Search results for: signal-off electrochemical biosensor

Authors: Abdur Rahim, Lauro Tatsuo Kubota, Yoshitaka Gushikem

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Carbon ceramic mesoporous SiO2/50wt%C (SBET= 170 m2g-1), where C is graphite, was prepared by the sol gel method. Scanning electron microscopy images and the respective element mapping showed that, within the magnification used, no phase segregation was detectable. It presented the electric conductivities of 0.49 S cm-1. This material was used to support cobalt phthalocyanine, prepared in situ, to assure a homogeneous dispersion of the electro active complex in the pores of the matrix. The surface density of cobalt phthalocyanine, on the matrix surfaces was 0.015 mol cm-2. Pressed disk, made with SiO2/50wt%C/CoPc, was used to fabricate an electrode and tested as sensors for nitrite determination by electro chemical technique. A linear response range between 0.039 and 0.42 mmol l−1,and correlation coefficient r=0.9996 was obtained. The electrode was chemically very stable and presented very high sensitivity for this analyte, with a limit of detection, LOD = 1.087 x 10-6 mol L-1.

Keywords: SiO2/C/CoPc, sol-gel method, electrochemical sensor, nitrite oxidation, carbon ceramic material, cobalt phthalocyanine

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Authors: Amandeep Singh Oberoi, John Andrews, Alan L. Chaffee, Lachlan Ciddor

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Electrochemical storage of hydrogen in activated carbon electrodes as part of a reversible fuel cell offers a potentially attractive option for storing surplus electrical energy from inherently variable solar and wind energy resources. Such a system – which we have called a proton flow battery – promises to have roundtrip energy efficiency comparable to lithium ion batteries, while having higher gravimetric and volumetric energy densities. Activated carbons with high internal surface area, high pore volume, light weight and easy availability have attracted considerable research interest as a solid-state hydrogen storage medium. This paper compares the physical characteristics and hydrogen storage capacities of four activated carbon electrodes made by different methods from brown coal. The fabrication methods for these samples are explained. Their proton conductivity was measured using electrochemical impedance spectroscopy, and their hydrogen storage capacity by galvanostatic charging and discharging in a three-electrode electrolytic cell with 1 mol sulphuric acid as electrolyte. The highest hydrogen storage capacity obtained was 1.29 wt%, which compares favourably with metal hydrides used in commercially available solid-state hydrogen storages. The hydrogen storage capacity of the samples increased monotonically with increasing BET surface area (calculated from CO2 adsorption method). The results point the way towards selecting high-performing electrodes for proton flow batteries that the competitiveness of this energy storage technology.

Keywords: activated carbon, electrochemical hydrogen storage, proton flow battery, proton conductivity

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Authors: M.S. Ashraf, Raja Rizwan Hussain, A. M. Alhozaimy

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The effect of supplementary cementitious materials (SCMs) with concrete pore solution on the protective properties of the oxide films that form on reinforcing steel bars has been experimentally investigated using electrochemical impedance spectroscopy (EIS) and Tafel Scan. The tests were conducted on oxide films grown in saturated calcium hydroxide solutions that included different representative amounts of NaOH and KOH. In addition to that, commonly used supplementary cementitious materials (natural pozzolan and fly ash) were also added. The results of electrochemical tests show that supplementary cementitious materials do have an effect on the protective properties of the passive oxide film. In particular, natural pozzolans has been shown to have a highly positive influence on the film quality. Fly ash also increases the protective qualities of the passive film.

Keywords: supplementary cementitious materials (SCMs), passive film, EIS, Tafel scan, rebar, concrete, simulated concrete pore solution (SPS)

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Authors: Yu. Mateyshina, A. Ulihin, N. Uvarov

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Supercapacitors are one of the most promising devices for energy storage applications as they can provide higher power density than batteries and higher energy density than conventional dielectric capacitors. Carbon materials with various microtextures are considered as main candidates for supercapacitors in terms of high surface area, interconnected pore structure, controlled pore size, high electrical conductivity and environmental friendliness. The specific capacitance (C) of the electrode material of the Electrochemical Double Layer Capacitors (EDLC) is known to depend on the specific surface area (Ss) and the pore structure. Activated carbons are most commonly used in supercapacitors because of their high surface area (Ss ≥ 1000 m2/g), good adhesion to electrolytes and low cost. In this work, electrochemical properties of new microporous and mesoporous carbon electrode materials were studied. The aim of the work was to investigate the relationship between the specific capacitance and specific surface area in a series of materials prepared from different organic precursors.. As supporting matrixes different carbon samples with Ss = 100-2000 m2/g were used. The materials were modified by treatment in acids (H2SO4, HNO3, acetic acid) in order to enable surface hydrophilicity. Then nanoparticles of transition metal oxides (for example NiO) were deposited on the carbon surfaces using methods of salts impregnation, mechanical treatment in ball mills and the precursors decomposition. The electrochemical characteristics of electrode hybrid materials were investigated in a symmetrical two-electrode cell using an impedance spectroscopy, voltammetry in both potentiodynamic and galvanostatic modes. It was shown that the value of C for the materials under study strongly depended on the preparation method of the electrode and the type of electrolyte (1 M H2SO4, 6 M KOH, 1 M LiClO4 in acetonitryl). Specific capacity may be increased by the introduction of nanoparticles from 50-100 F/g for initial carbon materials to 150-300 F/g for nanocomposites which may be used in supercapacitors. The work is supported by the по SC-14.604.21.0013.

