Search results for: electrochemical analysis

Authors: Hubert Beisch, Janik Marx, Svenja Garlof, Roman Shvets, Ivan Grygorchak, Andriy Kityk, Bodo Fiedler

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Three-dimensional carbon materials can be used as electrode materials for energy storage systems such as batteries and supercapacitors. Fast charging and discharging times are realizable without reducing the performance due to aging processes. Furthermore high specific surface area (SSA) of three-dimensional carbon structures leads to high specific capacities. One newly developed carbon foam is Globugraphite. This interconnected globular carbon morphology with statistically distributed hierarchical pores is manufactured by a chemical vapor deposition (CVD) process from ceramic templates resulting from a sintering process. Via scanning electron (SEM) and transmission electron microscopy (TEM), the morphology is characterized. Moreover, the SSA was measured by the Brunauer–Emmett–Teller (BET) theory. Measurements of Globugraphite in an organic and inorganic electrolyte show high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. A comparison of the specific values is summarized in a Ragone diagram. Energy densities up to 48 Wh/kg and power densities to 833 W/kg could be achieved for an SSA from 376 m²/g to 859 m²/g. For organic electrolyte, a specific capacity of 100 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, carbon foam, CVD process, electrochemical cell, Ragone diagram, SEM, TEM

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Authors: K. Sushma Varma, Rajesh Singh

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Non-engineered landfills cause serious environmental damage due to toxic emissions and mobilization of persistent pollutants, organic and inorganic contaminants, as well as soluble metal ions. The available treatment technologies for landfill leachate and solid waste are not effective from an economic, environmental, and social standpoint. The present study assesses the potential of the bioelectrochemical system (BES) integrated with sulfate-reducing bacteria (SRB) in the sustainable treatment and decontamination of landfill wastes. For this purpose, solid waste and landfill leachate collected from different landfill sites were evaluated for long-term treatment using the integrated SRB-BES anaerobic designed bioreactors after pre-treatment. Based on periodic gas composition analysis, physicochemical characterization of the leachate and solid waste, and metal concentration determination, the present system demonstrated significant improvement in volumetric hydrogen production by suppressing methanogenesis. High reduction percentages of Be, Cr, Pb, Cd, Sb, Ni, Cr, COD, and sTOC removal were observed. This mineralization can be attributed to the synergistic effect of ammonia-assisted pre-treatment complexation and microbial sulphide formation. Despite being amended with 0.1N ammonia, the treated leachate level of NO³⁻ was found to be reduced along with SO₄²⁻. This integrated SRB-BES system can be recommended as an eco-friendly solution for landfill reclamation. The BES-treated solid waste was evidently more stabilized, as shown by a five-fold increase in surface area, and potentially useful for leachate immobilization and bio-fortification of agricultural fields. The vector arrangement and magnitude showed similar treatment with differences in magnitudes for both leachate and solid waste. These findings support the efficacy of SRB-BES in the treatment of landfill leachate and solid waste sustainably, inching a step closer to our sustainable development goals. It utilizes low-cost treatment, and anaerobic SRB adapted to landfill sites. This technology may prove to be a sustainable treatment strategy upon scaling up as its outcomes are two-pronged: landfill waste treatment and energy recovery.

Keywords: bio-electrochemical system, leachate /solid waste treatment, landfill leachate, sulfate-reducing bacteria

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Authors: Asiful H. Seikh, Jabair A. Mohammed, Ubair A. Samad, Mohammad A. Alam, Saeed M. Al-Zahrani, El-Sayed M. Sherif

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Three coating formulations were fabricated by incorporating different percentages of MIO (micaceous iron oxide ) (1, 2, and wt%) with ball-milled nanocrystalline Al (2 wt%) particles, which was optimized earlier. These coatings were characterized by means of different methods, namely, SEM, TGA, pendulum hardness, scratch test, and nano-indentation. The EIS measurements were carried out to report the effect of adding MIO powder in fabricated coatings on their corrosion behavior in 3.5 wt% NaCl solutions. In order to report the effect of immersion time on the corrosion and degradation of the prepared coatings, the EIS data were also acquired after various exposure periods of time, i.e., 1 h, 7 d, 14 d, 21 d, and 30 d in the test chloride solution. It has been found that the obtained EIS data for the fabricated coatings proved that the presence of 2% MIO provided the highest corrosion resistance amongst all coatings and that effect was recorded after all immersion periods of time. But, the MIO-incorporated coatings have less corrosion resistance than Al based epoxy coatings. It was also shown that with prolonged immersion, the resistance to corrosion declined after 7d, then with a longer period of immersion, i.e. 14 d, 21 d, and 30 d increases the resistance to corrosion by forming oxide products on the coatings surface. The results obtained from both mechanical and electrochemical testing confirmed that the fabricated coating with 2 wt% Al exhibited better hardness and higher resistance to corrosion as compared to coatings with 1 wt% Al and 3 wt% Al.

