Search results for: ultrafast laser spectroscopy

Authors: Sri Sharath Kulkarni, Pauline Janssen, Alberto Berardi, Bastiaan Dickhoff, Sander van Gessel

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Blending is a common process in the production of pharmaceutical dosage forms where the high shear is used to obtain a homogenous dosage. The shear required can lead to uncontrolled attrition of excipients and affect API’s. This has an impact on the performance of the formulation as this can alter the structure of the mixture. Therefore, it is important to understand the driving mechanisms for attrition. The aim of this study was to increase the fundamental understanding of the attrition behavior of excipients. Attrition behavior of the excipients was evaluated using a high shear blender (Procept Form-8, Zele, Belgium). Twelve pure excipients are tested, with morphologies varying from crystalline (sieved), granulated to spray dried (round to fibrous). Furthermore, materials include lactose, microcrystalline cellulose (MCC), di-calcium phosphate (DCP), and mannitol. The rotational speed of the blender was set at 1370 rpm to have the highest shear with a Froude (Fr) number 9. Varying blending times of 2-10 min were used. Subsequently, after blending, the excipients were analyzed for changes in particle size distribution (PSD). This was determined (n = 3) by dry laser diffraction (Helos/KR, Sympatec, Germany). Attrition was found to be a surface phenomenon which occurs in the first minutes of the high shear blending process. An increase of blending time above 2 mins showed no change in particle size distribution. Material chemistry was identified as a key driver for differences in the attrition behavior between different excipients. This is mainly related to the proneness to fragmentation, which is known to be higher for materials such as DCP and mannitol compared to lactose and MCC. Secondly, morphology also was identified as a driver of the degree of attrition. Granular products consisting of irregular surfaces showed the highest reduction in particle size. This is due to the weak solid bonds created between the primary particles during the granulation process. Granular DCP and mannitol show a reduction of 80-90% in x10(µm) compared to a 20-30% drop for granular lactose (monohydrate and anhydrous). Apart from the granular lactose, all the remaining morphologies of lactose (spray dried-round, sieved-tomahawk, milled) show little change in particle size. Similar observations have been made for spray-dried fibrous MCC. All these morphologies have little irregular or sharp surfaces and thereby are less prone to fragmentation. Therefore, products containing brittle materials such as mannitol and DCP are more prone to fragmentation when exposed to shear. Granular products with irregular surfaces lead to an increase in attrition. While spherical, crystalline, or fibrous morphologies show reduced impact during high shear blending. These changes in size will affect the functionality attributes of the formulation, such as flow, API homogeneity, tableting, formation of dust, etc. Hence it is important for formulators to fully understand the excipients to make the right choices.

Keywords: attrition, blending, continuous manufacturing, excipients, lactose, microcrystalline cellulose, shear

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Authors: Navpreet Kaur, Himkusha Thakur, Nirmal Prabhakar

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One of the most publicized and controversial issue in crop production is the use of agrichemicals- also known as pesticides. This is evident in many reports that Organophosphate (OP) insecticides, among the broad range of pesticides are mainly involved in acute and chronic poisoning cases. Therefore, detection of OPs is very necessary for health protection, food and environmental safety. In our study, a nanocomposite of poly (3,4 ethylenedioxythiophene) (PEDOT) and multi-walled carbon nanotubes (MWCNTs) has been deposited electrochemically onto the surface of fluorine doped tin oxide sheets (FTO) for the analysis of malathion OP. The -COOH functionalization of MWCNTs has been done for the covalent binding with amino groups of AChE enzyme. The use of PEDOT-MWCNT films exhibited an excellent conductivity, enables fast transfer kinetics and provided a favourable biocompatible microenvironment for AChE, for the significant malathion OP detection. The prepared PEDOT-MWCNT/FTO and AChE/PEDOT-MWCNT/FTO nano-biosensors were characterized by Fourier transform infrared spectrometry (FTIR), Field emission-scanning electron microscopy (FE-SEM) and electrochemical studies. Electrochemical studies were done using Cyclic Voltammetry (CV) or Differential Pulse Voltammetry (DPV) and Electrochemical Impedance Spectroscopy (EIS). Various optimization studies were done for different parameters including pH (7.5), AChE concentration (50 mU), substrate concentration (0.3 mM) and inhibition time (10 min). The detection limit for malathion OP was calculated to be 1 fM within the linear range 1 fM to 1 µM. The activity of inhibited AChE enzyme was restored to 98% of its original value by 2-pyridine aldoxime methiodide (2-PAM) (5 mM) treatment for 11 min. The oxime 2-PAM is able to remove malathion from the active site of AChE by means of trans-esterification reaction. The storage stability and reusability of the prepared nano-biosensor is observed to be 30 days and seven times, respectively. The application of the developed nano-biosensor has also been evaluated for spiked lettuce sample. Recoveries of malathion from the spiked lettuce sample ranged between 96-98%. The low detection limit obtained by the developed nano-biosensor made them reliable, sensitive and a low cost process.