Keywords: supercapacitors, carbon electrode, mesoporous carbon, electrochemistry

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Authors: Andrea Pietrelli, Vincenzo Ferrara, Bruno Allard, Francois Buret, Irene Bavasso, Nicola Lovecchio, Francesca Costantini, Firas Khaled

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This paper aims to show some applications of microbial fuel cells (MFCs), an energy harvesting technique, as clean power source to supply low power device for application like wireless sensor network (WSN) for environmental monitoring. Furthermore, MFC can be used directly as biosensor to analyse parameters like pH and temperature or arranged in form of cluster devices in order to use as small power plant. An MFC is a bioreactor that converts energy stored in chemical bonds of organic matter into electrical energy, through a series of reactions catalysed by microorganisms. We have developed a lab-scale terrestrial microbial fuel cell (TMFC), based on soil that acts as source of bacteria and flow of nutrient and a lab-scale waste water microbial fuel cell (WWMFC), where waste water acts as flow of nutrient and bacteria. We performed large series of tests to exploit the capability as biosensor. The pH value has strong influence on the open circuit voltage (OCV) delivered from TMFCs. We analyzed three condition: test A and B were filled with same soil but changing pH from 6 to 6.63, test C was prepared using a different soil with a pH value of 6.3. Experimental results clearly show how with higher pH value a higher OCV was produced; indeed reactors are influenced by different values of pH which increases the voltage in case of a higher pH value until the best pH value of 7 is achieved. The influence of pH on OCV of lab-scales WWMFC was analyzed at pH value of 6.5, 7, 7.2, 7.5 and 8. WWMFCs are influenced from temperature more than TMFCs. We tested the power performance of WWMFCs considering four imposed values of ambient temperature. Results show how power performance increase proportionally with higher temperature values, doubling the output power from 20° to 40°. The best value of power produced from our lab-scale TMFC was equal to 310 μW using peaty soil, at 1KΩ, corresponding to a current of 0.5 mA. A TMFC can supply proper energy to low power devices of a WSN by means of the design of three stages scheme of an energy management system, which adapts voltage level of TMFC to those required by a WSN node, as 3.3V. Using a commercial DC/DC boost converter, that needs an input voltage of 700 mV, the current source of 0.5 mA, charges a capacitor of 6.8 mF until it will have accumulated an amount of charge equal to 700 mV in a time of 10 s. The output stage includes an output switch that close the circuit after a time of 10s + 1.5ms because the converter can boost the voltage from 0.7V to 3.3V in 1.5 ms. Furthermore, we tested in form of clusters connected in series up to 20 WWMFCs, we have obtained a high voltage value as output, around 10V, but low current value. MFC can be considered a suitable clean energy source to be used to supply low power devices as a WSN node or to be used directly as biosensor.

Keywords: energy harvesting, low power electronics, microbial fuel cell, terrestrial microbial fuel cell, waste-water microbial fuel cell, wireless sensor network

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Authors: Gaurav Bhanjana, Ganga Ram Chaudhary, Sandeep Kumar, Neeraj Dilbaghi

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Main sources of endocrine disrupting compounds in the ecosystem are hormones, pesticides, phthalates, flame retardants, dioxins, personal-care products, coplanar polychlorinated biphenyls (PCBs), bisphenol A, and parabens. These endocrine disrupting compounds are responsible for learning disabilities, brain development problems, deformations of the body, cancer, reproductive abnormalities in females and decreased sperm count in human males. Although discharge of these chemical compounds into the environment cannot be stopped, yet their amount can be retarded through proper evaluation and detection techniques. The available techniques for determination of these endocrine disrupting compounds mainly include high performance liquid chromatography (HPLC), mass spectroscopy (MS) and gas chromatography-mass spectrometry (GC–MS). These techniques are accurate and reliable but have certain limitations like need of skilled personnel, time consuming, interference and requirement of pretreatment steps. Moreover, these techniques are laboratory bound and sample is required in large amount for analysis. In view of above facts, new methods for detection of endocrine disrupting compounds should be devised that promise high specificity, ultra sensitivity, cost effective, efficient and easy-to-operate procedure. Nowadays, electrochemical sensors/biosensors modified with nanomaterials are gaining high attention among researchers. Bioelement present in this system makes the developed sensors selective towards analyte of interest. Nanomaterials provide large surface area, high electron communication feature, enhanced catalytic activity and possibilities of chemical modifications. In most of the cases, nanomaterials also serve as an electron mediator or electrocatalyst for some analytes.

Keywords: electrochemical, endocrine disruptors, microscopy, nanoparticles, sensors

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Authors: A. Hamam, D. Oukil, A. Dib, L. Makhloufi

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The aim of this work is to synthesize modified Polypyrrole films (PPy) containing nanoparticles of copper oxides onto a non conducting cellulosic substrate. Firstly, the chemical polymerization of polypyrrole onto cellulosic substrate is carried out using FeCl3 as an oxidant and Pyrrole as monomer. Different parameters were optimized (monomer concentration, duration of the experiment, nature of supporting electrolyte, temperature, etc.) in order to obtain films with different thickness and different morphologies. Thickness and topography of different PPy deposits were estimated by a profilometer apparatus. The electrochemical reactivity of the obtained electrodes were tested by cyclic voltammetry technique (CV) and electrochemical impedance spectroscopy (EIS). Secondly, the modification of the PPy film surface by incorporation of copper oxide nanonoparticles is conducted by applying a galvanostatic procedure from CuCl2 solution. Surface characterization has been carried out using scanning microscope (SEM) coupled with energy dispersive X-ray analysis (EDX), Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis showed the presence of the copper oxide nanoparticles (CuO) in the polymer films with dimensions less than 50 nm.

