH-sensitive block, the poly (2-diisopropylamino)ethyl methacrylate) (PDPA). The objective of this work was the development of polymeric pH-responsive nanoparticles to encapsulate and carry small RNAs as a model to further develop non-coding RNAs delivery systems with therapeutic value. The responsiveness of PDPA to pH allows the electrostatic interaction of these copolymers with nucleic acids at acidic pH, as a result of the protonation of the tertiary amine groups of this polymer at pH values below its pKa (around 6.2). Initially, the molecular weight parameters and chemical structure of the block copolymers were determined by size exclusion chromatography (SEC) and nuclear magnetic resonance (1H-NMR) spectroscopy, respectively. Then, the complexation with small RNAs was verified, generating polyplexes with sizes ranging from 300 to 600 nm and with encapsulation efficiencies around 80%, depending on the molecular weight of the polymers, their composition, and concentration used. The effect of pH on the morphology of nanoparticles was evaluated by scanning electron microscopy (SEM) being verified that at higher pH values, particles tend to lose their spherical shape. Since this work aims to develop systems for the delivery of non-coding RNAs, studies on RNA protection (contact with RNase, FBS, and Trypsin) and cell viability were also carried out. It was found that they induce some protection against constituents of the cellular environment and have no cellular toxicity. In summary, this research work contributes to the development of pH-sensitive polymers, capable of protecting and encapsulating RNA, in a relatively simple and efficient manner, to further be applied on drug delivery to specific sites where pH may have a critical role, as it can occur in several cancer environments.

Keywords: drug delivery systems, pH-responsive polymers, POEOMA-b-PDPA, small RNAs

Procedia PDF Downloads 258

Authors: Adebisi Adunola Demehin, Wanlaya Thamnarak, Jaruwan Chatwichien, Chatchakorn Eurtivong, Kiattawee Choowongkomon, Somsak Ruchirawat, Nopporn Thasana

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The epidermal growth factor receptor (EGFR) is a transmembrane glycoprotein involved in cellular signalling processes and, its aberrant activity is crucial in the development of many cancers such as lung cancer. Selaginellaceae are fern allies that have long been used in Chinese traditional medicine to treat various cancer types, especially lung cancer. Biflavonoids, the major secondary metabolites in Selaginellaceae, have numerous pharmacological activities, including anti-cancer and anti-inflammatory. For instance, amentoflavone induces a cytotoxic effect in the human NSCLC cell line via the inhibition of PARP-1. However, to the best of our knowledge, there are no studies on biflavonoids as EGFR inhibitors. Thus, this study aims to investigate the EGFR inhibitory activities of biflavonoids isolated from Selaginella siamensis and Selaginella bryopteris. Amentoflavone, tetrahydroamentoflavone, sciadopitysin, robustaflavone, robustaflavone-4-methylether, delicaflavone, and chrysocauloflavone were isolated from the ethyl-acetate extract of the whole plants. The structures were determined using NMR spectroscopy and mass spectrometry. In vitro study was conducted to evaluate their cytotoxicity against A549, HEPG2, and T47D human cancer cell lines using the MTT assay. In addition, a target-based assay was performed to investigate their EGFR inhibitory activity using the kinase inhibition assay. Finally, a molecular docking study was conducted to predict the binding modes of the compounds. Robustaflavone-4-methylether and delicaflavone showed the best cytotoxic activity on all the cell lines with IC50 (µM) values of 18.9 ± 2.1 and 22.7 ± 3.3 on A549, respectively. Of these biflavonoids, delicaflavone showed the most potent EGFR inhibitory activity with an 84% relative inhibition at 0.02 nM using erlotinib as a positive control. Robustaflavone-4-methylether showed a 78% inhibition at 0.15 nM. The docking scores obtained from the molecular docking study correlated with the kinase inhibition assay. Robustaflavone-4-methylether and delicaflavone had a docking score of 72.0 and 86.5, respectively. The inhibitory activity of delicaflavone seemed to be linked with the C2”=C3” and 3-O-4”’ linkage pattern. Thus, this study suggests that the structural features of these compounds could serve as a basis for developing new EGFR-TK inhibitors.

