Search results for: electro-chemical kinetics

Authors: Abidullah, Basharat Hussain, Jong Seok Kim

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Polymer electrolyte membrane fuel cell (PEMFC) is an electrochemical cell, which undergoes an oxygen reduction reaction to produce electrical energy. Platinum (Pt) metal has been used as a catalyst since its inception, but expensiveness is the major obstacle in the commercialization of fuel cells. Herein a non-precious group metal (NPGM) is employed instead of Pt to reduce the cost of PEMFCs. Manganese dioxide impregnated carbon nanotubes (MnO₂-CNTs composite) is a catalyst having excellent electrochemical properties and offers a better alternative to the Platinum-based PEMFC. The catalyst is synthesized by impregnating the transition metal on large surface carbonaceous CNTs by hydrothermal synthesis techniques. To enhance the catalytic activity and increase the volumetric current density, the sample was pyrolyzed at 800ᵒC under a nitrogen atmosphere. During pyrolysis, the nitrogen was doped in the framework of CNTs. Then the material was treated with acid for removing the unreacted metals and adding oxygen functional group to the CNT framework. This process ameliorates the catalytic activity of the manganese-based catalyst. The catalyst has been characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and the catalyst activity has been examined by rotating disc electrode (RDE) experiment. The catalyst was strong enough to withstand an austere alkaline environment in experimental conditions and had a high electrocatalytic activity for oxygen reduction reaction (ORR). Linear Sweep Voltammetry (LSV) depicts an excellent current density of -4.0 mA/cm² and an overpotential of -0.3V vs. standard calomel electrode (SCE) in 0.1M KOH electrolyte. Rotating disk electrode (RDE) was conducted at 400, 800, 1200, and 1600 rpm. The catalyst exhibited a higher methanol tolerance and long term durability with respect to commercial Pt/C. The results for MnO₂-CNT show that the low-cost catalyst will supplant the expensive Pt/C catalyst in the fuel cell.

Keywords: carbon nanotubes, methanol fuel cell, oxygen reduction reaction, MnO₂-CNTs

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Authors: Dileep Maarisetty, Janaki Komandur, Saroj S. Baral

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In the current work, photocatalytic degradation of phenol was carried both in UV and visible light to find the slowest step that is limiting the rate of photo-degradation process. Characterization such as XRD, SEM, FT-IR, TEM, XPS, UV-DRS, PL, BET, UPS, ESR and zeta potential experiments were conducted to assess the credibility of catalysts in boosting the photocatalytic activity. To explore the synergy, TiO₂ was doped with graphene and alumina. The orbital hybridization with alumina doping (mediated by graphene) resulted in higher electron transfer from the conduction band of TiO₂ to alumina surface where oxygen reduction reactions (ORR) occur. Besides, the doping of alumina and graphene introduced defects into Ti lattice and helped in improving the adsorptive properties of modified photo-catalyst. Results showed that these defects promoted the oxygen reduction reactions (ORR) on the catalyst’s surface. ORR activity aims at producing reactive oxygen species (ROS). These ROS species oxidizes the phenol molecules which is adsorbed on the surface of photo-catalysts, thereby driving the photocatalytic reactions. Since mass transfer is considered as rate limiting step, various mathematical models were applied to the experimental data to probe the best fit. By varying the parameters, it was found that intra-particle diffusion was the slowest step in the degradation process. Lagergren model gave the best R² values indicating the nature of rate kinetics. Similarly, different adsorption isotherms were employed and realized that Langmuir isotherm suits the best with tremendous increase in uptake capacity (mg/g) of TiO₂-rGO-Al₂O₃ as compared undoped TiO₂. This further assisted in higher adsorption of phenol molecules. The results obtained from experimental, kinetic modelling and adsorption isotherms; it is concluded that apart from changes in surface, optoelectronic and morphological properties that enhanced the photocatalytic activity, the intra-particle diffusion within the catalyst’s pores serve as rate-limiting step in deciding the fate of photo-catalytic degradation of phenol.

Keywords: ORR, phenol degradation, photo-catalyst, rate kinetics

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Authors: J. Tirano, H. Zea, C. Luhrs

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Photocatalysis has established as viable option in the development of processes for the treatment of pollutants and clean energy production. This option is based on the ability of semiconductors to generate an electron flow by means of the interaction with solar radiation. Owing to its electronic structure, TiO₂ is the most frequently used semiconductors in photocatalysis, although it has a high recombination of photogenerated charges and low solar energy absorption. An alternative to reduce these limitations is the use of nanostructured morphologies which can be produced during the synthesis of TiO₂ nanotubes (TNTs). Therefore, if possible to produce vertically oriented nanostructures it will be possible to generate a greater contact area with electrolyte and better charge transfer. At present, however, the development of these innovative structures still presents an important challenge for the development of competitive photoelectrochemical devices. This research focuses on established correlations between synthesis variables and 1D nanostructure morphology which has a direct effect on the photocatalytic performance. TNTs with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C-550 °C. Morphology and crystalline phase of the TNTs were carried out by SEM, EDS and XRD analysis. As results, the synthesis conditions were established to produce nanostructures with specific morphological characteristics. Anatase was the predominant phase of TNTs after thermal treatment. Nanotubes with 10 μm in length, 40 nm in pore diameter and a surface-volume ratio of 50 are important in photoelectrochemical applications based on TiO₂ due to their 1D characteristics, high surface-volume ratio, reduced radial dimensions and high oxide/electrolyte interface. Finally, this knowledge can be used to improve the photocatalytic activity of TNTs by making additional surface modifications with dopants that improve their efficiency.

Keywords: electrochemical anodization, morphology, self-organized nanotubes, TiO₂ nanotubes

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Authors: Seungmin Shin, Jin-Baek Kim

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Hematite (α-Fe2O3) has very good semiconducting properties with a band gap of 2.1 eV and is antiferromagnetic. Due to its electrochemical stability, low toxicity, wide abundance, and low-cost, hematite, it is a particularly attractive material for photoelectrochemical cells. Additionally, hematite has also found applications in gas sensing, field emission, heterogeneous catalysis, and lithium-ion battery electrodes. Here, we discovered a new universal top-down method for the synthesis of one-dimensional hematite nanowire arrays. Various shapes and lengths of hematite nanowire have been easily fabricated over large areas by sequential processes. The obtained hematite nanowire arrays are promising candidates as photoanodes in photoelectrochemical solar cells.