Keywords: polypyrrole, modified electrode, cellulosic substrate, copper oxide

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Authors: V. Pérez-Herranz, C. González-Buch, E. M. Ortega, S. Mestre

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In this work new macroporous Ni electrodes modified with Au nanoparticles for hydrogen production have been developed. The supporting macroporous Ni electrodes have been obtained by means of the electrodeposition at high current densities. Then, the Au nanoparticles were synthesized and added to the electrode surface. The electrocatalytic behaviour of the developed electrocatalysts was studied by means of pseudo-steady-state polarization curves, electrochemical impedance spectroscopy (EIS) and hydrogen discharge curves. The size of the Au synthetized nanoparticles shows a monomodal distribution, with a very sharp band between 10 and 50 nm. The characteristic parameters d10, d50 and d90 were 14, 20 and 31 nm respectively. From Tafel polarization data has been concluded that the Au nanoparticles improve the catalytic activity of the developed electrodes towards the HER respect to the macroporous Ni electrodes. EIS permits to obtain the electrochemically active area by means of the roughness factor value. All the developed electrodes show roughness factor values in the same order of magnitude. From the activation energy results it can be concluded that the Au nanoparticles improve the intrinsic catalytic activity of the macroporous Ni electrodes.

Keywords: Au nano particles, hydrogen evolution reaction, porous Ni electrodes, electrochemical impedance spectroscopy

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Authors: Jamal Hussain Al-Smail

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Hydrogen fuel cells (HFCs) are environmentally friendly, energy converter devices that convert the chemical energy of the reactants (oxygen and hydrogen) to electricity through electrochemical reactions. The level of the electricity production of HFCs mainly increases depending on the oxygen distribution in the HFC’s cathode gas diffusion layer (GDL). With a constant porosity of the GDL, the electrochemical reaction can have a great variation that reduces the cell’s productivity and stability. Our findings bring a methodology in finding porosity designs of the diffusion layer to improve the oxygen distribution such that it results in a stable oxygen-hydrogen reaction. We first introduce a mathematical model involving the mass and momentum transport equations, in which a porosity function of the GDL is incorporated as a control for the fluid flow. We then derive numerical methods for solving the mathematical model. In conclusion, we present our numerical results to show how to design the GDL porosity to result in a uniform oxygen distribution.

Keywords: fuel cells, material porosity design, mathematical modeling, porous media

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Authors: Ayomide A Sijuade, Nafiza Anjum

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The rising demand to meet the need for clean and sustainable energy solutions has led the market to create effective energy storage technologies. In this study, we look at the possibility of using a heterostructure made of polyaniline (PANI), titanium carbide (Ti₃C₂), and vanadium carbide (V₂C) for energy storage devices. V₂C is a two-dimensional transition metal carbide with remarkable mechanical and electrical conductivity. Ti₃C2 has solid thermal conductivity and mechanical strength. PANI, on the other hand, is a conducting polymer with customizable electrical characteristics and environmental stability. Layer-by-layer assembly creates the heterostructure of V₂C, Ti₃C₂, and PANI, allowing for precise film thickness and interface quality control. Structural and morphological characterization is carried out using X-ray diffraction, scanning electron microscopy, and atomic force microscopy. For energy storage applications, the heterostructure’s electrochemical performance is assessed. Electrochemical experiments, such as cyclic voltammetry and galvanostatic charge-discharge tests, examine the heterostructure’s charge storage capacity, cycle stability, and rate performance. Comparing the heterostructure to the individual components reveals better energy storage capabilities. V₂C, Ti₃C₂, and PANI synergize to increase specific capacitance, boost charge storage, and prolong cycling stability. The heterostructure’s unique arrangement of 2D materials and conducting polymers promotes effective ion diffusion and charge transfer processes, improving the effectiveness of energy storage. The heterostructure also exhibits remarkable electrochemical stability, which minimizes capacity loss after repeated cycling. The longevity and long-term dependability of energy storage systems depend on this quality. By examining the potential of V₂C, Ti₃C₂, and PANI heterostructures, the results of this study expand energy storage technology. These materials’ specialized integration and design show potential for use in hybrid energy storage systems, lithium-ion batteries, and supercapacitors. Overall, the development of high-performance energy storage devices utilizing V₂C, Ti₃C₂, and PANI heterostructures is clarified by this research, opening the door to the realization of effective, long-lasting, and eco-friendly energy storage solutions to satisfy the demands of the modern world.

Keywords: MXenes, energy storage materials, conductive polymers, composites

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Authors: Yunwei Zhang, Qiaochu Tang, Yao Zhang, Jiabin Wang, Ulrich Stimming, Alpha Lee

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Forecasting the state of health and remaining useful life of Li-ion batteries is an unsolved challenge that limits technologies such as consumer electronics and electric vehicles. Here we build an accurate battery forecasting system by combining electrochemical impedance spectroscopy (EIS) -- a real-time, non-invasive and information-rich measurement that is hitherto underused in battery diagnosis -- with Gaussian process machine learning. We collect over 20,000 EIS spectra of commercial Li-ion batteries at different states of health, states of charge and temperatures -- the largest dataset to our knowledge of its kind. Our Gaussian process model takes the entire spectrum as input, without further feature engineering, and automatically determines which spectral features predict degradation. Our model accurately predicts the remaining useful life, even without complete knowledge of past operating conditions of the battery. Our results demonstrate the value of EIS signals in battery management systems.