Keywords: epoxy coatings, nanomaterials, corrosion resistance, EIS, nanoindentation

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Authors: Ádám Vass, István Bakos, Irina Borbáth, Zoltán Pászti, István Sajó, András Tompos

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Important requirements for the anode side electrocatalysts of polymer electrolyte membrane (PEM) fuel cells are CO-tolerance, stability and corrosion resistance. Carbon is still the most common material for electrocatalyst supports due to its low cost, high electrical conductivity and high surface area, which can ensure good dispersion of the Pt. However, carbon becomes degraded at higher potentials and it causes problem during application. Therefore it is important to explore alternative materials with improved stability. Molybdenum-oxide can improve the CO-tolerance of the Pt/C catalysts, but it is prone to leach in acidic electrolyte. The Mo was stabilized by isovalent substitution of molybdenum into the rutile phase titanium-dioxide lattice, achieved by a modified multistep sol-gel synthesis method optimized for preparation of Ti0.7Mo.3O2-C composite. High degree of Mo incorporation into the rutile lattice was developed. The conductivity and corrosion resistance across the anticipated potential/pH window was ensured by mixed oxide – activated carbon composite. Platinum loading was carried out using NaBH4 and ethylene glycol; platinum content was 40 wt%. The electrocatalyst was characterized by both material investigating methods (i.e. XRD, TEM, EDS, XPS techniques) and electrochemical methods (cyclic-voltammetry, COads stripping voltammetry, hydrogen oxidation reaction on rotating disc electrode). The electrochemical activity of the sample was compared to commercial 40 wt% Pt/C (Quintech) and PtRu/C (Quintech, Pt= 20 wt%, Ru= 10 wt%) references. Enhanced CO tolerance of the electrocatalyst prepared using the Ti0.7Mo.3O2-C composite material was evidenced by the appearance of a CO-oxidation related 'pre-peak' and by the pronounced shift of the maximum of the main CO oxidation peak towards less positive potential compared to Pt/C. Fuel cell polarization measurements were also carried out using Bio-Logic and Paxitech FCT-150S test device. All details on the design, preparation, characterization and testing by both electrochemical measurements and fuel cell test device of electrocatalyst supported on Ti0.7Mo.3O2-C composite material will be presented and discussed.

Keywords: anode electrocatalyst, composite material, CO-tolerance, TiMoOx

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Authors: Indu Elizabeth

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Antimony/Multi Walled Carbon nano tube nanocomposite (Sb/MWCNT) is synthesized using ethylene glycol mediated reduction process. Binder free, self-supporting and flexible Sb/MWCNT nanocomposite paper has been prepared by employing the vacuum filtration technique. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy (RS), and thermal gravimetric analysis (TGA) to evaluate the structure of anode and tested for its performance in a Lithium rechargeable cell. Electrochemical measurements demonstrate that the Sb/MWCNT composite paper anode delivers a specific discharge capacity of ~400 mAh g-1 up to a current density of 100 mA g-1.

Keywords: antimony, lithium ion battery, multiwalled carbon nanotube, specific capacity

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Authors: R. Sharma, A. Sil, S. Ray

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Nanocomposites gel polymer electrolytes are gaining more and more attention among the researchers worldwide due to their possible applications in various electrochemical devices particularly in solid-state Li-ion batteries. In this work we have investigated the effect of nanofibers on the electrical properties of PVDF-HFP based gel electrolytes. The nanocomposites polymer electrolytes have been synthesized by solution casting technique with 10wt% of ZrO2. By analysis of impedance spectroscopy it has been demonstrated that the incorporation of ZrO2 into PVDF-HFP–(PC+DEC)–LiClO4 gel polymer electrolyte system significantly enhances the ionic conductivity of the electrolyte. The enhancement of ionic conductivity seems to be correlated with the fact that the dispersion of ZrO2 to PVDF-HFP prevents polymer chain reorganization due to the high aspect ratio of ZrO2, resulting in reduction in polymer crystallinity, which gives rise to an increase in ionic conductivity. The decrease of crystallinity of PVDF-HFP due the addition of ZrO2 has been confirmed by XRD. The interaction of ZrO2 with various constituents of polymer electrolytes has been studied by FTIR spectroscopy. TEM results show that the fillers (ZrO2) has distributed uniformly in the polymer electrolytes. Moreover, ZrO2 added gel polymer electrolytes offer better thermal stability as compared to that of ZrO2 free electrolytes as confirmed by TGA analysis.