Keywords: anticancer, biflavonoids, EGFR, molecular docking, Selaginellaceae

Procedia PDF Downloads 197

Authors: Sesethu G. Njokweni, Marelize Botes, Emile W. H. Van Zyl

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An alternative strategy to the production of bioethanol is by examining the degradability of biomass in a natural system such as the rumen of mammals. This anaerobic microbial community has higher cellulolytic activities than microbial communities from other habitats and degrades cellulose to produce volatile fatty acids (VFA), methane and CO₂. VFAs have the potential to serve as intermediate products for electrochemical conversion to hydrocarbon fuels. In vitro mimicking of this process would be more cost-effective than bioethanol production as it does not require chemical pre-treatment of biomass, a sterile environment or added enzymes. The strategies of the carboxylate platform and the co-cultures of a bovine ruminal microbiota from cannulated cows were combined in order to investigate and optimize the bioconversion of agricultural biomass (apple and grape pomace, citrus pulp, sugarcane bagasse and triticale straw) to high value VFAs as intermediates for biofuel production in a consolidated bioprocess. Optimisation of reactor conditions was investigated using five different ruminal inoculum concentrations; 5,10,15,20 and 25% with fixed pH at 6.8 and temperature at 39 ˚C. The ANKOM 200/220 fiber analyser was used to analyse in vitro neutral detergent fiber (NDF) disappearance of the feedstuffs. Fresh and cryo-frozen (5% DMSO and 50% glycerol for 3 months) rumen cultures were tested for the retainment of fermentation capacity and durability in 72 h fermentations in 125 ml serum vials using a FURO medical solutions 6-valve gas manifold to induce anaerobic conditions. Fermentation of apple pomace, triticale straw, and grape pomace showed no significant difference (P > 0.05) in the effect of 15 and 20 % inoculum concentrations for the total VFA yield. However, high performance liquid chromatographic separation within the two inoculum concentrations showed a significant difference (P < 0.05) in acetic acid yield, with 20% inoculum concentration being the optimum at 4.67 g/l. NDF disappearance of 85% in 96 h and total VFA yield of 11.5 g/l in 72 h (A/P ratio = 2.04) for apple pomace entailed that it was the optimal feedstuff for this process. The NDF disappearance and VFA yield of DMSO (82% NDF disappearance and 10.6 g/l VFA) and glycerol (90% NDF disappearance and 11.6 g/l VFA) stored rumen also showed significantly similar degradability of apple pomace with lack of treatment effect differences compared to a fresh rumen control (P > 0.05). The lack of treatment effects was a positive sign in indicating that there was no difference between the stored samples and the fresh rumen control. Retaining of the fermentation capacity within the preserved cultures suggests that its metabolic characteristics were preserved due to resilience and redundancy of the rumen culture. The amount of degradability and VFA yield within a short span was similar to other carboxylate platforms that have longer run times. This study shows that by virtue of faster rates and high extent of degradability, small scale alternatives to bioethanol such as rumen microbiomes and other natural fermenting microbiomes can be employed to enhance the feasibility of biofuels large-scale implementation.

Keywords: agricultural wastes, carboxylate platform, rumen microbiome, volatile fatty acids