Keywords: PEDOT-MWCNT, malathion, organophosphates, acetylcholinesterase, nano-biosensor, oxime (2-PAM)

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Authors: Shiying Fan, Xinyong Li

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The development of highly efficient multifunctional catalytic materials towards HER, ORR and Photo-fuel cell applications in terms of combined electrochemical and photo-electrochemical principles have currently confronted with dire challenges. In this study, novel palladium (Pd) and ruthenium (Ru) Bimetal Quantum Dots (BQDs) co-anchored on Titania nanotube (NTs) arrays electrodes have been successfully constructed by facial two-step electrochemical strategy. Double Schottky junctions with superior performance in electrocatalytic (EC) hydrogen generations and solar fuel cell energy conversions (PE) have been found. Various physicochemical techniques including UV-vis spectroscopy, TEM/EDX/HRTEM, SPV/TRV and electro-chemical strategy including EIS, C-V, I-V, and I-T, etc. were chronically utilized to systematically characterize the crystal-, electronic and micro-interfacial structures of the composites with double Schottky junction, respectively. The characterizations have implied that the marvelous enhancement of separation efficiency of electron-hole pairs generations is mainly caused by the Schottky-barriers within the nanocomposites, which would greatly facilitate the interfacial charge transfer for H₂ generations and solar fuel cell energy conversions. Moreover, the DFT calculations clearly indicated that the oriented growth of Ru and Pd bimetal atoms at the anatase (101) surface is mainly driven by the interaction between Ru/Pd and surface atoms, and the most active site for bimetal Ru and Pd adatoms on the perfect TiO₂ (101) surface is the 2cO-6cTi-3cO bridge sites and the 2cO-bridge sites with the highest adsorption energy of 9.17 eV. Furthermore, the electronic calculations show that in the nanocomposites, the number of impurity (i.e., co-anchored Ru-Pd BQDs) energy levels near Fermi surface increased and some were overlapped with original energy level, promoting electron energy transition and reduces the band gap. Therefore, this work shall provide a deeper insight for the molecular design of Bimetal Quantum Dots (BQDs) assembled onto Tatiana NTs composites with superior performance for electrocatalytic hydrogen productions and solar fuel cell energy conversions (PE) simultaneously.

Keywords: eletrocatalytic, Ru-Pd bimetallic quantum dots, titania nanotube arrays, double Schottky junctions, hydrogen production

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Authors: Sami Khan, Kripa Varanasi