Keywords: polymer electrolytes, ZrO2, ionic conductivity, FTIR

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Authors: Nikki A. Barla, P. K. Ghosh, Sourav Das

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Two different groove sizes 13.6 mm (narrow groove) and 7.5 mm (ultra-narrow groove) of 304 LN austenitic stainless steel (ASS) plate was welded using pulse gas metal arc welding (P-GMAW). These grooves were welded using multi-pass single seam per layer (MSPPL) deposition technique with full assurance of groove wall fusion. During bead on plate deposition process, the thermal cycle was recorded using strain buster (temperature measuring device). Both the groove has heat affected Zone (HAZ) width of 1-2 mm. After welding, the microstructure studies was done which revealed that there was higher sensitization (Chromium carbide formation in grain boundary) in the HAZ of 13.6 mm groove weldment as compared to the HAZ of 7.5 mm weldment. Electrochemical potentiokinetic reactivation test (EPR) was done in 0.5 N H₂SO₄ + 1 M KSCN solution to study the degree of sensitization (DOS) and it was observed that 7.5 mm groove HAZ has lower DOS. Mass deposition in the 13.6 mm weld is higher than 7.5mm groove weld, which naturally induces higher residual stress in 13.6 mm weld. Comparison between microstructural studies and corrosion test summarized that the residual stress affects the sensitization property of welded ASS.

Keywords: austenitic stainless steel (ASS), electrochemical potentiokinetic reactivation test (EPR), microstructure, pulse gas metal arc welding (P-GMAW), sensitization

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Authors: Wenxin Mei, Jinhua Sun, Qingsong Wang

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The volume expansion of lithium-ion batteries is mainly induced by intercalation induced stress within the negative electrode, resulting in capacity degradation and even battery failure. Stress generation due to lithium intercalation into graphite particles is investigated based on an electrochemical-mechanical model in this work. The two-dimensional model presented is fully coupled, inclusive of the impacts of intercalation-induced stress, stress-induced intercalation, to evaluate the lithium concentration, stress generation, and displacement intra and inter-particle. The results show that the distribution of lithium concentration and stress exhibits an analogous pattern, which reflects the relation between lithium diffusion and stress. The results of inter-particle stress indicate that larger Von-Mises stress is displayed where the two particles are in contact with each other, and deformation at the edge of particles is also observed, predicting fracture. Additionally, the maximum inter-particle stress at the end of lithium intercalation is nearly ten times the intraparticle stress. And the maximum inter-particle displacement is increased by 24% compared to the single-particle. Finally, the effect of graphite particle arrangement on inter-particle stress is studied. It is found that inter-particle stress with tighter arrangement exhibits lower stress. This work can provide guidance for predicting the intra and inter-particle stress to take measures to avoid cracking of electrode material.

Keywords: electrochemical-mechanical model, graphite particle, lithium concentration, lithium ion battery, stress

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Authors: M. S. Ashraf, Raja Rizwan Hussain, A. M. Alhozaimy, A. I. Al-Negheimish

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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 which are the compounds commonly observed in ordinary portland cement concrete pore solution. In addition to that, commonly used mineral admixtures (silica fume, natural pozzolan and fly ash) were also added to the simulated concrete pore solution. 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, silica fume has been shown to have a negative influence on the film quality though it has positive effect on the concrete properties. Fly ash and natural pozzolan increase the protective qualities of the passive film. The research data in this area is very limited in the past and needed further investigation.

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

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Authors: Mariana-Dana Damaceanu