Keywords: hematite, lithography, nanowire, top-down process

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Authors: Y. El Kaissi, M. Allam, A. Koulou, M. Galai, M. Ebn Touhami

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The aim of our work is to develop an industrial bath of nickel alloy deposit on mild steel. The optimization of the operating parameters made it possible to obtain a stable Ni-P alloy deposition formulation. To understand the reaction mechanism of the deposition process, a kinetic study was performed by cyclic voltammetry and by electrochemical impedance spectroscopy (EIS). The coatings obtained have a very high corrosion resistance in a very aggressive acid medium which increases with the heat treatment.

Keywords: cyclic voltammetry, EIS, electroless Ni–P coating, heat treatment, potentiodynamic polarization

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Authors: Abdullah Faqihi, John Hedley

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Biosensors play a significant role in the healthcare sectors, scientific and technological progress. Developing electrodes that are easy to manufacture and deliver better electrochemical performance is advantageous for diagnostics and biosensing. They can be implemented extensively in various analytical tasks such as drug discovery, food safety, medical diagnostics, process controls, security and defence, in addition to environmental monitoring. Development of biosensors aims to create high-performance electrochemical electrodes for diagnostics and biosensing. A biosensor is a device that inspects the biological and chemical reactions generated by the biological sample. A biosensor carries out biological detection via a linked transducer and transmits the biological response into an electrical signal; stability, selectivity, and sensitivity are the dynamic and static characteristics that affect and dictate the quality and performance of biosensors. In this research, a developed experimental study for laser scribing technique for graphene oxide inside a vacuum chamber for processing of graphene oxide is presented. The processing of graphene oxide (GO) was achieved using the laser scribing technique. The effect of the laser scribing on the reduction of GO was investigated under two conditions: atmosphere and vacuum. GO solvent was coated onto a LightScribe DVD. The laser scribing technique was applied to reduce GO layers to generate rGO. The micro-details for the morphological structures of rGO and GO were visualised using scanning electron microscopy (SEM) and Raman spectroscopy so that they could be examined. The first electrode was a traditional graphene-based electrode model, made under normal atmospheric conditions, whereas the second model was a developed graphene electrode fabricated under a vacuum state using a vacuum chamber. The purpose was to control the vacuum conditions, such as the air pressure and the temperature during the fabrication process. The parameters to be assessed include the layer thickness and the continuous environment. Results presented show high accuracy and repeatability achieving low cost productivity.

Keywords: laser scribing, lightscribe DVD, graphene oxide, scanning electron microscopy

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Authors: Seema Kothari, Dinesh Panday

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An observed correlation of the reaction rates with the changes in the nature of substituent present on one of the reactants often reveals the nature of transition state. Selective oxidation of organic compounds under non-aqueous media is an important transformation in synthetic organic chemistry. Inorganic chromates and dichromates being drastic oxidant and are generally insoluble in most organic solvents, a number of different chromium (VI) derivatives have been synthesized. Benzimidazolium dichromate (BIDC) is one of the recently reported Cr(VI) reagents which is neither hygroscopic nor light sensitive being, therefore, much stable. Not many reports on the kinetics of the oxidations by BIDC are seemed to be available in the literature. In the present investigation, the kinetics and mechanism of benzyl alcohol (BA) and a number of para- and meta-substituted benzyl alcohols by benzimidazolium dichromate (BIDC), in dimethyl sulphoxide, is reported. The reactions were followed spectrophotometrically at 364 nm by monitoring the decrease in [BIDC] for up to 85-90% reaction, the temperature being constant. The observed oxidation product is the corresponding benzaldehyde. The reactions were of first order with respect to each the alcohol and BIDC. The reactions are catalyzed by proton, and the dependence is of the form: kobs = a + b[H+]. The reactions thus follow both, an acid-dependent and acid-independent paths. The oxidation of [1,1 2H2]benzyl alcohol exhibited the presence of a substantial kinetic isotope effect ( kH/kD = 6.20 at 298 K ). This indicated the cleavage of a α-C-H bond in the rate-determining step. An analysis of the temperature dependence of the deuterium isotope effect showed that the loss of hydrogen proceeds through a concerted cyclic process. The rate of oxidation of BA was determined in 19 organic solvents. An analysis of the solvent effect by Swain’s equation indicated that though both the anion and cation-solvating powers of the solvent contribute to the observed solvent effect, the role of cation-solvation is major. The rates of the para and meta compounds, at 298 K, failed to exhibit a significant correlation in terms of Hammett or Brown's substituent constants. The rates were then subjected to analyses in terms of dual substituent parameter (DSP) equations. The rates of oxidation of the para-substituted benzyl alcohols show an excellent correlation with Taft's σI and σRBA values. However, the rates for the meta-substituted benzyl alcohols show an excellent correlation with σI and σR0. The polar reaction constants are negative indicating an electron-deficient transition state. Hence the overall mechanism is proposed to involve the formation of a chromate ester in a fast pre-equilibrium and then a decomposition of the ester in a subsequent slow step via a cyclic concerted symmetrical transition state, involving hydride-ion transfer, leading to the product. The first order dependence on alcohol may be accounted in terms of the small value of the formation constant of the ester intermediate. An another reaction mechanism accounting the acid-catalysis involve the formation of a protonated BIDC prior to formation of an ester intermediate which subsequently decomposes in a slow step leading to the product.

Keywords: benzimidazolium dichromate, benzyl alcohols, correlation analysis, kinetics, oxidation

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Authors: Rekha M. Y., Punith Kumar, Anshul Kamboj, Chandan Srivastava