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Corrosion is a widespread problem in several industries and developing surfaces that resist corrosion has been an area of interest since the last several decades. Superhydrophobic surfaces that combine hydrophobic coatings along with surface texture have been shown to improve corrosion resistance by creating voids filled with air that minimize the contact area between the corrosive liquid and the solid surface. However, these air voids can incorporate corrosive liquids over time, and any mechanical faults such as cracks can compromise the coating and provide pathways for corrosion. As such, there is a need for self-healing corrosion-resistance surfaces. In this work, the anti-corrosion properties of textured surfaces impregnated with a lubricant have been systematically studied. Since corrosion resistance depends on the area and physico-chemical properties of the material exposed to the corrosive medium, lubricant-impregnated surfaces (LIS) have been designed based on the surface tension, viscosity and chemistry of the lubricant and its spreading coefficient on the solid. All corrosion experiments were performed in a standard three-electrode cell using iron, which readily corrodes in a 3.5% sodium chloride solution. In order to obtain textured iron surfaces, thin films (~500 nm) of iron were sputter-coated on silicon wafers textured using photolithography, and subsequently impregnated with lubricants. Results show that the corrosion rate on LIS is greatly reduced, and offers an over hundred-fold improvement in corrosion protection. Furthermore, it is found that the spreading characteristics of the lubricant are significant in ensuring corrosion protection: a spreading lubricant (e.g., Krytox 1506) that covers both inside the texture, as well as the top of the texture, provides a two-fold improvement in corrosion protection as compared to a non-spreading lubricant (e.g., Silicone oil) that does not cover texture tops. To enhance corrosion protection of surfaces coated with a non-spreading lubricant, pyramid-shaped textures have been developed that minimize exposure to the corrosive solution, and a consequent twenty-fold increased in corrosion protection is observed. An increase in viscosity of the lubricant scales with greater corrosion protection. Finally, an equivalent cell-circuit model is developed for the lubricant-impregnated systems using electrochemical impedance spectroscopy. Lubricant-impregnated surfaces find attractive applications in harsh corrosive environments, especially where the ability to self-heal is advantageous.

Keywords: lubricant-impregnated surfaces, self-healing surfaces, wettability, nano-engineered surfaces

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Authors: Baha Eddine Aissou, Aichouche Belhadj Aissa

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Light detection and ranging (LiDAR) is an active remote sensing technology used for several applications. Airborne LiDAR is becoming an important technology for the acquisition of a highly accurate dense point cloud. A classification of airborne laser scanning (ALS) point cloud is a very important task that still remains a real challenge for many scientists. Support vector machine (SVM) is one of the most used statistical learning algorithms based on kernels. SVM is a non-parametric method, and it is recommended to be used in cases where the data distribution cannot be well modeled by a standard parametric probability density function. Using a kernel, it performs a robust non-linear classification of samples. Often, the data are rarely linearly separable. SVMs are able to map the data into a higher-dimensional space to become linearly separable, which allows performing all the computations in the original space. This is one of the main reasons that SVMs are well suited for high-dimensional classification problems. Only a few training samples, called support vectors, are required. SVM has also shown its potential to cope with uncertainty in data caused by noise and fluctuation, and it is computationally efficient as compared to several other methods. Such properties are particularly suited for remote sensing classification problems and explain their recent adoption. In this poster, the SVM classification of ALS LiDAR data is proposed. Firstly, connected component analysis is applied for clustering the point cloud. Secondly, the resulting clusters are incorporated in the SVM classifier. Radial basic function (RFB) kernel is used due to the few numbers of parameters (C and γ) that needs to be chosen, which decreases the computation time. In order to optimize the classification rates, the parameters selection is explored. It consists to find the parameters (C and γ) leading to the best overall accuracy using grid search and 5-fold cross-validation. The exploited LiDAR point cloud is provided by the German Society for Photogrammetry, Remote Sensing, and Geoinformation. The ALS data used is characterized by a low density (4-6 points/m²) and is covering an urban area located in residential parts of the city Vaihingen in southern Germany. The class ground and three other classes belonging to roof superstructures are considered, i.e., a total of 4 classes. The training and test sets are selected randomly several times. The obtained results demonstrated that a parameters selection can orient the selection in a restricted interval of (C and γ) that can be further explored but does not systematically lead to the optimal rates. The SVM classifier with hyper-parameters is compared with the most used classifiers in literature for LiDAR data, random forest, AdaBoost, and decision tree. The comparison showed the superiority of the SVM classifier using parameters selection for LiDAR data compared to other classifiers.

Keywords: classification, airborne LiDAR, parameters selection, support vector machine

Procedia PDF Downloads 125

Authors: I. Belyamani, M. K. Hassan, J. U. Otaigbe, W. R. Fielding, K. A. Mauritz, J. S. Wiggins, W. L. Jarrett