Procedia PDF Downloads 129

Authors: Marek Dosbaba

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Within the mining sector, SEM-based Automated Mineralogy (AM) has been the standard application for quickly and efficiently handling mineral processing tasks. Over the last decade, the trend has been to analyze larger numbers of samples, often with a higher level of detail. This has necessitated a shift from interactive sample analysis performed by an operator using a SEM, to an increased reliance on offline processing to analyze and report the data. In response to this trend, TESCAN TIMA Mineral Analyzer is designed to quickly create a virtual copy of the studied samples, thereby preserving all the necessary information. Depending on the selected data acquisition mode, TESCAN TIMA can perform hyperspectral mapping and save an X-ray spectrum for each pixel or segment, respectively. This approach allows the user to browse through elemental distribution maps of all elements detectable by means of energy dispersive spectroscopy. Re-evaluation of the existing data for the presence of previously unconsidered elements is possible without the need to repeat the analysis. Additional tiers of data such as a secondary electron or cathodoluminescence images can also be recorded. To take full advantage of these information-rich datasets, TIMA utilizes a new archiving tool introduced by TESCAN. The dataset size can be reduced for long-term storage and all information can be recovered on-demand in case of renewed interest. TESCAN TIMA is optimized for network storage of its datasets because of the larger data storage capacity of servers compared to local drives, which also allows multiple users to access the data remotely. This goes hand in hand with the support of remote control for the entire data acquisition process. TESCAN also brings a newly extended open-source data format that allows other applications to extract, process and report AM data. This offers the ability to link TIMA data to large databases feeding plant performance dashboards or geometallurgical models. The traditional tabular particle-by-particle or grain-by-grain export process is preserved and can be customized with scripts to include user-defined particle/grain properties.

Keywords: Tescan, electron microscopy, mineralogy, SEM, automated mineralogy, database, TESCAN TIMA, open format, archiving, big data

Procedia PDF Downloads 108

Authors: Uraib Sharaha, Ahmad Salman, Eladio Rodriguez-Diaz, Elad Shufan, Klaris Riesenberg, Irving J. Bigio, Mahmoud Huleihel

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Antimicrobial drugs have an important role in controlling illness associated with infectious diseases in animals and humans. However, the increasing resistance of bacteria to a broad spectrum of commonly used antibiotics has become a global health-care problem. Rapid determination of antimicrobial susceptibility of a clinical isolate is often crucial for the optimal antimicrobial therapy of infected patients and in many cases can save lives. The conventional methods for susceptibility testing like disk diffusion are time-consuming and other method including E-test, genotyping are relatively expensive. Fourier transform infrared (FTIR) microscopy is rapid, safe, and low cost method that was widely and successfully used in different studies for the identification of various biological samples including bacteria. The new modern infrared (IR) spectrometers with high spectral resolution enable measuring unprecedented biochemical information from cells at the molecular level. Moreover, the development of new bioinformatics analyses combined with IR spectroscopy becomes a powerful technique, which enables the detection of structural changes associated with resistivity. The main goal of this study is to evaluate the potential of the FTIR microscopy in tandem with machine learning algorithms for rapid and reliable identification of bacterial susceptibility to antibiotics in time span of few minutes. The bacterial samples, which were identified at the species level by MALDI-TOF and examined for their susceptibility by the routine assay (micro-diffusion discs), are obtained from the bacteriology laboratories in Soroka University Medical Center (SUMC). These samples were examined by FTIR microscopy and analyzed by advanced statistical methods. Our results, based on 550 E.coli samples, were promising and showed that by using infrared spectroscopic technique together with multivariate analysis, it is possible to classify the tested bacteria into sensitive and resistant with success rate higher than 85% for eight different antibiotics. Based on these preliminary results, it is worthwhile to continue developing the FTIR microscopy technique as a rapid and reliable method for identification antibiotic susceptibility.

Keywords: antibiotics, E. coli, FTIR, multivariate analysis, susceptibility

Procedia PDF Downloads 264

Authors: Aurea C. L. Lacerda, Paulo R. H. Moreno, Bruna M. P. Vianna, Cristina H. R. Serra, Airton Martin, André R. Baby, Vladi O. Consiglieri, Telma M. Kaneko