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Electrochemical oxidation is one of the most convenient ways to obtain conjugated polymer films as polypyrrole, polyaniline, polythiophene or polycarbazole. The research in the field has been mainly directed to the study of electrical conduction properties of the materials obtained by electropolymerization, often the main reason being their use as electroconducting electrodes, and very little attention has been paid to the morphological and optical quality of the films electrodeposited on flat surfaces. Electropolymerization of the monomer solution was scarcely used in the past to manufacture polymer-based light-emitting diodes (PLED), most probably due to the difficulty of obtaining defectless polymer films with good mechanical and optical properties, or conductive polymers with well controlled molecular weights. Here we report our attempts in using electrochemical deposition as appropriate method for preparing ultrathin films of fluorene-based polymers for PLED applications. The properties of these films were evaluated in terms of structural morphology, optical properties, and electrochemical conduction. Thus, electropolymerization of 4,4'-(9-fluorenylidene)-dianiline was performed in dichloromethane solution, at a concentration of 10-2 M, using 0.1 M tetrabutylammonium tetrafluoroborate as electrolyte salt. The potential was scanned between 0 and 1.3 V on the one hand, and 0 - 2 V on the other hand, when polymer films with different structures and properties were obtained. Indium tin oxide-coated glass substrate of different size was used as working electrode, platinum wire as counter electrode and calomel electrode as reference. For each potential range 100 cycles were recorded at a scan rate of 100 mV/s. The film obtained in the potential range from 0 to 1.3 V, namely poly(FDA-NH), is visible to the naked eye, being light brown, transparent and fluorescent, and displays an amorphous morphology. Instead, the electrogrowth poly(FDA) film in the potential range of 0 - 2 V is yellowish-brown and opaque, presenting a self-assembled structure in aggregates of irregular shape and size. The polymers structure was identified by FTIR spectroscopy, which shows the presence of broad bands specific to a polymer, the band centered at approx. 3443 cm-1 being ascribed to the secondary amine. The two polymer films display two absorption maxima, at 434-436 nm assigned to π-π* transitions of polymers, and another at 832 and 880 nm assigned to polaron transitions. The fluorescence spectra indicated the presence of emission bands in the blue domain, with two peaks at 422 and 488 nm for poly (FDA-NH), and four narrow peaks at 422, 447, 460 and 484 nm for poly(FDA), peaks originating from fluorene-containing segments of varying degrees of conjugation. Poly(FDA-NH) exhibited two oxidation peaks in the anodic region and the HOMO energy value of 5.41 eV, whereas poly(FDA) showed only one oxidation peak and the HOMO level localized at 5.29 eV. The electrochemical data are discussed in close correlation with the proposed chemical structure of the electrogrowth films. Further research will be carried out to study their use and performance in light-emitting devices.

Keywords: electrogrowth polymer films, fluorene, morphology, optical properties

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Authors: Shiying Fan, Xinyong Li

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

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

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Authors: Neşe Taşci, Soner Çubuk, Ece Kök Yetimoğlu, M. Vezir Kahraman

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Bisphenol-A (BPA), 2,2-bis(4-hydroxyphenly)propane, is one of the highest usage volume chemicals in the world. Studies showed that BPA maybe has negative effects on the central nervous system, immune and endocrine systems. Several of analytical methods for the analysis of BPA have been reported including electrochemical processes, chemical oxidation, ozonization, spectrophotometric, chromatographic techniques. Compared with other conventional analytical techniques, optic sensors are reliable, providing quick results, low cost, easy to use, stands out as a much more advantageous method because of the high precision and sensitivity. In this work, a new photocured polymeric fluorescence sensor was prepared and characterized for Bisphenol-A (BPA) analysis. Characterization of the membrane was carried out by Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR) and Scanning Electron Microscope (SEM) techniques. The response characteristics of the sensor including dynamic range, pH effect and response time were systematically investigated. Acknowledgment: This work was supported by the Scientific and Technological Research Council of Turkey (TUBITAK) under Grant 115Y469.

Keywords: bisphenol-a, fluorescence, photopolymerization, polymeric sensor

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Authors: Zakaria Ahmed, Khaled Charradi, Sherif M. A. S. Keshk, Radhouane Chtourou

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Sulfonated poly ether ether ketone (SPEEK) with a low sulfonation degree was blended using nanofiller Layered Double Hydroxide (LDH, Mg2AlCl) /sepiolite nanostructured material as additive to use as an electrolyte membrane for fuel cell application. Characterization assessments, i.e., mechanical stability, thermal gravimetric analysis, ion exchange capability, swelling properties, water uptake capacities, electrochemical impedance spectroscopy analysis, and Fourier transform infrared spectroscopy (FTIR) of the composite membranes were conducted. The presence of LDH/sepiolite nanoarchitecture material within SPEEK was found to have the highest water retention and proton conductivity value at high temperature rather than LDH/SPEEK and pristine SPEEK membranes.

Keywords: SPEEK, sepiolite clay, LDH clay, proton exchange membrane

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Authors: Bryan D. Llenarizas, Maria Carla F. Manzano

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The rapid growth of electricity demand has led to a pursuit of alternative energy sources with high power output and not harmful to the environment. The fuel cell is a device that generates electricity via chemical reactions between the fuel and oxidant. Fuel cells have been known for decades, but the development of high-power output and durability was still one of the drawbacks of this energy source. This study investigates the potential of layer-by-layer composite for fuel cell applications. A two-electrode electrochemical cell was used for the galvanostatic electrochemical deposition method to fabricate a Polypyrrole/rGO|Polypyrrole/ZnO layer-by-layer composite material for fuel cell applications. In the synthesis, the first layer comprised 0.1M pyrrole monomer and 1mg of rGO, while the second layer had 0.1M pyrrole monomer and variations of ZnO concentration ranging from 0.08M up to 0.12M. A constant current density of 8mA/cm² was applied for 1 hour in fabricating each layer. Scanning electron microscopy (SEM) for the fabricated LBL material shows a globular surface with white spots. These white spots are the ZnO particles confirmed by energy-dispersive X-ray spectroscopy, indicating a successful deposition of the second layer onto the first layer. The observed surface morphology was consistent for each variation of ZnO concentrations. AC measurements were conducted to obtain the AC resistance of the fabricated film. Results show a decrease in AC resistance as the concentration of ZnO increases.