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Coatings plays an important role in providing protection for a substrate and in improving the surface quality. Graphene/graphene oxide (GO) using in coating systems provides an environmental friendly solution towards protection against corrosion. Issues such as, lack of scale, high cost, low quality limits the practical application of graphene/GO as corrosion resistant coating material. One other way to employ these materials for corrosion protection is to incorporate them into coatings that are conventionally used for corrosion protection. Due to the extraordinary properties of graphene/GO, it has been demonstrated that the coatings containing graphene/GO are more corrosion resistant than pure metal/alloy coatings. In the present work, Cr-graphene and SnZn-GO composite coatings were investigated in enhancing the corrosion resistant property when compared to pure Cr coating and pure SnZn coating respectively. All the coatings were electrodeposited over mild-steel substrate. Graphene and GO were synthesized by electrochemical exfoliation method and modified Hummers’ method respectively. In Cr coatings, the microstructural study revealed that the addition of formic acid in the coatings reduced the number of cracks in the coatings. Further addition of graphene in Cr coating enhanced the Cr coating’s morphology. Chemically synthesized ZnO nanoparticles were also embedded in the as-deposited Cr and Cr-graphene coatings to enhance the adhesion of the coating, to improve the surface finish and to increase the corrosion resistant property of the coatings. Diffraction analysis revealed that the addition of graphene also altered the texture of the Cr coatings. In SnZn alloy coatings, the morphological and topographical characterization revealed that the relative smoothness and compactness of the coatings increased with increase in the addition of GO in the coatings. The microstructural investigation revealed large-scale segregation of Zn-rich and Sn-rich phases in the pure SnZn coating. However, in SnZn-GO composite coating the uniform distribution of Zn phase in the Sn-rich matrix was observed. This distribution caused the early and uniform formation of ZnO, which is the corrosion product, yielding better corrosion resistance for the SnZn-GO composite coatings as compared to pure SnZn coating. A significant improvement in corrosion resistance in terms of reduction in corrosion current and corrosion rate and increase in the polarization resistance was observed in Cr coating containing graphene and in SnZn coatings containing GO.

Keywords: coatings, corrosion, electrodeposition, graphene, graphene-oxide

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Authors: Malory Beaujolais

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Chlordecone is an organochlorine pesticide with a bishomocubane structure which led to high stability in organic matter. Microbial fuel cell is a type of electrochemical system that can convert organic matters into electricity thanks to electroactive bacteria. This technique has been used with mangrove swamp from Martinique to try to reduce chlordecone rates. Those experiments led to characterize the behavior of the electroactive biofilm formed at the cathode, without added redox mediator. The designed bioelectrochemical system seems to provide the necessary conditions for chlordecone degradation.

Keywords: bioelectrochemistry, bioremediation, chlordecone, mangrove swamp

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Authors: Neumoin Anton Ivanovich, Opra Denis Pavlovich

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Materials based on titanium oxide compounds are widely used in such areas as solar energy, photocatalysis, food industry and hygiene products, biomedical technologies, etc. Demand for them has also formed in the battery industry (an example of this is the commercialization of Li4Ti5O12), where much attention has recently been paid to the development of next-generation systems and technologies, such as sodium-ion batteries. This dictates the need to search for new materials with improved characteristics, as well as ways to obtain them that meet the requirements of scalability. One of the ways to solve these problems can be the creation of nanomaterials that often have a complex of physicochemical properties that radically differ from the characteristics of their counterparts in the micro- or macroscopic state. At the same time, it is important to control the texture (specific surface area, porosity) of such materials. In view of the above, among other methods, the hydrothermal technique seems to be suitable, allowing a wide range of control over the conditions of synthesis. In the present study, a method was developed for the preparation of mesoporous nanostructured sodium trititanate (Na2Ti3O7) with a hierarchical architecture. The materials were synthesized by hydrothermal processing and exhibit a complex hierarchically organized two-layer architecture. At the first level of the hierarchy, materials are represented by particles having a roughness surface, and at the second level, by one-dimensional nanotubes. The products were found to have high specific surface area and porosity with a narrow pore size distribution (about 6 nm). As it is known, the specific surface area and porosity are important characteristics of functional materials, which largely determine the possibilities and directions of their practical application. Electrochemical impedance spectroscopy data show that the resulting sodium trititanate has a sufficiently high electrical conductivity. As expected, the synthesized complexly organized nanoarchitecture based on sodium trititanate with a porous structure can be practically in demand, for example, in the field of new generation electrochemical storage and energy conversion devices.

Keywords: sodium trititanate, hierarchical materials, mesoporosity, nanotubes, hydrothermal synthesis

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Authors: L. Bazzi, E. Azzouyahar, A. Lamiri, M. Essahli

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Effect of addition of linseed oil (LSO) on the corrosion of aluminium in 0.1 M Na2CO3 has been studied by weight loss measurements, potentiodynamic polarization and Electrochemical Impedance Spectroscopy (EIS) measurements. The inhibition efficiency was found to increase with inhibitor content to attain 70% for LSO at 4g/L. Inhibition efficiency E (%) obtained from the various methods is in good agreement. The temperature effect on the corrosion behavior of aluminium was studied by potentiodynamic technique in the range from 298 to 308 K.

Keywords: aluminum, corrosion, green inhibitors, carbonate, linseed oil

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Authors: Umar Hayatu Sidik

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Application of liquid base petroleum fuel (petrol and diesel) for transportation fuel causes emissions of greenhouse gases (GHGs), while natural gas (NG) reduces the emissions of greenhouse gases (GHGs). At present, compression and liquefaction are the most matured technology used for transportation system. For transportation use, compression requires high pressure (200–300 bar) while liquefaction is impractical. A relatively low pressure of 30-40 bar is achievable by adsorbed natural gas (ANG) to store nearly compressed natural gas (CNG). In this study, adsorbents for high-pressure adsorption of methane (CH4) was prepared from coconut shells and polyetheretherketone (PEEK) using potassium hydroxide (KOH) and microwave-assisted activation. Design expert software version 7.1.6 was used for optimization and prediction of preparation conditions of the adsorbents for CH₄ adsorption. Effects of microwave power, activation time and quantity of PEEK on the adsorbents performance toward CH₄ adsorption was investigated. The adsorbents were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric (TG) and derivative thermogravimetric (DTG) and scanning electron microscopy (SEM). The ideal CH4 adsorption capacities of adsorbents were determined using volumetric method at pressures of 5, 17, and 35 bar at an ambient temperature and 5 oC respectively. Isotherm and kinetics models were used to validate the experimental results. The optimum preparation conditions were found to be 15 wt% amount of PEEK, 3 minutes activation time and 300 W microwave power. The highest CH4 uptake of 9.7045 mmol CH4 adsorbed/g adsorbent was recorded by M33P15 (300 W of microwave power, 3 min activation time and 15 wt% amount of PEEK) among the sorbents at an ambient temperature and 35 bar. The CH4 equilibrium data is well correlated with Sips, Toth, Freundlich and Langmuir. Isotherms revealed that the Sips isotherm has the best fit, while the kinetics studies revealed that the pseudo-second-order kinetic model best describes the adsorption process. In all scenarios studied, a decrease in temperature led to an increase in adsorption of both gases. The adsorbent (M33P15) maintained its stability even after seven adsorption/desorption cycles. The findings revealed the potential of coconut shell-PEEK as CH₄ adsorbents.