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We have investigated the flame-retardant efficiency of special new phosphate glass (P-glass) compositions having different glass transition temperatures (Tg) on the processing conditions of polyamide 6,6 (PA6,6) and the final hybrid flame retardancy (FR). We have showed that the low Tg P glass composition (i.e., ILT 1) is a promising flame retardant for PA6,6 at a concentration of up to 15 wt. % compared to intermediate (IIT 3) and high (IHT 1) Tg P glasses. Cone calorimetry data showed that the ILT 1 decreased both the peak heat release rate and the total heat amount released from the PA6,6/ILT 1 hybrids, resulting in an efficient formation of a glassy char layer. These intriguing findings prompted to address several questions concerning the mechanism of action of the different P glasses studied. The general mechanism of action of phosphorous based FR additives occurs during the combustion stage by enhancing the morphology of the char and the thermal shielding effect. However, the present work shows that P glass based FR additives act during melt processing of PA6,6/P glass hybrids. Dynamic mechanical analysis (DMA) revealed that the Tg of PA6,6/ILT 1 was significantly shifted to a lower Tg (~65 oC) and another transition appeared at high temperature (~ 166 oC), thus indicating a strong interaction between PA6,6 and ILT 1. This was supported by a drop in the melting point and crystallinity of the PA6,6/ILT 1 hybrid material as detected by differential scanning calorimetry (DSC). The dielectric spectroscopic investigation of the networks’ molecular level structural variations (i.e. hybrids chain motion, Tg and sub-Tg relaxations) agreed very well with the DMA and DSC findings; it was found that the three different P glass compositions did not show any effect on the PA6,6 sub-Tg relaxations (related to the NH2 and OH chain end groups motions). Nevertheless, contrary to IIT 3 and IHT 1 based hybrids, the PA6,6/ILT 1 hybrid material showed an evidence of splitting the PA6,6 Tg relaxations into two peaks. Finally, the CPMAS 31P-NMR data confirmed the miscibility between ILT 1 and PA6,6 at the molecular level, as a much larger enhancement in cross-polarization for the PA6,6/15%ILT 1 hybrids was observed. It can be concluded that compounding low Tg P-glass (i.e. ILT 1) with PA6,6 facilitates hydrolytic chain scission of the PA6,6 macromolecules through a potential chemical interaction between phosphate and the alpha-Carbon of the amide bonds of the PA6,6, leading to better flame retardant properties.

Keywords: broadband dielectric spectroscopy, composites, flame retardant, polyamide, phosphate glass, sustainable

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Authors: R. P. Hewawasam, A. F. Dulhunty

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The ryanodine receptor (RyR) is an intracellular ion channel that releases Ca2+ from the sarcoplasmic reticulum and is essential for the excitation-contraction coupling and contraction in striated muscle. Human muscle specific glutathione transferase M2-2 (GSTM2-2) is a highly specific inhibitor of cardiac ryanodine receptor (RyR2) activity. Single channel-lipid bilayer studies and Ca2+ release assays performed using the C-terminal half of the GSTM2-2 and its mutants F157A and Y160A confirmed the ability of the C terminal domain of GSTM2-2 to specifically inhibit the cardiac ryanodine receptor activity. Objective of the present study is to determine the effect of C terminal domain of GSTM2-2 (GSTM2-2C) and the mutants, F157A and Y160A on the Ca2+ transients of neonatal ventricular cardiomyocytes. Primary cardiomyocytes were cultured from neonatal rats. They were treated with GSTM2-2C and the two mutants F157A and Y160A at 15µM and incubated for 2 hours. Then the cells were led with Fluo-4AM, fluorescent Ca2+ indicator, and the field stimulated (1 Hz, 3V and 2ms) cells were excited using the 488 nm argon laser. Contractility of the cells were measured and the Ca2+ transients in the stained cells were imaged using Leica SP5 confocal microscope. Peak amplitude of the Ca2+ transient, rise time and decay time from the peak were measured for each transient. In contrast to GSTM2C which significantly reduced the % shortening (42.8%) in the field stimulated cells, F157A and Y160A failed to reduce the % shortening.Analysis revealed that the average amplitude of the Ca2+ transient was significantly reduced (P<0.001) in cells treated with the wild type GSTM2-2C compared to that of untreated cells. Cells treated with the mutants F157A and Y160A didn’t change the Ca2+ transient significantly compared to the control. A significant increase in the rise time (P< 0.001) and a significant reduction in the decay time (P< 0.001) were observed in cardiomyocytes treated with GSTM2-2C compared to the control but not with F157A and Y160A. These results are consistent with the observation that GSTM2-2C reduced the Ca2+ release from the cardiac SR significantly whereas the mutants, F157A and Y160A didn’t show any effect compared to the control. GSTM2-2C has an isoform-specific effect on the cardiac ryanodine receptor activity and also it inhibits RyR2 channel activity only during diastole. Selective inhibition of RyR2 by GSTM2-2C has significant clinical potential in the treatment of cardiac arrhythmias and heart failure. Since GSTM2-2C-terminal construct has no GST enzyme activity, its introduction to the cardiomyocyte would not exert any unwanted side effects that may alter its enzymatic action. The present study further confirms that GSTM2-2C is capable of decreasing the Ca2+ release from the cardiac SR during diastole. These results raise the future possibility of using GSTM2-2C as a template for therapeutics that can depress RyR2 function when the channel is hyperactive in cardiac arrhythmias and heart failure.