Keywords: anode, composite material, electropolymerization, fuel cell, galvanostatic, polypyrrole

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Authors: Maryam Kiani

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This study focuses on the development of composite nanomaterials based on SiO₂ and carbon black for oxygen reduction reaction (ORR) electrocatalysts in batteries and fuel cells. The aim was to explore the potential of these composite materials as efficient catalysts for ORR, which is a critical process in energy conversion devices. The SiO₂/carbon black composite nanomaterials were synthesized using a facile and scalable method. The morphology, structure, and electrochemical properties of the materials were characterized using various techniques including scanning electron microscopy (SEM), X-ray diffraction (XRD), and electrochemical measurements. The results demonstrated that the incorporation of SiO₂ into the carbon black matrix enhanced the ORR performance of the composite material. The composite nanomaterials exhibited improved electrocatalytic activity, enhanced stability, and increased durability compared to pure carbon black. The presence of SiO₂ facilitated the formation of active sites, improved electron transfer, and increased the surface area available for ORR. This study contributes to the advancement of battery and fuel cell technology by offering a promising approach for the development of high-performance ORR electrocatalysts. The SiO₂/carbon black composite nanomaterials show great potential for improving the efficiency and durability of energy conversion devices, leading to more sustainable and efficient energy solutions.

Keywords: ORR, fuel cells, batteries, electrocatalyst

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Authors: Mehak Munjal, Raj Kishore Sharma, Gurmeet Singh

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Microbial Fuel Cells (MFCs) are an alternative sustainable approach that utilize bacteria present in waste water as a bio-catalyst for the production of energy. It is a promising growing technology with minimal requirement for chemical supplements. Here electrode material plays a vital role in its performance. The present study represents CoFe2O4 spinel as a novel anode material in the MFC. It not only improve the bacterial metabolics but also enhance the power output. Generally, biocompatible conductive carbon paper/cloth, graphite and stainless steel are utilised as anode in MFCs. However, these materials lack electrochemical activity for anodic microbial reaction. Therefore, we developed CoFe2O4 on graphite sheet which enhanced the anodic charge transfer process. Redox pair in CoFe2O4 helped in improvement of extracellular electron transfer, thereby enhancing the performance. The physical characterizations (FT-IR, XRD, Raman) and electrochemical measurements demonstrate the strong interaction with E.coli bacteria and thus providing an excellent power density i.e. 1850 mW/m2 .The maximum anode half -cell potential is measured to be 0.65V. Therefore, use of noble metal free anodic material further decrease the cost and the long term cell stability makes it an effective material for practical applications.

Keywords: microbial fuel cell, cobalt ferrite, E. coli, bioelectricity

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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: Malek Mahmoudi, Jonas Keruckas, Dmytro Volyniuk, Jurate Simokaitiene, Juozas V. Grazulevicius

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Host materials have been discovered as one of the most appealing methods for harvesting triplet states in organic materials for application in organic light-emitting diodes (OLEDs). The ideal host-guest system for emission in thermally delayed fluorescence OLEDs with 20% guest concentration for efficient energy transfer has been demonstrated in the present investigation. In this work, 3,3'-bis[9-(4-fluorophenyl) carbazole] (bFPC) has been used as the host, which induces balanced charge carrier transport for high-efficiency OLEDs.For providing a complete characterization of the synthesized compound, photophysical, photoelectrical, charge-transporting, and electrochemical properties of the compound have been examined. Excited-state lifetimes and singlet-triplet energy gaps were measured for characterization of photophysical properties, while thermogravimetric analysis, as well as differential scanning calorimetry measurements, were performed for probing of electrochemical and thermal properties of the compound. The electrochemical properties of this compound were investigated by cyclic voltammetry (CV) method, and ionization potential (IPCV) value of 5.68 eV was observed. UV–Vis absorption and photoluminescence spectrum of a solution of the compound in toluene (10-5 M) showed maxima at 302 and 405 nm, respectively. Photoelectron emission spectrometry was used for the characterization of charge-injection properties of the studied compound in solid. The ionization potential of this material was found to be 5.78 eV, and time-of-flight measurement was used for testing charge-transporting properties and hole mobility estimated using this technique in a vacuum-deposited layer reached 4×10-4 cm2 V-1s-1. Since the compound with high charge mobilities was tested as a host in an organic light-emitting diode. The device was fabricated by successive deposition onto a pre-cleaned indium tin oxide (ITO) coated glass substrate under a vacuum of 10-6 Torr and consisting of an indium-tin-oxide anode, hole injection and transporting layer(MoO3, NPB), emitting layer with bFPC as a host and 4CzIPN (2,4,5,6-tetra(9-carbazolyl)isophthalonitrile) which is a new highly efficient green thermally activated delayed fluorescence (TADF) material as an emitter, an electron transporting layer(TPBi) and lithium fluoride layer topped with aluminum layer as a cathode exhibited the highest maximum current efficiency and power efficiency of 33.9 cd/A and 23.5 lm/W, respectively and the electroluminescence spectrum showed only a peak at 512nm. Furthermore, the new bicarbazole-based compound was tested as a host in thermally activated delayed fluorescence organic light-emitting diodes are reaching luminance of 25300 cd m-2 and external quantum efficiency of 10.1%. Interestingly, the turn-on voltage was low enough (3.8 V), and such a device can be used for highly efficient light sources.