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The modified Franz cell is the most widely used model for in vitro permeation studies, however it still presents some disadvantages. Thus, some alternative methods have been developed such as Skin PAMPA, which is a bio- artificial membrane that has been applied for skin penetration estimation of xenobiotics based on HT permeability model consisting. Skin PAMPA greatest advantage is to carry out more tests, in a fast and inexpensive way. The membrane system mimics the stratum corneum characteristics, which is the primary skin barrier. The barrier properties are given by corneocytes embedded in a multilamellar lipid matrix. This layer is the main penetration route through the paracellular permeation pathway and it consists of a mixture of cholesterol, ceramides, and fatty acids as the dominant components. However, there is no consensus on the membrane composition. The objective of this work was to compare the performance among different bio-artificial membranes for studying the permeation in skin PAMPA system. Material and methods: In order to mimetize the lipid composition`s present in the human stratum corneum six membranes were developed. The membrane composition was equimolar mixture of cholesterol, ceramides 1-O-C18:1, C22, and C20, plus fatty acids C20 and C24. The membrane integrity assay was based on the transport of Brilliant Cresyl Blue, which has a low permeability; and Lucifer Yellow with very poor permeability and should effectively be completely rejected. The membrane characterization was performed using Confocal Laser Raman Spectroscopy, using stabilized laser at 785 nm with 10 second integration time and 2 accumulations. The membrane behaviour results on the PAMPA system were statistically evaluated and all of the compositions have shown integrity and permeability. The confocal Raman spectra were obtained in the region of 800-1200 cm-1 that is associated with the C-C stretches of the carbon scaffold from the stratum corneum lipids showed similar pattern for all the membranes. The ceramides, long chain fatty acids and cholesterol in equimolar ratio permitted to obtain lipid mixtures with self-organization capability, similar to that occurring into the stratum corneum. Conclusion: The artificial biological membranes studied for Skin PAMPA showed to be similar and with comparable properties to the stratum corneum.

Keywords: bio-artificial membranes, comparison, confocal Raman, skin PAMPA

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Authors: Anshuman Srivastava, Shiv Singh, Sheelendra Pratap Singh

Abstract:

A simple, sensitive and effective gas chromatography tandem mass spectrometry (GC-MS/MS) method was developed for simultaneous analysis of multi pesticide residues (organophosphate, organochlorines, synthetic pyrethroids and herbicides) in food commodities using phenolic resin based activated carbon fibers (ACFs) as reversed-dispersive solid phase extraction (r-DSPE) sorbent in modified QuEChERS (Quick Easy Cheap Effective Rugged Safe) method. The acetonitrile-based QuEChERS technique was used for the extraction of the analytes from food matrices followed by sample cleanup with ACFs instead of traditionally used primary secondary amine (PSA). Different physico-chemical characterization techniques such as Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and Brunauer-Emmet-Teller surface area analysis were employed to investigate the engineering and structural properties of ACFs. The recovery of pesticides and herbicides was tested at concentration levels of 0.02 and 0.2 mg/kg in different commodities such as cauliflower, cucumber, banana, apple, wheat and black gram. The recoveries of all twenty-six pesticides and herbicides were found in acceptable limit (70-120%) according to SANCO guideline with relative standard deviation value < 15%. The limit of detection and limit of quantification of the method was in the range of 0.38-3.69 ng/mL and 1.26 -12.19 ng/mL, respectively. In traditional QuEChERS method, PSA used as r-DSPE sorbent plays a vital role in sample clean-up process and demonstrates good recoveries for multiclass pesticides. This study reports that ACFs are better in terms of removal of co-extractives in comparison of PSA without compromising the recoveries of multi pesticides from food matrices. Further, ACF replaces the need of charcoal in addition to the PSA from traditional QuEChERS method which is used to remove pigments. The developed method will be cost effective because the ACFs are significantly cheaper than the PSA. So the proposed modified QuEChERS method is more robust, effective and has better sample cleanup efficiency for multiclass multi pesticide residues analysis in different food matrices such as vegetables, grains and fruits.

Keywords: QuEChERS, activated carbon fibers, primary secondary amine, pesticides, sample preparation, carbon nanomaterials

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