Keywords: adsorption, desorption, activated carbon, coconut shells, polyetheretherketone

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Authors: Mihaela Beregoi, Horia Iovu, Cristina Busuioc, Alexandru Evanghelidis, Elena Matei, Monica Enculescu, Ionut Enculescu

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Nanomaterials field is very attractive for all researchers who are attempting to develop new devices with the same or improved properties than the micro-sized ones, while reducing the reagents and power consumptions. In this way, a wide range of nanomaterials were fabricated and integrated in applications for electronics, optoelectronics, solar cells, tissue reconstruction and drug delivery. Obviously, the most appealing ones are those dedicated to the medical domain. Different types of nano-sized materials, such as particles, fibers, films etc., can be synthesized by using physical, chemical or electrochemical methods. One of these techniques is electrospinning, which enable the production of fibers with nanometric dimensions by pumping a polymeric solution in a high electric field; due to the electrostatic charging and solvent evaporation, the precursor mixture is converted into nonwoven meshes with different fiber densities and mechanical properties. Moreover, polyaniline is a conducting polymer with interesting optical properties, suitable for displays and electrochromic windows. Otherwise, polyaniline is an electroactive polymer that can contract/expand by applying electric stimuli, due to the oxidation/reduction reactions which take place in the polymer chains. These two main properties can be exploited in order to synthesize smart materials that change their dimensions, exhibiting in the same time good electrochromic properties. In the context aforesaid, a poly(methyl metacrylate) solution was spun to get webs composed of fibers with diameter values between 500 nm and 1 µm. Further, the polymer meshes were covered with a gold layer in order to make them conductive and also appropriate as working electrode in an electrochemical cell. The gold shell was deposited by DC sputtering. Such metalized fibers can be transformed into smart materials by covering them with a thin layer of conductive polymer. Thus, the webs were coated with a polyaniline film by the electrochemical route, starting from and aqueous solution of aniline and sulfuric acid, where sulfuric acid acts as oxidant agent. For the polymerization of aniline, a saturated calomel electrode was employed as reference, a platinum plate as counter electrode and the gold covered webs as working electrode. Chronoamperometry was selected as deposition method for polyaniline, by modifying the deposition time. Metalized meshes with different fiber densities were used, the transmission ranging between 70 and 80 %. The morphological investigation showed that polyaniline layer has a granular structure for all deposition experiments. As well, some preliminary optical tests were done by using sulfuric acid as electrolyte, which revealed the modification of polyaniline colour from green to dark blue when applying a voltage. In conclusion, new multilayered materials were obtained by a simple approach: the merge of the electrospinning method benefits with polyaniline chemistry. This synthesis method allows the fabrication of structures with reproducible characteristics, suitable for display or tissue substituents.

Keywords: electrospinning, fibers, smart materials, polyaniline

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Authors: C. D’Urso, L. Frusteri, M. Samperi, G. Leonardi

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Solid metal halides are used as active cathode ingredients in the case of Na-NiCl2 batteries that require a fused secondary electrolyte, sodium tetrachloraluminate (NaAlCl4), to facilitate the movement of the Na+ ion into the cathode. The sodium-nickel chloride (Na - NiCl2) battery has been extensively investigated as a promising system for large-scale energy storage applications. The growth of Ni and NaCl particles in the cathodes is one of the most important factors that degrade the performance of the Na-NiCl2 battery. The larger the particles of active ingredients contained in the cathode, the smaller the active surface available for the electrochemical reaction. Therefore, the growth of Ni and NaCl particles can lead to an increase in cell polarization resulting from the reduced active area. A higher current density, a higher state of charge (SOC) at the end of the charge (EOC) and a lower Ni / NaCl ratio are the main parameters that result in the rapid growth of Ni particles. In light of these problems, cathode and chemistry Nano-materials with recognized and well-documented electrochemical functions have been studied and manufactured to simultaneously improve battery performance and develop less expensive and more performing, sustainable and environmentally friendly materials. Starting from the well-known cathodic material (Na-NiCl2), the new electrolytic materials have been prepared on the replacement of nickel with iron (10-90%substitution of Nichel with Iron), to obtain a new material with potential advantages compared to current battery technologies; for example,, (1) lower cost of cathode material compared to state of the art as well as (2) choices of cheaper materials (stainless steels could be used for cell components, including cathode current collectors and cell housings). The study on the particle size of the cathode and the physicochemical characterization of the cathode was carried out in the test cell using, where possible, the GITT method (galvanostatic technique of intermittent titration). Furthermore, the impact of temperature on the different cathode compositions of the positive electrode was studied. Especially the optimum operating temperature is an important parameter of the active material.

Keywords: critical raw materials, energy storage, sodium metal halide, battery

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Authors: K. Sruthi, Sai Snehitha Yadavalli, Swathi Gosh Acharyya

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Water is the most crucial element for sustaining life on earth. Increasing water pollution directly or indirectly leads to harmful effects on human life. Most of the heavy metal ions are harmful in their cationic form. These heavy metal ions are released by various activities like disposing of batteries, industrial wastes, automobile emissions, and soil contamination. Ions like (Pb, Co, Cd) are carcinogenic and show many harmful effects when consumed more than certain limits proposed by WHO. The simultaneous detection of the heavy metal ions (Pb, Co, Cd), which are highly toxic, is reported in this study. There are many analytical methods for quantifying, but electrochemical techniques are given high priority because of their sensitivity and ability to detect and recognize lower concentrations. Square wave voltammetry was preferred in electrochemical methods due to the absence of background currents which is interference. Square wave voltammetry was performed on GCE for the quantitative detection of ions. Three electrode system consisting of a glassy carbon electrode as the working electrode (3 mm diameter), Ag/Agcl electrode as the reference electrode, and a platinum wire as the counter electrode was chosen for experimentation. The mechanism of detection was done by optimizing the experimental parameters, namely pH, scan rate, and temperature. Under the optimized conditions, square wave voltammetry was performed for simultaneous detection. Scan rates were varied from 5 mV/s to 100 mV/s and found that at 25 mV/s all the three ions were detected simultaneously with proper peaks at particular stripping potential. The variation of pH from 3 to 8 was done where the optimized pH was taken as pH 5 which holds good for three ions. There was a decreasing trend at starting because of hydrogen gas evolution, and after pH 5 again there was a decreasing trend that is because of hydroxide formation on the surface of the working electrode (GCE). The temperature variation from 25˚C to 45˚C was done where the optimum temperature concerning three ions was taken as 35˚C. Deposition and stripping potentials were given as +1.5 V and -1.5 V, and the resting time of 150 seconds was given. Three ions were detected at stripping potentials of Cd²⁺ at -0.84 V, Pb²⁺ at -0.54 V, and Co²⁺ at -0.44 V. The parameters of detection were optimized on a glassy carbon electrode for simultaneous detection of the ions at lower concentrations by square wave voltammetry.