Keywords: thermally-activated delayed fluorescence, host material, ionization energy, charge mobility, electroluminescence

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Authors: Muhammad Hassan, Kemal Celebi

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Developing a highly efficient electrochromic energy storage device with sufficient color fluctuation and significant electrochemical performance is highly desirable for practical energy-saving applications. Here, to achieve a highly stable material with a large electrochemical storage capacity, a W₁₈O₄₉ NW/Ti₃C₂Tₓ composite has been fabricated and deposited on a pre-assembled Ag and W₁₈O₄₉ NW conductive network by Langmuir-Blodgett technique. The resulting hybrid electrode composed of 15 layers of W₁₈O₄₉ NW/Ti₃C₂Tₓ exhibits an areal capacitance of 125 mF/cm², with a fast and reversible switching response. An optical modulation of 98.2% can be maintained at a current density of 5 mAcm⁻². Using this electrode, we fabricated a bifunctional symmetric electrochromic supercapacitor device having an energy density of 10.26 μWh/cm² and a power density of 0.605 mW/cm², with high capacity retention and full columbic efficiency over 4000 charge-discharge cycles. Meanwhile, the device displays remarkable electrochromic characteristics, including fast switching time (5 s for coloring and 7 s for bleaching) and a significant coloration efficiency of 116 cm²/C with good optical modulation stability. In addition, the device exhibits remarkable mechanical flexibility and fast switching while being stable over 100 bending cycles, which is promising for real-world applications.

Keywords: MXene, nanowires, supercapacitor, ion diffusion, electrochromic, coloration efficiency

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

Abstract:

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: Maryam Kiani

Abstract:

This study focuses on the development of composite nanomaterials based on SiO2 and carbon black for oxygen reduction reaction (ORR) electrocatalysts in batteries and fuel cells. The aim was to explore the potential of these composite materials as efficient catalysts for ORR, which is a critical process in energy conversion devices. The SiO2/carbon black composite nanomaterials were synthesized using a facile and scalable method. The morphology, structure, and electrochemical properties of the materials were characterized using various techniques, including scanning electron microscopy (SEM), X-ray diffraction (XRD), and electrochemical measurements. The results demonstrated that the incorporation of SiO2 into the carbon black matrix enhanced the ORR performance of the composite material. The composite nanomaterials exhibited improved electrocatalytic activity, enhanced stability, and increased durability compared to pure carbon black. The presence of SiO2 facilitated the formation of active sites, improved electron transfer, and increased the surface area available for ORR. This study contributes to the advancement of battery and fuel cell technology by offering a promising approach for the development of high-performance ORR electrocatalysts. The SiO2/carbon black composite nanomaterials show great potential for improving the efficiency and durability of energy conversion devices, leading to more sustainable and efficient energy solutions.

Keywords: oxygen reduction reaction, batteries, fuel cells, electrrocatalyst

Procedia PDF Downloads 67

Authors: Zohreh Derikvand, Hadis Cheraghi, Azadeh Azadbakht, Vaclav Eigner, Michal Dusek

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Two new one and two dimensional metal organic coordination polymers of Cu(II), [Cu(3-nph)2(H2O)2pz]n (1) and Ag(I), {[Ag(3-nph)pz].H2O}n (2) with pyrazine (pz) and 3- nitrophthalic acid (3-nph) have been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. We used these compounds to preparation modified electrode with Au/Pt nanosparticles in order to investigation electrochemistry and electrocatalysis activities. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). The Ag(I) coordination polymer shows a 2D layer structure constructed from dinuclear silver (I) building blocks in which two crystallographically Ag+ ions are connected to each other by a covalent bond. The pyrazine ligands adopt μ2 bridging modes, linking the metal centers into a one and two -dimensional coordination framework in 1 and 2. The two AgI cations are surrounded by pyrazine and 3-nitrophthalate mono anions and indicate distorted tetrahedral geometry. In the crystal structures of Ag(I) complex there are non-classical hydrogen bonding arrangements, C–O•••π and π–π stacking interactions. In Cu(II) coordination polymer, the coordination geometry around Cu(II) atom is a distorted octahedron. Interestingly, the structural analysis illustrates that the strong and weak hydrogen bond accompanied with C–H•••π and C–O•••π stacking interactions assemble the crystal structure of 1 and 2 into fascinating 3D supramolecular architecture.