Keywords: arrhythmia, cardiac muscle, cardiac ryanodine receptor, GSTM2-2

Procedia PDF Downloads 267

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: Abdulaziz Bashir Kutawa1, 2, *, Khairulmazmi Ahmad 1, 3, Mohd Zobir Hussein 4, Asgar Ali 5, * Mohd Aswad Abdul Wahab1, Amara Rafi3, Mahesh Tiran Gunasena1, 6, Muhammad Ziaur Rahman1, 7, Md Imam Hossain1, And Syazwan Afif Mohd Zobir1

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Various abiotic and biotic stresses have an impact on rice production all around the world. The most serious and prevalent disease in rice plants, known as rice blast, is one of the major obstacles to the production of rice. It is one of the diseases that has the greatest negative effects on rice farming globally, the disease is caused by a fungus called Magnaporthe grisae. Since nanoparticles were shown to have an inhibitory impact on certain types of fungus, nanotechnology is a novel notion to enhance agriculture by battling plant diseases. Utilizing nanocarrier systems enables the active chemicals to be absorbed, attached, and encapsulated to produce efficient nanodelivery formulations. The objectives of this research work were to determine the efficacy and mode of action of the nanofungicides (in-vitro) and in field conditions (in-vivo). Ionic gelation method was used in the development of the nanofungicides. Using the poisoned media method, the synthesized agronanofungicides' in-vitro antifungal activity was assessed against M. grisae. The potato dextrose agar (PDA) was amended in several concentrations; 0.001, 0.005, 0.01, 0.025, 0.05, 0.1, 0.15, 0.20, 0.25, 0.30, and 0.35 ppm for the nanofungicides. Medium with the only solvent served as a control. Every day, mycelial growth was measured, and PIRG (percentage inhibition of radial growth) was also computed. Every day, mycelial growth was measured, and PIRG (percentage inhibition of radial growth) was also computed. Based on the results of the zone of inhibition, the chitosan-hexaconazole agronanofungicide (2g/mL) was the most effective fungicide to inhibit the growth of the fungus with 100% inhibition at 0.2, 0.25, 0.30, and 0.35 ppm, respectively. Then followed by carbendazim analytical fungicide that inhibited the growth of the fungus (100%) at 5, 10, 25, 50, and 100 ppm, respectively. The least were found to be propiconazole and basamid fungicides with 100% inhibition only at 100 ppm. The scanning electron microscope (SEM), confocal laser scanning microscope (CLSM), and transmission electron microscope (TEM) were used to study the mechanisms of action of the M. grisae fungal cells. The results showed that both carbendazim, chitosan-hexaconazole, and HXE were found to be the most effective fungicides in disrupting the mycelia of the fungus, and internal structures of the fungal cells. The results of the field assessment showed that the CHDEN treatment (5g/L, double dosage) was found to be the most effective fungicide to reduce the intensity of the rice blast disease with DSI of 17.56%, lesion length (0.43 cm), DR of 82.44%, AUDPC of 260.54 Unit2, and PI of 65.33%, respectively. The least treatment was found to be chitosan-hexaconazole-dazomet (2.5g/L, MIC). The usage of CHDEN and CHEN nanofungicides will significantly assist in lessening the severity of rice blast in the fields, increasing output and profit for rice farmers.