Keywords: cadmium, cobalt, lead, glassy carbon electrode, square wave anodic stripping voltammetry

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Authors: Bhargav Baruah, Ali Shemsedin Reshad, Pankaj Tiwari

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This work presents a detailed study on the thermal degradation kinetics of co-pyrolysis of oil shale of Upper Assam, India with rubber seed shell, and lab-scale pyrolysis to investigate the influence of pyrolysis parameters on product yield and composition of products. The physicochemical characteristics of oil shale and rubber seed shell were studied by proximate analysis, elemental analysis, Fourier transform infrared spectroscopy and X-ray diffraction. The physicochemical study showed the mixture to be of low moisture, high ash, siliceous, sour with the presence of aliphatic, aromatic, and phenolic compounds. The thermal decomposition of the oil shale with rubber seed shell was studied using thermogravimetric analysis at heating rates of 5, 10, 20, 30, and 50 °C/min. The kinetic study of the oil shale pyrolysis process was performed on the thermogravimetric (TGA) data using three model-free isoconversional methods viz. Friedman, Flynn Wall Ozawa (FWO), and Kissinger Akahira Sunnose (KAS). The reaction mechanisms were determined using the Criado master plot. The understanding of the composition of Indian oil shale and rubber seed shell and pyrolysis process kinetics can help to establish the experimental parameters for the extraction of valuable products from the mixture. Response surface methodology (RSM) was employed usinf central composite design (CCD) model to setup the lab-scale experiment using TGA data, and optimization of process parameters viz. heating rate, temperature, and particle size. The samples were pre-dried at 115°C for 24 hours prior to pyrolysis. The pyrolysis temperatures were set from 450 to 650 °C, at heating rates of 2 to 20°C/min. The retention time was set between 2 to 8 hours. The optimum oil yield was observed at 5°C/min and 550°C with a retention time of 5 hours. The pyrolytic oil and gas obtained at optimum conditions were subjected to characterization using Fourier transform infrared spectroscopy (FT-IR) gas chromatography and mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (NMR).

Keywords: Indian oil shale, rubber seed shell, co-pyrolysis, isoconversional methods, gas chromatography, nuclear magnetic resonance, Fourier transform infrared spectroscopy

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Authors: Kotbia Labiod, Mohamed Mouldi Tlili

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The presence of different mineral salts in natural waters may precipitate and form hard deposits in water distribution systems. In this respect, we have developed numerous works on scaling by Algerian water with a very high hardness of 102 °F. The aim of our work is to study the influence of water dynamics and its composition on mineral salts on the precipitation of calcium carbonate (CaCO3). To achieve this objective, we have adopted two precipitation techniques based on controlled degassing of dissolved CO2. This study will identify the causes and provide answers to this complex phenomenon.

Keywords: calcium carbonate, controlled degassing, precipitation, scaling

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Authors: Mohamed M. Ibrahim, Gaber A. M. Mersal, Salih Al-Juaid, Samir A. El-Shazly

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A series of mixed ligand complexes, viz., [Cu(BPy)(Gly)X]Y {X = Cl (1), Y = 0; X = 0, Y = ClO4- (2); X = H2O, Y = NO3- (3); X = H2O, Y = CH3COO- (4); and [Cu(BPy)(Gly)-(H2O)]2(SO4) (5) have been synthesized. Their structures and properties were characterized by elemental analysis, thermal analaysis, IR, UV–vis, and ESR spectroscopy, as well as electrochemical measurements including cyclic voltammetry, electrical molar conductivity, and magnetic moment measurements. Complexes 1 and 2 formed slightly distorted square-pyramidal coordination geometries of CuN3OCl and CuN3O2, respectively in which the N,O-donor glycine and N,N-donor bipyridyl bind at the basal plane with chloride ion or water as the axial ligand. Complex 3 shows square planar CuN3O coordination geometry, which exhibits chemically significant hydrogen bonding interactions besides showing coordination polymer formation. The superoxide dismutase and catalase-like activities of all complexes were tested and were found to be promising candidates as durable electron-transfer catalyst being close to the efficiency of the mimicking enzymes displaying either catalase or tyrosinase activity to serve for complete reactive oxygen species (ROS) detoxification, both with respect to superoxide radicals and related peroxides. The DNA binding interaction with super coiled pGEM-T plasmid DNA was investigated by using spectral (absorption and emission) titration and electrochemical techniques. The results revealed that DNA intercalate with complexes 1 and 2 through the groove binding mode. The calculated intrinsic binding constant (Kb) of 1 and 2 were 4.71 and 2.429 × 105 M−1, respectively. Gel electrophoresis study reveals the fact that both complexes cleave super coiled pGEM-T plasmid DNA to nicked and linear forms in the absence of any additives. On the other hand, the interaction of both complexes with DNA, the quasi-reversible CuII/CuI redox couple slightly improves its reversibility with considerable decrease in current intensity. All the experimental results indicate that the bipyridyl mixed copper(II) complex (1) intercalate more effectively into the DNA base pairs.