Keywords: battery degradation, machine learning method, electrochemical impedance spectroscopy, battery diagnosis

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Authors: B. D. Polat, Ö. Keleş

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Physical vapor deposition under conditions of an obliquely incident flux results in a film formation with an inclined columnar structure. These columns will be oriented toward the vapor source because of the self-shadowing effect, and they are homogenously distributed on the substrate surface because of the limited surface diffusion ability of ad-atoms when there is no additional substrate heating. In this work, the oblique angle electron beam evaporation technique is used to fabricate thin films containing inclined nanorods. The results demonstrate that depending on the thin film composition, the morphology of the nanorods changed as well. The galvanostatic analysis of these thin film anodes reveals that a composite CuSn nanorods having approximately 900mAhg-1 of initial discharge capacity, performs higher electrochemical performance compared to pure Sn nanorods containing anode material. The long cycle life and the advanced electrochemical properties of the nano-structured composite electrode might be attributed to its improved mechanical tolerance and enhanced electrical conductivity depending on the Cu presence in the nanorods.

Keywords: Cu-Sn thin film, oblique angle deposition, lithium ion batteries, anode

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Authors: Ashish Kumar Singh, Preeti Tiwari, Shubham Srivastava, Rajiv Prakash, Herman Terryn, Gopal Ji

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Corrosion inhibition potential of azo dyes namely Allura red (AR), Sunset Yellow (SY) and Amaranth (AN) have been investigated in 0.5 M H2SO4 solutions by electrochemical impedance spectroscopy (EIS), Tafel polarization curves, linear polarization curves, open circuit potential (ocp) curves, UV-Visible spectroscopy, Fourier Transform Infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) techniques. Amaranth dye is found to provide highest corrosion inhibition (90 %) against mild steel corrosion in sulfuric acid solutions among all the tested dyes; while SY and AR dye shows 80% and 78% corrosion inhibition efficiency respectively. The electrochemical measurements and surface morphology analysis reveal that molecular adsorption of dyes at metal acid interface is accountable for inhibition of mild steel corrosion in H2SO4 solutions. The adsorption behavior of dyes has been investigated by various isotherms models, which verifies that it is in accordance with Langmuir isotherm.

Keywords: mild steel, Azo dye, EIS, Langmuir isotherm

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Authors: Rovina Kobun, Shafiquzzaman Siddiquee

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A novel and simple electrochemical sensor for the determination of melamine was developed based on modified gold electrode (AuE) with chitosan (CHIT) nanocomposite membrane, zinc oxide nanoparticles (ZnONPs) and ionic liquids ([EMIM][Otf]) to enhance the potential current response of melamine. Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behaviour between melamine and modified AuE in the presence of methylene blue as a redox indicator. The experimental results indicated that the interaction of melamine with CHIT/ZnONPs/([EMIM][Otf])/AuE were based on the strong interaction of hydrogen bonds. The morphological characterization of modified AuE was observed under scanning electron microscope. Under optimal conditions, the current signal was directly proportional to the melamine concentration ranging from 9.6 x 10-5 to 9.6 x 10-11 M, with a correlation coefficient of 0.9656. The detection limit was 9.6 x 10-12 M. Finally, the proposed method was successfully applied and displayed an excellent sensitivity in the determination of melamine in milk samples.

Keywords: melamine, gold electrode, zinc oxide nanoparticles, cyclic voltammetries, differential pulse voltammetries

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Authors: Christian Fercher, Jiaul Islam, Simon R. Corrie

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Fluorescence-based immunodiagnostics are an emerging field in biosensor development and exhibit several advantages over traditional detection methods. While various affinity biosensors have been developed to generate a fluorescence signal upon sensing varying concentrations of analytes, reagentless, reversible, and continuous monitoring of complex biological samples remains challenging. Here, we aimed to genetically engineer biosensors based on single-chain antibody fragments (scFv) that are site-specifically labeled with environmentally sensitive fluorescent unnatural amino acids (UAA). A rational design approach resulted in quantifiable analyte-dependent changes in peak fluorescence emission wavelength and enabled antigen detection in vitro. Incorporation of a polarity indicator within the topological neighborhood of the antigen-binding interface generated a titratable wavelength blueshift with nanomolar detection limits. In order to ensure continuous analyte monitoring, scFv candidates with fast binding and dissociation kinetics were selected from a genetic library employing a high-throughput phage display and affinity screening approach. Initial rankings were further refined towards rapid dissociation kinetics using bio-layer interferometry (BLI) and surface plasmon resonance (SPR). The most promising candidates were expressed, purified to homogeneity, and tested for their potential to detect biomarkers in a continuous microfluidic-based assay. Variations of dissociation kinetics within an order of magnitude were achieved without compromising the specificity of the antibody fragments. This approach is generally applicable to numerous antibody/antigen combinations and currently awaits integration in a wide range of assay platforms for one-step protein quantification.