Keywords: chitosan, hexaconazole, disease incidence, and magnaporthe grisae

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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

Procedia PDF Downloads 279

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: L. Le Priol, A. Nesterenko, K. El Kirat, K. Saleh

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Introduction and objectives: Polyunsaturated fatty acids (PUFAs) omega-3 and omega-6 are widely recognized as being beneficial to the health and normal growth. Unfortunately, due to their highly unsaturated nature, these molecules are sensitive to oxidation and thermic degradation leading to the production of toxic compounds and unpleasant flavors and smells. Hence, it is necessary to find out a suitable way to protect them. Microencapsulation by spray-drying is a low-cost encapsulation technology and most commonly used in the food industry. Many compounds can be used as wall materials, but there is a growing interest in the use of biopolymers, such as proteins and polysaccharides, over the last years. The objective of this study is to increase the oxidative stability of sunflower oil by microencapsulation in plant protein matrices using spray-drying technique. Material and methods: Sunflower oil was used as a model substance for oxidable food oils. Proteins from brown rice, hemp, pea, soy and sunflower seeds were used as emulsifiers and microencapsulation wall materials. First, the proteins were solubilized in distilled water. Then, the emulsions were pre-homogenized using a high-speed homogenizer (Ultra-Turrax) and stabilized by using a high-pressure homogenizer (HHP). Drying of the emulsion was performed in a Mini Spray Dryer. The oxidative stability of the encapsulated oil was determined by performing accelerated oxidation tests with a Rancimat. The size of the microparticles was measured using a laser diffraction analyzer. The morphology of the spray-dried microparticles was acquired using environmental scanning microscopy. Results: Pure sunflower oil was used as a reference material. Its induction time was 9.5 ± 0.1 h. The microencapsulation of sunflower oil in pea and soy protein matrices significantly improved its oxidative stability with induction times of 21.3 ± 0.4 h and 12.5 ± 0.4 h respectively. The encapsulation with hemp proteins did not significantly change the oxidative stability of the encapsulated oil. Sunflower and brown rice proteins were ineffective materials for this application, with induction times of 7.2 ± 0.2 h and 7.0 ± 0.1 h respectively. The volume mean diameter of the microparticles formulated with soy and pea proteins were 8.9 ± 0.1 µm and 16.3 ± 1.2 µm respectively. The values for hemp, sunflower and brown rice proteins could not be obtained due to the agglomeration of the microparticles. ESEM images showed smooth and round microparticles with soy and pea proteins. The surfaces of the microparticles obtained with sunflower and hemp proteins were porous. The surface was rough when brown rice proteins were used as the encapsulating agent. Conclusion: Soy and pea proteins appeared to be efficient wall materials for the microencapsulation of sunflower oil by spray drying. These results were partly explained by the higher solubility of soy and pea proteins in water compared to hemp, sunflower, and brown rice proteins. Acknowledgment: This work has been performed, in partnership with the SAS PIVERT, within the frame of the French Institute for the Energy Transition (Institut pour la Transition Energétique (ITE)) P.I.V.E.R.T. (www.institut-pivert.com) selected as an Investments for the Future (Investissements d’Avenir). This work was supported, as part of the Investments for the Future, by the French Government under the reference ANR-001-01.

Keywords: biopolymer, edible oil, microencapsulation, oxidative stability, release, spray-drying

Procedia PDF Downloads 115

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

Procedia PDF Downloads 275

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

Procedia PDF Downloads 248

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

Procedia PDF Downloads 208

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

Procedia PDF Downloads 98

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

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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

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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

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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 156

Authors: Maja Benkovic, Dubravka Novotni, Bojana Voucko, Duska Curic, Damir Jezek, Nikolina Cukelj