Keywords: enzyme mimics, mixed ligand complexes, X-ray structures, antioxidant, DNA-binding, DNA cleavage

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Authors: Hao-Wen Chang, Santhanamoorthi Nachimuthu, Jyh-Chiang Jiang

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All-solid-state lithium batteries (ASSLBs) are increasingly recognized as a safer and more reliable alternative to conventional lithium-ion batteries due to their non-flammable nature and enhanced safety performance. ASSLBs utilize a range of solid-state electrolytes, including solid polymer electrolytes (SPEs), inorganic solid electrolytes (ISEs), and composite polymer electrolytes (CPEs). SPEs are particularly valued for their flexibility, ease of processing, and excellent interfacial compatibility with electrodes, though their ionic conductivity remains a significant limitation. ISEs, on the other hand, provide high ionic conductivity, broad electrochemical windows, and strong mechanical properties but often face poor interfacial contact with electrodes, impeding performance. CPEs, which merge the strengths of SPEs and ISEs, represent a compelling solution for next-generation ASSLBs by addressing both electrochemical and mechanical challenges. Despite their potential, the mechanisms governing lithium-ion transport within these systems remain insufficiently understood. In this study, we designed CPEs based on argyrodite-type Li₆PS₅Cl (LPSC) combined with two distinct polymer matrices: poly(ethylene oxide) (PEO) with 24.5 wt% lithium bis(trifluoromethane)sulfonimide (LiTFSI) and polycaprolactone (PCL) with 25.7 wt% LiTFSI. Through density functional theory (DFT) calculations, we investigated the interfacial chemistry of these materials, revealing critical insights into their stability and interactions. Additionally, ab initio molecular dynamics (AIMD) simulations of lithium electrodes interfaced with LPSC layers containing polymers and LiTFSI demonstrated that the polymer matrix significantly mitigates LPSC decomposition, compared to systems with only a lithium electrode and LPSC layers. These findings underscore the pivotal role of CPEs in improving the performance and longevity of ASSLBs, offering a promising path forward for next-generation energy storage technologies.

Keywords: all-solid-state lithium-ion batteries, composite solid electrolytes, DFT calculations, Li-ion transport

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Authors: P. S. D. Perera, S. U. Adikary

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The gelation behavior of Chitosan/nanohydroxyapatite sol in the presence of a crosslinking agent Na ₂CO₃ was investigated experimentally. In this case, the gelation time(tgel) was determined by the rheological measurements of the final mixture. The tgel has been determined from dynamic viscosity slope experiments. We found that chitosan/nHA sol with 1% nano-hydroxyapatite and 1.6% Na2CO3 required coagulant performance. Hence Na ₂CO₃ and nanohydroxyapatite concentrations remain constant over the experiment. The order of reaction was first order with respect to chitosan and rate constant of the gel system was 9.0 x 10-4 s-1, respectively, depending on the temperature of the system. The gelation temperature was carried out at 37 ⁰C.

Keywords: kinetics, gelation, sol-gel system, chitosan/ nHA/ Na ₂CO₃ composite

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Authors: Mecabih Zohra

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Water is such an important element of many manufacturing processes which that use a big amount of chemical substances, It is likely to cause it contamination of water returning to rivers by industrial discharged. These contaminants can be a high in suspended solid and chemical oxygen demand. In this study, urban wastewater of sidi bel abbes city (Algeria) was treated by adsorption using modified bentonite from Magnia (Algeria) by conducting batch experiments to investigate its equilibrium characteristics and kinetics. Purified bentonite is characterized by; CEC, XRF, BET, FITR, XRD, SEM and 27Al spectroscopy. The results showed the removal of suspended solids exceeds 98.47% and COD up to 99.52%, and regarding of sorption efficiencies (qm), the maximum COD sorption efficiencies (qm) calculated using the Langmuir model is 156.23, 64.47 and 17.19 mg/g respectively, for a pH range of 4 to 9.

Keywords: adsorption, bentonite, COD, wastewater

Procedia PDF Downloads 87

Authors: Mecabih Zohra

Abstract:

Water is such an important element of many manufacturing processes which that use a big amount of chemical substances, It is likely to cause it contamination of water returning to rivers by industrial discharged. These contaminants can be a high in suspended solid and chemical oxygen demand. In this study, urban wastewater of sidi bel abbes city (Algeria) was treated by adsorption using modified bentonite from Magnia (Algeria) by conducting batch experiments to investigate its equilibrium characteristics and kinetics. Purified bentonite is characterized by; CEC, XRF, BET, FITR, XRD, SEM and 27Al spectroscopy. The results showed the removal of suspended solids exceeds 98.47% and COD up to 99.52%, and regarding of sorption efficiencies (qm), the maximum COD sorption efficiencies (qm) calculated using the Langmuir model is 156.23, 64.47 and 17.19 mg/g respectively, for a pH range of 4 to 9.

Keywords: adsorption, bentonite, COD, wastewater

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Authors: Adrienn Kiss, Karoly Zauer, Gyorgy Keglevich, Rita Molnarne Bernath

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Ginger (Zingiber officinale) is a perennial plant from Southeast Asia, widely used as a spice, herb, and medicine for many illnesses since its beneficial health effects were observed thousands of years ago. Among the compounds found in ginger, zingerone [4-hydroxy-3- methoxyphenyl-2-butanone] deserves special attention: it has an anti-inflammatory and antispasmodic effect, it can be used in case of diarrheal disease, helps to prevent the formation of blood clots, has antimicrobial properties, and can also play a role in preventing the Alzheimer's disease. Ferulic acid [(E)-3-(4-hydroxy-3-methoxyphenyl)-prop-2-enoic acid] is another cinnamic acid derivative in ginger, which has promising properties. Like many phenolic compounds, ferulic acid is also an antioxidant. Based on the results of animal experiments, it is assumed to have a direct antitumoral effect in lung and liver cancer. It also deactivates free radicals that can damage the cell membrane and the DNA and helps to protect the skin against UV radiation. The aim of this work was to synthesize these two compounds by new methods. A few of the reactions were based on the hydrogenation of dehydrozingerone [4-(4-Hydroxy-3-methoxyphenyl)-3-buten-2-one] to zingerone. Dehydrozingerone can be synthesized by a relatively simple method from acetone and vanillin with good yield (80%, melting point: 41 °C). Hydrogenation can be carried out chemically, for example by the reaction of zinc and acetic acid, or Grignard magnesium and ethyl alcohol. Another way to complete the reduction is the electrochemical pathway. The electrolysis of dehydrozingerone without diaphragm in aqueous media was attempted to produce ferulic acid in the presence of sodium carbonate and potassium iodide using platinum electrodes. The electrolysis of dehydrozingerone in the presence of potassium carbonate and acetic acid to prepare zingerone was carried out similarly. Ferulic acid was expected to be converted to dihydroferulic acid [3-(4-Hydroxy-3-methoxyphenyl)propanoic acid] in potassium hydroxide solution using iron electrodes, separating the anode and cathode space with a Soxhlet paper sheath impregnated with saturated magnesium chloride solution. For this reaction, ferulic acid was synthesized from vanillin and malonic acid in the presence of pyridine and piperidine (yield: 88.7%, melting point: 173°C). Unfortunately, in many cases, the expected transformations did not happen or took place in low conversions, although gas evolution occurred. Thus, a deeper understanding of these experiments and optimization are needed. Since both compounds are found in different plants, they can also be obtained by alkaline extraction or steam distillation from distinct plant parts (ferulic acid from ground bamboo shoots, zingerone from grated ginger root). The products of these reactions are rich in several other organic compounds as well; therefore, their separation must be solved to get the desired pure material. The products of the reactions described above were characterized by infrared spectral data and melting points. The use of these two simple methods may be informative for the formation of the products. In the future, we would like to study the ferulic acid and zingerone content of other plants and extract them efficiently. The optimization of electrochemical reactions and the use of other test methods are also among our plans.