Keywords: antibody engineering, biosensor, phage display, unnatural amino acids

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Authors: Celine Bonnaud, Isabelle Billard, Nicolas Papaiconomou, Eric Chainet

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Thanks to their high magnetization and low mass, permanent magnets (NdFeB and SmCo) have quickly became essential for new energies (wind turbines, electrical vehicles…). They contain large quantities of neodymium, samarium and dysprosium, that have been recently classified as critical elements and that therefore need to be recycled. Electrochemical processes including electrodissolution followed by electrodeposition are an elegant and environmentally friendly solution for the recycling of such lanthanides contained in permanent magnets. However, electrochemistry of the lanthanides is a real challenge as their standard potentials are highly negative (around -2.5V vs ENH). Consequently, non-aqueous solvents are required. Ionic liquids (IL) are novel electrolytes exhibiting physico-chemical properties that fulfill many requirements of the sustainable chemistry principles, such as extremely low volatility and non-flammability. Furthermore, their chemical and electrochemical properties (solvation of metallic ions, large electrochemical windows, etc.) render them very attractive media to implement alternative and sustainable processes in view of integrated processes. All experiments that will be presented were carried out using butyl-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide. Linear sweep, cyclic voltammetry and potentiostatic electrochemical techniques were used. The reliability of electrochemical experiments, performed without glove box, for the classic three electrodes cell used in this study has been assessed. Deposits were obtained by chronoamperometry and were characterized by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The IL cathodic behavior under different constraints (argon, nitrogen, oxygen atmosphere or water content) and using several electrode materials (Pt, Au, GC) shows that with argon gas flow and gold as a working electrode, the cathodic potential can reach the maximum value of -3V vs Fc+/Fc; thus allowing a possible reduction of lanthanides. On a gold working electrode, the reduction potential of samarium and neodymium was found to be -1.8V vs Fc+/Fc while that of dysprosium was -2.1V vs Fc+/Fc. The individual deposits obtained were found to be porous and presented some significant amounts of C, N, F, S and O atoms. Selective deposition of neodymium in presence of dysprosium was also studied and will be discussed. Next, metallic Sm, Nd and Dy electrodes were used in replacement of Au, which induced changes in the reduction potential values and the deposit structures of lanthanides. The individual corrosion potentials were also measured in order to determine the parameters influencing the electrodissolution of these metals. Finally, a full recycling process was investigated. Electrodissolution of a real permanent magnet sample was monitored kinetically. Then, the sequential electrodeposition of all lanthanides contained in the IL was investigated. Yields, quality of the deposits and consumption of chemicals will be discussed in depth, in view of the industrial feasibility of this process for real permanent magnets recycling.

Keywords: electrodeposition, electrodissolution, ionic liquids, lanthanides, rcycling

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Authors: Yen-Ping Peng, Ku-Fan Chen, Ken-Lin Chang, Jian Sun

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In this study, palladium loaded titanium dioxide nanotube arrays (Pd/TNAs) was successfully synthesized by anodic oxidation etching method combined with microwave hydrothermal method, using tea or coffee as a green reductant. Pd/TNAs was employed as an electrode in a photoelectrochemcial (PEC) system to simultaneously remove azo-dye and to generate hydrogen in the anodic and cathodic chamber, respectively. The chemical and physical properties of as-synthesized Pd/TNAs were characterized by scanning electron microscopy (SEM), ultraviolet–visible spectroscopy (UV-vis), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). SEM image indicates the diameter and the length of Pd/TNAs were approximately 300 nm and 2.5 μm, respectively. XPS analyses indicate that 1.13% (atomic %) of Pd was loaded onto the surface of TNAs. UV-vis results show that the band gap of TNAs was reduced from 3.2 eV to 2.37 eV after Pd loading. In addition, the electrochemical performances of Pd/TNAs were investigated by photocurrent density test and electrochemical impedance spectroscopy (EIS). The photocurrent (4.0 mA/cm²) of Pd /TNAs was higher than that of the uncoated TNAs (1.4 mA/cm²) at a bias potential of 1 V (vs. Ag/AgCl), indicating that Pd/TNAs-C can effectively separate photogenerated electrons and holes. The mechanism of our PEC system was proposed and discussed in detail in this study.

Keywords: Pd/TNAs, photoelectrochemical, azo-dye degradation, hydrogen generation

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Authors: H. B. Rekha, Usha N. Murthy, Prashanth, Ashoka

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Dyes are manufactured to have high chemical resistance because they are normally species, very difficult to degrade (reactive dyes). It damages flora and fauna. Furthermore, coloured components are highly hazardous. So removal of dyes becomes a challenge for both textile industry and water treatment facility. Dyeing wastewater is usually treated by conventional methods such as biological oxidation and adsorption but nowadays them becoming in-adequate because of large variability of composition of waste water. In the present investigation, mild steel electrodes of varying surface area were used for treatment of synthetic textile dye. It appears that electro-chemical coagulation could be very effective in removing coloured from wastewater; it could also be used to remove other parameters like chlorides, COD, and solids to some extent. In the present study, coloured removal up to 99% was obtained for surface area of mild steel electrode of 80 cm2 and 96% of surface area of mild steel electrode of 50 cm2. The findings from this study could be used to improve the design of electro-chemical treatment systems and modify existing systems to improve efficiency.

Keywords: electrochemical coagulation, mild steel, colour, environmental engineering

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Authors: N. Al-Orfi, M. S. El-Shahawi, A. S. Bashammakh

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The electrochemical response of glassy carbon electrode (GCE) for the sensitive and selective determination of dianabol steroid (DS) in phosphate, Britton-Robinson (B-R) and HEPES buffers of pH 2.0 - 11, 2.0 - 11 and 6.2 - 8.0, respectively using cyclic voltammetry (CV) and differential pulse- adsorptive cathodic stripping voltammetry (DP-CSV) at bare GCE was studied. The dependence of the CV response of the developed cathodic peak potential (Ep, c), peak current (ip, c) and the current function (ip, c / υ1/2) on the scan rate (υ) at the bare GCE revealed the occurrence of electrode coupled chemical reaction of EC type mechanism. The selectivity of the proposed method was assessed in the presence of high concentrations of major interfering species e.g. uric acid, ascorbic acid, citric acid, glucose, fructose, sucrose, starch and ions Na+, K+, PO4-3, NO3- and SO42-. The recovery of the method was not significant where t(critical)=2.20 > texp=1.81-1.93 at 95% confidence. The analytical application of the sensor for the quantification of DS in biological fluids as urine was investigated. The results were demonstrated as recovery percentages in the range 95±2.5-97±4.7% with relative standard deviation (RSD) of 0.5-1.5%.