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Cryo-grinding is an ultra-fine grinding method used in the pharmaceutical industry, production of herbs and spices and in the production and handling of cereals, due to its ability to produce powders with small particle sizes which maintain their favorable bioactive profile. The aim of this study was to determine the particle size distributions of the proso millet (Panicum miliaceum) bran fraction grinded at cryogenic temperature (using liquid nitrogen (LN₂) cooling, T = - 196 °C), in comparison to non-cooled grinding. Proso millet bran is primarily used as an animal feed, but has a potential in food applications, either as a substrate for extraction of bioactive compounds or raw material in the bakery industry. For both applications finer particle sizes of the bran could be beneficial. Thus, millet bran was ground for 2, 4, 8 and 12 minutes using the ball mill (CryoMill, Retsch GmbH, Haan, Germany) at three grinding modes: (I) without cooling, (II) at cryo-temperature, and (III) at cryo-temperature with included 1 minute of intermediate cryo-cooling step after every 2 minutes of grinding, which is usually applied when samples require longer grinding times. The sample was placed in a 50 mL stainless steel jar containing one grinding ball (Ø 25 mm). The oscillation frequency in all three modes was 30 Hz. Particle size distributions of the bran were determined by a laser diffraction particle sizing method (Mastersizer 2000) using the Scirocco 2000 dry dispersion unit (Malvern Instruments, Malvern, UK). Three main effects of the grinding set-up were visible from the results. Firstly, grinding time at all three modes had a significant effect on all particle size parameters: d(0.1), d(0.5), d(0.9), D[3,2], D[4,3], span and specific surface area. Longer grinding times resulted in lower values of the above-listed parameters, e.g. the averaged d(0.5) of the sample (229.57±1.46 µm) dropped to 51.29±1.28 µm after 2 minutes grinding without LN₂, and additionally to 43.00±1.33 µm after 4 minutes of grinding without LN₂. The only exception was the sample ground for 12 minutes without cooling, where an increase in particle diameters occurred (d(0.5)=62.85±2.20 µm), probably due to particles adhering to one another and forming larger particle clusters. Secondly, samples with LN₂ cooling exhibited lower diameters in comparison to non-cooled. For example, after 8 minutes of non-cooled grinding d(0.5)=46.97±1.05 µm was achieved, while the LN₂ cooling enabled collection of particles with average sizes of d(0.5)=18.57±0.18 µm. Thirdly, the application of intermediate cryo-cooling step resulted in similar particle diameters (d(0.5)=15.83±0.36 µm, 12 min of grinding) as cryo-milling without this step (d(0.5)=16.33±2.09 µm, 12 min of grinding). This indicates that intermediate cooling is not necessary for the current application, which consequently reduces the consumption of LN₂. These results point out the potential beneficial effects of millet bran grinding at cryo-temperatures. Further research will show if the lower particle size achieved in comparison to non-cooled grinding could result in increased bioavailability of bioactive compounds, as well as protein digestibility and solubility of dietary fibers of the proso millet bran fraction.

Keywords: ball mill, cryo-milling, particle size distribution, proso millet (Panicum miliaceum) bran

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Authors: Poojan Gharat, Haridas Pal, Sharmistha Dutta Choudhury

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Tuning photophysical properties of guest dyes through host-guest interactions involving macrocyclic hosts are the attractive research areas since past few decades, as these changes can directly be implemented in chemical sensing, molecular recognition, fluorescence imaging and dye laser applications. Excited state intramolecular proton transfer (ESIPT) is an intramolecular prototautomerization process display by some specific dyes. The process is quite amenable to tunability by the presence of different macrocyclic hosts. The present study explores the interesting effect of p-sulfonatocalix[n]arene (SCXn) and cyclodextrin (CD) hosts on the excited-state prototautomeric equilibrium of Chrysazine (CZ), a model antitumour drug. CZ exists exclusively in its normal form (N) in the ground state. However, in the excited state, the excited N* form undergoes ESIPT along with its pre-existing intramolecular hydrogen bonds, giving the excited state prototautomer (T*). Accordingly, CZ shows a single absorption band due to N form, but two emission bands due to N* and T* forms. Facile prototautomerization of CZ is considerably inhibited when the dye gets bound to SCXn hosts. However, in spite of lower binding affinity, the inhibition is more profound with SCX6 host as compared to SCX4 host. For CD-CZ system, while prototautomerization process is hindered by the presence of β-CD, it remains unaffected in the presence of γCD. Reduction in the prototautomerization process of CZ by SCXn and βCD hosts is unusual, because T* form is less dipolar in nature than the N*, hence binding of CZ within relatively hydrophobic hosts cavities should have enhanced the prototautomerization process. At the same time, considering the similar chemical nature of two CD hosts, their effect on prototautomerization process of CZ would have also been similar. The atypical effects on the prototautomerization process of CZ by the studied hosts are suggested to arise due to the partial inclusion or external binding of CZ with the hosts. As a result, there is a strong possibility of intermolecular H-bonding interaction between CZ dye and the functional groups present at the portals of SCXn and βCD hosts. Formation of these intermolecular H-bonds effectively causes the pre-existing intramolecular H-bonding network within CZ molecule to become weak, and this consequently reduces the prototautomerization process for the dye. Our results suggest that rather than the binding affinity between the dye and host, it is the orientation of CZ in the case of SCXn-CZ complexes and the binding stoichiometry in the case of CD-CZ complexes that play the predominant role in influencing the prototautomeric equilibrium of the dye CZ. In the case of SCXn-CZ complexes, the results obtained through experimental findings are well supported by quantum chemical calculations. Similarly for CD-CZ systems, binding stoichiometries obtained through geometry optimization studies on the complexes between CZ and CD hosts correlate nicely with the experimental results. Formation of βCD-CZ complexes with 1:1 stoichiometry while formation of γCD-CZ complexes with 1:1, 1:2 and 2:2 stoichiometries are revealed from geometry optimization studies and these results are in good accordance with the observed effects by the βCD and γCD hosts on the ESIPT process of CZ dye.