Keywords: ferulic acid, ginger, synthesis, zingerone

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Authors: Sukrit Ghorai, Akku Aby Mathews

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Corrosion in reinforcing steel is the leading cause for deterioration in concrete structures. It is an electrochemical process which leads to volumetric change in concrete and causes cracking, delamination and spalling. The objective of the study is to provide a rational method to estimate the probable chloride concentration at the reinforcement level for a known surface chloride concentration. The paper derives the formulation of design charts to aid engineers for quick calculation of the chloride concentration. Furthermore, the paper focuses on comparison of durability design against corrosion with American, European and Indian design standards.

Keywords: chloride infiltration, concrete, corrosion, design charts

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Authors: Abdelghani Boucheham, Ahcene Karaali, Amar Manseri

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Nanostructured Titania layers formed on the surface of titanium and titanium alloys by anodic oxidation play an important role in the enhancement of their biocompatibility and osseointegration in the human body. In the current work, highly ordered titania nanotube array films were elaborated on Ti₆Al₄V medical grade alloys in organic electrolyte containing ethylene glycol, 0.2 wt. % NH₄F and 4 vol. % H₂O at an applied potential of 60 V for different durations. The diameters, lengths and wall thicknesses of the obtained nanotubes were characterized by scanning electronic microscopy (SEM).

Keywords: anodization, dental implants, titania nanotubes, titanium alloys, SEM

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Authors: Gökçe Erdemir, İlhan Yaylım, Serap Erdem-Kuruca, Musa Mutlu Can

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It has been determined that the main reason for the death of cancer disease is caused by metastases rather than the primary tumor. The cells that leave the primary tumor and enter the circulation and cause metastasis in the secondary organs are called "circulating tumor cells" (CTCs). The presence and number of circulating tumor cells has been associated with poor prognosis in many major types of cancer, including breast, prostate, and colorectal cancer. It is thought that knowledge of circulating tumor cells, which are seen as the main cause of cancer-related deaths due to metastasis, plays a key role in the diagnosis and treatment of cancer. The fact that tissue biopsies used in cancer diagnosis and follow-up are an invasive method and are insufficient in understanding the risk of metastasis and the progression of the disease have led to new searches. Liquid biopsy tests performed with a small amount of blood sample taken from the patient for the detection of CTCs are easy and reliable, as well as allowing more than one sample to be taken over time to follow the prognosis. However, since these cells are found in very small amounts in the blood, it is very difficult to capture them and specially designed analytical techniques and devices are required. Methods based on the biological and physical properties of the cells are used to capture these cells in the blood. Early diagnosis is very important in following the prognosis of tumors of epithelial origin such as breast, lung, colon and prostate. Molecules such as EpCAM, vimentin, and cytokeratins are expressed on the surface of cells that pass into the circulation from very few primary tumors and reach secondary organs from the circulation, and are used in the diagnosis of cancer in the early stage. For example, increased EpCAM expression in breast and prostate cancer has been associated with prognosis. These molecules can be determined in some blood or body fluids to be taken from patients. However, more sensitive methods are required to be able to determine when they are at a low level according to the course of the disease. The aim is to detect these molecules found in very few cancer cells with the help of sensitive, fast-sensing biosensors, first in breast cancer cells reproduced in vitro and then in blood samples taken from breast cancer patients. In this way, cancer cells can be diagnosed early and easily and effectively treated.

Keywords: electrochemical biosensors, breast cancer, circulating tumor cells, EpCAM, Vimentin, Cytokeratins

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Authors: C. Amrane, D. Haman

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Aluminum-magnesium alloys are widely used in industry thanks to their mechanical properties and corrosion resistivity. These properties are related to the magnesium content and to the applied heat treatments. Although they are already well studied, questions concerning the microstructural stability and the effect of different heat treatments are still being asked. In this work we have presented a comparative study on the behavior of the precipitation reactions during different heat treatment in two different Al-Mg alloys (Al–8 wt. % Mg and Al–12 wt. % Mg). For this purpose, we have used various experimental techniques as dilatometry, calorimetry, optical microscopy, and microhardness measurements. The obtained results shown that, the precipitation kinetics and the mechanical responses to the applied heat treatments, of the two studied alloys, are different.

Keywords: Al-Mg alloys, precipitation, hardness, heat treatments

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Authors: Eduardo Martínez González, Mousumi Dey, Pekka Peljo

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Transitioning to a renewable energy model is inevitable owing to the effects of climate change. These energies are aimed at sustainability and a positive impact on the environment, but they are intermittent energies; their connection to the electrical grid depends on creating long-term, efficient, and low-cost energy storage devices. Redox flow batteries are attractive technologies to address this problem, as they store energy in solution through external tanks known as posolyte (solution to storage positive charge) and negolyte (solution to storage negative charge). During the charging process of the device, the posolyte and negolyte solutions are pumped into an electrochemical cell (which has the anode and cathode separated by an ionic membrane), where they undergo oxidation and reduction reactions at electrodes, respectively. The electrogenerated species should be stable and diffuse into the bulk solution. It has been possible to connect gigantic redox flow batteries to the electrical grid. However, the devices created do not fit with the sustainability criteria since their electroactive material consists of vanadium (material scarce and expensive) solutions dissolved in an acidic medium (e.g., 9 mol L-1 of H₂SO₄) that is highly corrosive; so, work is being done on the design of organic-electroactive electrolytes (posolytes and nogolytes) for their operation at different pH values, including neutral medium. As a main characteristic, negolyte species should have low reduction potential values, while the reverse is true for the oxidation process of posolytes. A wide variety of negolytes that store 1 and up to 2 electrons per molecule (in aqueous medium) have been publised. Gallocyanine compound was recently introduced as an electroactive material for developing alkaline flow battery negolytes. The system can storage two electrons per molecule, but its unexpectedly low water solubility was improved with an amino sulphonic acid additive. The cycling stability of and improved gallocyanine electrolyte was demonstrated by operating a flow battery cell (pairing the system to a posolyte composed of ferri/ferrocyanide solution) outside a glovebox. We also discovered that the additive improves the solubility of gallocyanine, but there is a kinetic price to pay for this advantage. Therefore, in this work, the effect of different amino sulphonic acid derivatives on the kinetics and solubility of gallocyanine compound was studied at alkaline solutions. The additive providing a faster electron transfer rate and high solubility was tested in a flow battery cell. An aqueous organic flow battery electrolyte working outside a glovebox with 15 mAhL-1 will be discussed. Acknowledgments: To Bi3BoostFlowBat Project (2021-2025), funded by the European Research Concil. For support with infrastructure, reagents, and a postdoctoral fellowship to Dr. Martínez-González.