Keywords: dianabol, determination, modified electrode, urine

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Authors: M. Ardelean, F. Manea, A. Pop, J. Schoonman

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The presence of pharmaceuticals in the environment and especially in water has gained increasing attention. They are included in emerging class of pollutants, and for most of them, legal limits have not been set-up due to their impact on human health and ecosystem was not determined and/or there is not the advanced analytical method for their quantification. In this context, the development of various advanced analytical methods for the quantification of pharmaceuticals in water is required. The electrochemical methods are known to exhibit the great potential for high-performance analytical methods but their performance is in direct relation to the electrode material and the operating techniques. In this study, two types of carbon-based electrodes materials, i.e., boron-doped diamond (BDD) and carbon nanofiber (CNF)-epoxy composite electrodes have been investigated through voltammetric techniques for the detection of naproxen in water. The comparative electrochemical behavior of naproxen (NPX) on both BDD and CNF electrodes was studied by cyclic voltammetry, and the well-defined peak corresponding to NPX oxidation was found for each electrode. NPX oxidation occurred on BDD electrode at the potential value of about +1.4 V/SCE (saturated calomel electrode) and at about +1.2 V/SCE for CNF electrode. The sensitivities for NPX detection were similar for both carbon-based electrode and thus, CNF electrode exhibited superiority in relation to the detection potential. Differential-pulsed voltammetry (DPV) and square-wave voltammetry (SWV) techniques were exploited to improve the electroanalytical performance for the NPX detection, and the best results related to the sensitivity of 9.959 µA·µM^-1 were achieved using DPV. In addition, the simultaneous detection of NPX and fluoxetine -a very common antidepressive drug, also present in water, was studied using CNF electrode and very good results were obtained. The detection potential values that allowed a good separation of the detection signals together with the good sensitivities were appropriate for the simultaneous detection of both tested pharmaceuticals. These results reclaim CNF electrode as a valuable tool for the individual/simultaneous detection of pharmaceuticals in water.

Keywords: boron-doped diamond electrode, carbon nanofiber-epoxy composite electrode, emerging pollutans, pharmaceuticals

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Authors: Gabriel Wosiak, Jeyse da Silva, Sthefany S. Sena, Renato N. de Andrade, Ernesto Pereira

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The bubble formation during hydrogen production by electrolysis and several electrochemical processes is an inherent phenomenon and can impact the energy consumption of the processes. In this work, it was reported both experimental and computational results describe the effect of bubble displacement, which, under the cases investigated, leads to the formation of a convective flow in the solution. The process is self-sustained, and a solution vortex is formed, which modifies the bubble growth and covering at the electrode surface. Using the experimental data, we have built a model to simulate it, which, with high accuracy, describes the phenomena. Then, it simulated many different experimental conditions and evaluated the effects of the boundary conditions on the bubble surface covering the surface. We have observed a position-dependent bubble covering the surface, which has an effect on the water-splitting efficiency. It was shown that the bubble covering is not uniform at the electrode surface, and using statistical analysis; it was possible to evaluate the influence of the gas type (H2 and O2), current density, and the bubble size (and cross-effects) on the covering fraction and the asymmetric behavior over the electrode surface.

Keywords: water splitting, bubble, electrolysis, hydrogen production

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Authors: Monisha Elumalai, Joana Guerreiro, Joana Carvalho, Marta Prado

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DNA biosensors popularity has been increasing over the past few years. Traditional analytical techniques tend to require complex steps and expensive equipment however DNA biosensors have the advantage of getting simple, fast and economic. Additionally, the combination of DNA biosensors with nanomaterials offers the opportunity to improve the selectivity, sensitivity and the overall performance of the devices. DNA biosensors are based on oligonucleotides as sensing elements. These oligonucleotides are highly specific to complementary DNA sequences resulting in the hybridization of the strands. DNA biosensors are not only an advantage in the clinical field but also applicable in numerous research areas such as food analysis or environmental control. Zebra Mussels (ZM), Dreissena polymorpha are invasive species responsible for enormous negative impacts on the environment and ecosystems. Generally, the detection of ZM is made when the observation of adult or macroscopic larvae's is made however at this stage is too late to avoid the harmful effects. Therefore, there is a need to develop an analytical tool for the early detection of ZM. Here, we present a portable plasmonic biosensor for the detection of environmental DNA (eDNA) released to the environment from this invasive species. The plasmonic DNA biosensor combines gold nanoparticles, as transducer elements, due to their great optical properties and high sensitivity. The detection strategy is based on the immobilization of a short base pair DNA sequence on the nanoparticles surface followed by specific hybridization in the presence of a complementary target DNA. The hybridization events are tracked by the optical response provided by the nanospheres and their surrounding environment. The identification of the DNA sequences (synthetic target and probes) to detect Zebra mussel were designed by using Geneious software in order to maximize the specificity. Moreover, to increase the optical response enzyme amplification of DNA might be used. The gold nanospheres were synthesized and characterized by UV-visible spectrophotometry and transmission electron microscopy (TEM). The obtained nanospheres present the maximum localized surface plasmon resonance (LSPR) peak position are found to be around 519 nm and a diameter of 17nm. The DNA probes modified with a sulfur group at one end of the sequence were then loaded on the gold nanospheres at different ionic strengths and DNA probe concentrations. The optimal DNA probe loading will be selected based on the stability of the optical signal followed by the hybridization study. Hybridization process leads to either nanoparticle dispersion or aggregation based on the presence or absence of the target DNA. Finally, this detection system will be integrated into an optical sensing platform. Considering that the developed device will be used in the field, it should fulfill the inexpensive and portability requirements. The sensing devices based on specific DNA detection holds great potential and can be exploited for sensing applications in-loco.