Keywords: intermolecular proton transfer, macrocyclic hosts, quantum chemical studies, photophysical studies

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Authors: O. Gsib, U. Peirera, C. Egles, S. A. Bencherif

Abstract:

In skin regenerative medicine, one of the critical issues is to produce a three-dimensional scaffold with optimized porosity for dermal fibroblast infiltration and neovascularization, which exhibits high mechanical properties and displays sufficient wound healing characteristics. In this study, we report on the synthesis and characterization of macroporous sequential interpenetrating polymer networks (IPNs) combining skin wound healing properties of fibrin with the excellent physical properties of polyethylene glycol (PEG). Fibrin fibers serve as a provisional biologically active network to promote cell adhesion and proliferation while PEG provides the mechanical stability to maintain the entire 3D construct. After having modified both PEG and Serum Albumin (used for promoting enzymatic degradability) by adding methacrylate residues (PEGDM and SAM, respectively), Fibrin/PEGDM-SAM sequential IPNs were synthesized as follows: Macroporous sponges were first produced from PEGDM-SAM hydrogels by a freeze-drying technique and then rehydrated by adding the fibrin precursors. Environmental Scanning Electron Microscopy (ESEM) and Confocal Laser Scanning Microscopy (CLSM) were used to characterize their microstructure. Human dermal fibroblasts were cultivated during one week in the constructs and different cell culture parameters (viability, morphology, proliferation) were evaluated. Subcutaneous implantations of the scaffolds were conducted on five-week old male nude mice to investigate their biocompatibility in vivo. We successfully synthesized interconnected and macroporous Fibrin/PEGDM-SAM sequential IPNs. The viability of primary dermal fibroblasts was well maintained (above 90%) after 2 days of culture. Cells were able to adhere, spread and proliferate in the scaffolds suggesting the suitable porosity and intrinsic biologic properties of the constructs. The fibrin network adopted a spider web shape that covered partially the pores allowing easier cell infiltration into the macroporous structure. To further characterize the in vitro cell behavior, cell proliferation (EdU incorporation, MTS assay) is being studied. Preliminary histological analysis of animal studies indicated the persistence of hydrogels even after one-month post implantation and confirmed the absence of inflammation response, good biocompatibility and biointegration of our scaffolds within the surrounding tissues. These results suggest that our Fibrin/PEGDM-SAM IPNs could be considered as potential candidates for dermis regenerative medicine. Histological analysis will be completed to further assess scaffold remodeling including de novo extracellular matrix protein synthesis and early stage angiogenesis analysis. Compression measurements will be conducted to investigate the mechanical properties.

Keywords: fibrin, hydrogels for dermal reconstruction, polyethylene glycol, semi-interpenetrating polymer network

Procedia PDF Downloads 208

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

Abstract:

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 550

Authors: Saad Mohamed Elsaid Onaizah

Abstract:

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 43