Keywords: alkaline flow battery, gallocyanine electroactive material, amine-sulphonic acid additives, improved solubility

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Authors: Wenyu Guo, Malachy O’Rourke, Mark Bowkett, Michael Gilchrist

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Many devices for real-time monitoring of surface water have been developed in the past few years to provide early warning of pollutions and so to decrease the risk of environmental pollution efficiently. One of the most common methodologies used in the detection system is a colorimetric process, in which a container with fixed volume is filled with target ions and reagents to combine a colorimetric dye. The colorimetric ions can sensitively absorb a specific-wavelength radiation beam, and its absorbance rate is proportional to the concentration of the fully developed product, indicating the concentration of target nutrients in the pre-mixed water samples. In order to achieve precise and rapid detection effect, channels with dimensions in the order of micrometers, i.e., microfluidic systems have been developed and introduced into these diagnostics studies. Microfluidics technology largely reduces the surface to volume ratios and decrease the samples/reagents consumption significantly. However, species transport in such miniaturized channels is limited by the low Reynolds numbers in the regimes. Thus, the flow is extremely laminar state, and diffusion is the dominant mass transport process all over the regimes of the microfluidic channels. The objective of this present work has been to analyse the mixing effect and chemistry kinetics in a stop-flow microfluidic device measuring Nitride concentrations in fresh water samples. In order to improve the temporal resolution of the Nitride microfluidic sensor, we have used computational fluid dynamics to investigate the influence that the effectiveness of the mixing process between the sample and reagent within a microfluidic device exerts on the time to completion of the resulting chemical reaction. This computational approach has been complemented by physical experiments. The kinetics of the Griess reaction involving the conversion of sulphanilic acid to a diazonium salt by reaction with nitrite in acidic solution is set in the Laminar Finite-rate chemical reaction in the model. Initially, a methodology was developed to assess the degree of mixing of the sample and reagent within the device. This enabled different designs of the mixing channel to be compared, such as straight, square wave and serpentine geometries. Thereafter, the time to completion of the Griess reaction within a straight mixing channel device was modeled and the reaction time validated with experimental data. Further simulations have been done to compare the reaction time to effective mixing within straight, square wave and serpentine geometries. Results show that square wave channels can significantly improve the mixing effect and provides a low standard deviations of the concentrations of nitride and reagent, while for straight channel microfluidic patterns the corresponding values are 2-3 orders of magnitude greater, and consequently are less efficiently mixed. This has allowed us to design novel channel patterns of micro-mixers with more effective mixing that can be used to detect and monitor levels of nutrients present in water samples, in particular, Nitride. Future generations of water quality monitoring and diagnostic devices will easily exploit this technology.

Keywords: nitride detection, computational fluid dynamics, chemical kinetics, mixing effect

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Authors: Lacramioara Ochiuz, Aurelia Vasile, Iulian Stoleriu, Cristina Ghiciuc, Maria Ignat

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Topical administration of chemotherapeutic agents (eg. carmustine, bexarotene, mechlorethamine etc.) in local treatment of cutaneous T-cell lymphoma (CTCL) is accompanied by multiple side effects, such as contact hypersensitivity, pruritus, skin atrophy or even secondary malignancies. A known method of reducing the side effects of anticancer agent is the development of modified drug release systems using drug incapsulation in biocompatible nanoporous inorganic matrices, such as mesoporous MCM-41 silica. Mesoporous MCM-41 silica is characterized by large specific surface, high pore volume, uniform porosity, and stable dispersion in aqueous medium, excellent biocompatibility, in vivo biodegradability and capacity to be functionalized with different organic groups. Therefore, MCM-41 is an attractive candidate for a wide range of biomedical applications, such as controlled drug release, bone regeneration, protein immobilization, enzymes, etc. The main advantage of this material lies in its ability to host a large amount of the active substance in uniform pore system with adjustable size in a mesoscopic range. Silanol groups allow surface controlled functionalization leading to control of drug loading and release. This study shows (I) the amino-grafting optimization of mesoporous MCM-41 silica matrix by means of co-condensation during synthesis and post-synthesis using APTES (3-aminopropyltriethoxysilane); (ii) loading the therapeutic agent (carmustine) obtaining a modified drug release systems; (iii) determining the profile of in vitro carmustine release from these systems; (iv) assessment of carmustine release kinetics by fitting on four mathematical models. Obtained powders have been described in terms of structure, texture, morphology thermogravimetric analysis. The concentration of the therapeutic agent in the dissolution medium has been determined by HPLC method. In vitro dissolution tests have been done using cell Enhancer in a 12 hours interval. Analysis of carmustine release kinetics from mesoporous systems was made by fitting to zero-order model, first-order model Higuchi model and Korsmeyer-Peppas model, respectively. Results showed that both types of highly ordered mesoporous silica (amino grafted by co-condensation process or post-synthesis) are thermally stable in aqueous medium. In what regards the degree of loading and efficiency of loading with the therapeutic agent, there has been noticed an increase of around 10% in case of co-condensation method application. This result shows that direct co-condensation leads to even distribution of amino groups on the pore walls while in case of post-synthesis grafting many amino groups are concentrated near the pore opening and/or on external surface. In vitro dissolution tests showed an extended carmustine release (more than 86% m/m) both from systems based on silica functionalized directly by co-condensation and after synthesis. Assessment of carmustine release kinetics revealed a release through diffusion from all studied systems as a result of fitting to Higuchi model. The results of this study proved that amino-functionalized mesoporous silica may be used as a matrix for optimizing the anti-cancer topical therapy by loading carmustine and developing prolonged-release systems.

Keywords: carmustine, silica, controlled, release

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