Keywords: ZM DNA, DNA probes, nicking enzyme, gold nanoparticles

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Authors: T. Abohalkuma, J. Telegdi

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Preparation, characterization, and application of self-assembled monolayers (SAM) formed by fluorophosphonic and undecenyl phosphonic acids on carbon steel surfaces as anticorrosive nanocoatings were demonstrated. The anticorrosive efficacy of these SAM layers was followed by atomic force microscopy, as the change in the surface morphology caused by layer deposition and corrosion processes was monitored. The corrosion process was determined by electrochemical potentiodynamic polarization, whereas the surface wettability of the carbon steel samples was tested with the use of static and dynamic contact angle measurements. Results showed that both chemicals produced good protection against corrosion as they performed as anodic inhibitors, especially with increasing the time of layer formation, which results in a more compact molecular film. According to the atomic force microscope (AFM) images, the fluoro-phosphonic acid self-assembled molecular layer can control the general as well as the pitting corrosion, but the SAM layers of the undecenyl-phosphonic acid cannot inhibit the pitting corrosion. The AFM and the contact angle measurements confirmed the results achieved by electrochemical measurements.

Keywords: nanolayers, corrosion, phosphonic acids, coatings

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Authors: Rinlee Butch M. Cervera, Princess Stephanie P. Llanos

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Lithium iron phosphate (LiFePO₄) is a potential cathode material for lithium-ion batteries due to its promising characteristics. In this study, pure LiFePO₄ (LFP) and carbon-coated nanograined LiFePO₄ (LFP-C) is synthesized and characterized for its microstructural properties. X-ray diffraction patterns of the synthesized samples can be indexed to an orthorhombic LFP structure with about 63 nm crystallite size as calculated by using Scherrer’s equation. Agglomerated particles that range from 200 nm to 300 nm are observed from scanning electron microscopy images. Transmission electron microscopy images confirm the crystalline structure of LFP and coating of amorphous carbon layer. Elemental mapping using energy dispersive spectroscopy analysis revealed the homogeneous dispersion of the compositional elements. In addition, galvanostatic charge and discharge measurements were investigated for the cathode performance of the synthesized LFP and LFP-C samples. The results showed that the carbon-coated sample demonstrated the highest capacity of about 140 mAhg^-1 as compared to non-coated and micrograined sized commercial LFP.

Keywords: ceramics, energy storage, electrochemical measurements, transmission electron microscope

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Authors: Sarmiza Stanca, Wolfgang Fritzsche, Christoph Krafft, Jürgen Popp

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Independent of the cell type a thin layer of a few nanometers thickness surrounds the cell interior as the cellular membrane. The transport of ions and molecules through the membrane is achieved in a very precise way by pores. Understanding the process of opening and closing the pores due to an electrochemical gradient across the membrane requires knowledge of the pore constitutive proteins. Recent reports prove the access to the molecular level of the cellular membrane by atomic force microscopy (AFM). This technique also permits an electrochemical study in the immediate vicinity of the tip. Specific molecules can be electrochemically localized in the natural cellular membrane. Our work aims to recognize the protein domains of the pores using an AFM probe as a miniaturized amperometric sensor, and to follow the protein behavior while changing the applied potential. The intensity of the current produced between the surface and the AFM probe is amplified and detected simultaneously with the surface imaging. The AFM probe plays the role of the working electrode and the substrate, a conductive glass on which the cells are grown, represent the counter electrode. For a better control of the electric potential on the probe, a third electrode Ag/AgCl wire is mounted in the circuit as a reference electrode. The working potential is applied between the electrodes with a programmable source and the current intensity in the circuit is recorded with a multimeter. The applied potential considers the overpotential at the electrode surface and the potential drop due to the current flow through the system. The reported method permits a high resolved electrochemical study of the protein domains on the living cell membrane. The amperometric map identifies areas of different current intensities on the pore depending on the applied potential. The reproducibility of this method is limited by the tip shape, the uncontrollable capacitance, which occurs at the apex and a potential local charge separation.

Keywords: AFM, sensor, membrane, pores, proteins

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Authors: Gopal Ji, Priyanka Dwivedi, Shanthi Sundaram, Rajiv Prakash

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Inhibition effect of aqueous Argemone Mexicana root extract (AMRE) on mild steel corrosion in 1 M HCl has been studied by weight loss, Tafel polarization curves, electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. Results indicate that inhibition ability of AMRE increases with the increasing amount of the extract. A maximum corrosion inhibition of 94% is acknowledged at the extract concentration of 400 mg L-1. Polarization curves and impedance spectra reveal that both cathodic and anodic reactions are suppressed due to passive layer formation at metal-acid interface. It is also confirmed by SEM micro graphs and FTIR studies. Furthermore, the effects of acid concentration (1-5 M), immersion time (120 hours) and temperature (30-60˚C) on inhibition potential of AMRE have been investigated by weight loss method and electrochemical techniques. Adsorption mechanism is also proposed on the basis of weight loss results, which shows good agreement with Langmuir isotherm.

Keywords: mild steel, polarization, SEM, acid corrosion, EIS, green inhibition

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Authors: Lucja Rodzik, Joanna Lewandowska-Lancucka, Michal Szuwarzynski, Krzysztof Szczubialka, Maria Nowakowska

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The analysis of nucleobases is of great importance for bioscience since their abnormal concentration in body fluids suggests the deficiency and mutation of the immune system, and it is considered to be an important parameter for diagnosis of various diseases. The presented conjugate meets the need for development of the effective, selective and highly sensitive sensor for nucleobase/nucleoside detection. The novel, highly fluorescent cadmium telluride quantum dots (CdTe QDs) functionalized with thymine and stabilized with thioglycolic acid (TGA) conjugates has been developed and thoroughly characterized. Successful formation of the material was confirmed by elemental analysis, and UV–Vis fluorescence and FTIR spectroscopies. The crystalline structure of the obtained product was characterized with X-ray diffraction (XRD) method. The composition of CdTe QDs and their thymine conjugate was also examined using X-ray photoelectron spectroscopy (XPS). The size of the CdTe-thymine was 3-6 nm as demonstrated using atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM) imaging. The plasmon resonance fluorescence band at 540 nm on excitation at 351 nm was observed for these nanoparticles. The intensity of this band increased with the increase in the amount of conjugated thymine with no shift in its position. Based on the fluorescence measurements, it was found that the CdTe-thymine conjugate interacted efficiently and selectively not only with adenine, a nucleobase complementary to thymine, but also with nucleosides and adenine-containing modified nucleosides, i.e., 5′-deoxy-5′-(methylthio)adenosine (MTA) and 2’-O-methyladenosine, the urinary tumor markers which allow monitoring of the disease progression. The applicability of the CdTe-thymine sensor for the real sample analysis was also investigated in simulated urine conditions. High sensitivity and selectivity of CdTe-thymine fluorescence towards adenine, adenosine and modified adenosine suggest that obtained conjugate can be potentially useful for development of the biosensor for complementary nucleobase/nucleoside detection.

Keywords: CdTe quantum dots, conjugate, sensor, thymine

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Authors: Imtiaz Ahmed Khan, Sabu John, Sania Waqar, Lijing Wang, Mac Fergusson, Ilija Najdovski

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Evolution of textiles, from its orthodox to more interactive role has stirred the researchers to uncover its application in numerous arenas. The idea of using textile based materials for wearable energy harvesting and storage devices have gained immense popularity. This is mainly due to textile comfort and flexibility features. In this work, nano-carbonous materials were infused on cellulosic fibers using caustic soda treatment. This paper presents the complete procedure of yarn supercapacitors fabrication process through dip coating technique and its characterization method. The main objective is to study, the effect of varying caustic soda concentration on mass loading of activated carbon on yarns and the related capacitance output of the designed yarn supercapacitor. Polyvinyl alcohol and Phosphoric acid were used as electrolyte in a two-electrode cell assembly to measure device electrochemical performance. The results show a promising increase in capacitance value using this technique.

Keywords: yarn supercapacitors, activated carbon, dip coating, caustic soda, electrolyte, electrochemical characterization

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Authors: A. Asselah, A. Khalfi, M. A.Toumi, A.Tazerouti

Abstract:

The study of the corrosion inhibition of a standard carbon steel "API 5L grade X70" by two biodegradable anionic surfactants derived from fatty acids by photo sulfochlorination, called sodium lauryl methyl ester sulfonates and sodium palmityl methyl ester sulfonates was carried. A solution at 2.5 g/l NaCl saturated with carbon dioxide is used as a corrosive medium. The gravimetric and electrochemical technics (stationary and transient) were used in order to quantify the rate of corrosion and to evaluate the electrochemical inhibition efficiency, thus the nature of the mode of action of the inhibitor, in addition to a surface characterization by scanning electron microscopy (MEB) coupled to energy dispersive X-ray spectroscopy (EDX). The variation of the concentration and the temperature were examined, and the mode of adsorption of these inhibitors on the surface of the metal was established by assigning it the appropriate isotherm and determining the corresponding thermodynamic parameters. The MEB-EDX allowed the visualization of good adhesion of the protective film formed by the surfactants to the surface of the steel. The corrosion inhibition was evaluated at around 93% for sodium lauryl methyl ester sulfonate surfactant at 20 ppm and 87.2% at 50 ppm for sodium palmityl methyl ester sulfonate surfactant.

Keywords: carbon steel, oilfield, corrosion, anionic surfactants

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Authors: Abdi Djamila, Haffar Hichem

Abstract:

The poly methylene bleu (PMB) has been successfully electro deposited on fluorine doped tin oxide (FTO) conducting glass as substrate. Its optical, electrical and photoelectrochemical characterizations have been carried out in order to show the performances of such polymer. The deposited film shows a good electric conductivity which is well confirmed by the low gap value determinated optically by UV–vis spectroscopy. Like all polymers the PMB presents an absorption difference in the visible range function of the polarization potential, it is expressed by the strong conjugation at oxidized state but is weakened with leucoform formation at reduced state. The electrochemical analysis of the films permit to show the cyclic voltamperogram with the anodic oxidation and cathodic reduction states of the polymer and to locate the corresponding energy levels HOMO and LUMO of this later. The electrochemical impedance spectroscopy permit to see the conductive character of such film and to calculate important parameters as Rtc and CPE. The study of the photoelectro activity of our polymer shows that under exposure to intermittent light source this later exhibit important photocurrents which enables it to be used in photo organic ells.

Keywords: polymethylene blue, electropolymerization, homo-lumo, photocurrents

Procedia PDF Downloads 252