Keywords: 3-nithrophethalic acid, crystal structure, coordination polymer, electrocatalysis

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Authors: Alejandra Martin-Dominguez, Javier Canto-Rios, Velitchko Tzatchkov

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Electrocoagulation is a water treatment technology that consists of generating coagulant species in situ by electrolytic oxidation of sacrificial anode materials triggered by electric current. It removes suspended solids, heavy metals, emulsified oils, bacteria, colloidal solids and particles, soluble inorganic pollutants and other contaminants from water, offering an alternative to the use of metal salts or polymers and polyelectrolyte addition for breaking stable emulsions and suspensions. The method essentially consists of passing the water being treated through pairs of consumable conductive metal plates in parallel, which act as monopolar electrodes, commonly known as ‘sacrificial electrodes’. Physicochemical, electrochemical and hydraulic processes are involved in the efficiency of this type of treatment. While the physicochemical and electrochemical aspects of the technology have been extensively studied, little is known about the influence of the hydraulics. However, the hydraulic process is fundamental for the reactions that take place at the electrode boundary layers and for the coagulant mixing. Electrocoagulation reactors can be open (with free water surface) and closed (pressurized). Independently of the type of rector, hydraulic head loss is an important factor for its design. The present work focuses on the study of the total hydraulic head loss and flow velocity and pressure distribution in electrocoagulation reactors with single or multiple concentric annular cross sections. An analysis of the head loss produced by hydraulic wall shear friction and accessories (minor head losses) is presented, and compared to the head loss measured on a semi-pilot scale laboratory model for different flow rates through the reactor. The tests included laminar, transitional and turbulent flow. The observed head loss was compared also to the head loss predicted by several known conceptual theoretical and empirical equations, specific for flow in concentric annular pipes. Four single concentric annular cross section and one multiple concentric annular cross section reactor configuration were studied. The theoretical head loss resulted higher than the observed in the laboratory model in some of the tests, and lower in others of them, depending also on the assumed value for the wall roughness. Most of the theoretical models assume that the fluid elements in all annular sections have the same velocity, and that flow is steady, uniform and one-dimensional, with the same pressure and velocity profiles in all reactor sections. To check the validity of such assumptions, a computational fluid dynamics (CFD) model of the concentric annular pipe reactor was implemented using the ANSYS Fluent software, demonstrating that pressure and flow velocity distribution inside the reactor actually is not uniform. Based on the analysis, the equations that predict better the head loss in single and multiple annular sections were obtained. Other factors that may impact the head loss, such as the generation of coagulants and gases during the electrochemical reaction, the accumulation of hydroxides inside the reactor, and the change of the electrode material with time, are also discussed. The results can be used as tools for design and scale-up of electrocoagulation reactors, to be integrated into new or existing water treatment plants.

Keywords: electrocoagulation reactors, hydraulic head loss, concentric annular pipes, computational fluid dynamics model

Procedia PDF Downloads 199

Authors: Sabina Żołędowska, Tadeusz Ossowski, Robert Bogdanowicz, Jacek Ryl, Paweł Rostkowski, Michał Kruczkowski, Michał Sobaszek, Zofia Cebula, Grzegorz Skowierzak, Paweł Jakóbczyk, Lilit Hovhannisyan, Paweł Ślepski, Iwona Kaczmarczyk, Mattia Pierpaoli, Bartłomiej Dec, Dawid Nidzworski

Abstract:

The circular economy of water presents a pressing environmental challenge in our society. Water contains various harmful substances, such as drugs, antibiotics, hormones, and dioxides, which can pose silent threats. Water pollution has severe consequences for aquatic ecosystems. It disrupts the balance of ecosystems by harming aquatic plants, animals, and microorganisms. Water pollution poses significant risks to human health. Exposure to toxic chemicals through contaminated water can have long-term health effects, such as cancer, developmental disorders, and hormonal imbalances. However, effective remediation systems can be implemented to remove these contaminants using electrocatalytic processes, which offer an environmentally friendly alternative to other treatment methods, and one of them is the innovative iCLARE system. The project's primary focus revolves around a few main topics: Reactor design and construction, selection of a specific type of reticulated vitreous carbon foams (RVC), analytical studies of harmful contaminants parameters and AI implementation. This high-performance electrochemical reactor will be build based on a novel type of electrode material. The proposed approach utilizes the application of reticulated vitreous carbon foams (RVC) with deposited modified metal oxides (MMO) and diamond thin films. The following setup is characterized by high surface area development and satisfactory mechanical and electrochemical properties, designed for high electrocatalytic process efficiency. The consortium validated electrode modification methods that are the base of the iCLARE product and established the procedures for the detection of chemicals detection: - deposition of metal oxides WO3 and V2O5-deposition of boron-doped diamond/nanowalls structures by CVD process. The chosen electrodes (porous Ferroterm electrodes) were stress tested for various parameters that might occur inside the iCLARE machine–corosis, the long-term structure of the electrode surface during electrochemical processes, and energetic efficacy using cyclic polarization and electrochemical impedance spectroscopy (before and after electrolysis) and dynamic electrochemical impedance spectroscopy (DEIS). This tool allows real-time monitoring of the changes at the electrode/electrolyte interphase. On the other hand, the toxicity of iCLARE chemicals and products of electrolysis are evaluated before and after the treatment using MARA examination (IBMM) and HPLC-MS-MS (NILU), giving us information about the harmfulness of using electrode material and the efficiency of iClare system in the disposal of pollutants. Implementation of data into the system that uses artificial intelligence and the possibility of practical application is in progress (SensDx).

Keywords: waste water treatement, RVC, electrocatalysis, paracetamol

Procedia PDF Downloads 52

Authors: Navpreet Kaur, Himkusha Thakur, Nirmal Prabhakar

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

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

Procedia PDF Downloads 427

Authors: Raj Kumar Rajak, Bharat Mishra

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Bio-battery represents an entirely new long term, reasonable, reachable and ecofriendly approach to production of sustainable energy. Types of batteries have been developed using MnO₂ in various ways. MnO₂ is suitable with physical, chemical, electrochemical, and catalytic properties, serving as an effective cathodic depolarizer and may be considered as being the life blood of the battery systems. In the present experimental work, we have studied the effect of generation of power by bio-battery using different concentrations of MnO₂. The tests show that it is possible to generate electricity using cow’s urine as an electrolyte. After ascertaining the optimum concentration of MnO₂, various battery parameters and performance indicates that cow urine solely produces power of 695 mW, while a combination with MnO₂ (40%) enhances power of bio-battery, i.e. 1377 mW. On adding more and more MnO₂ to the electrolyte, the power suppressed because inflation of internal resistance. The analysis of the data produced from experiment shows that MnO₂ is quite suitable to energize the bio-battery.

Keywords: bio-batteries, cow’s urine, manganese dioxide, non-conventional

Procedia PDF Downloads 232

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: Aida Rafat, Ramazan Kahraman, Mert Atilhan

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The aggressive corrosion behavior of conventional amine solvents is one of main barriers against large scale commerizaliation of amine absorption process for carbon capture application. Novel CO2 absorbents that exhibit minimal corrosivity against operation conditions are essential to lower corrosion damage and control and ensure more robustness in the capture plant. This work investigated corrosion behavior of carbon steel CS1018 in various CO2 absrobent solvents. The tested solvents included the classical amines MEA, DEA and MDEA, piperazine activated solvents MEA/PZ, MDEA/PZ and MEA/MDEA/PZ as well as mixtures of MEA and Room Temperature Ionic Liquids RTIL, namely MEA/[C4MIM][BF4] and MEA/[C4MIM][Otf]. Electrochemical polarization technique was used to determine the system corrosiveness in terms of corrosion rate and polarization behavior. The process parameters of interest were CO2 loading and solution temperature. Electrochemical resulted showed corrosivity order of classical amines at 40°C is MDEA> MEA > DEA wherase at 80°C corrosivity ranking changes to MEA > DEA > MDEA. Corrosivity rankings were mainly governed by CO2 absorption capacity at the test temperature. Corrosivity ranking for activated amines at 80°C was MEA/PZ > MDEA/PZ > MEA/MDEA/PZ. Piperazine addition seemed to have a dual advanatge in terms of enhancing CO2 absorption capacity as well as nullifying corrosion. For MEA/RTIL mixtures, the preliminary results showed that the partial repalcement of aqueous phase in MEA solution by the more stable nonvolatile RTIL solvents reduced corrosion rates considerably.

Keywords: corrosion, amines, CO2 capture, piperazine, ionic liquids

Procedia PDF Downloads 439

Authors: Sajad Haghanifar, Seyed-Farshid Kashani Bozorg

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Nano-crystalline Mg2Ni-based powder was produced by mechanical alloying technique using binary and ternary powder mixtures with stoichiometric compositions of Mg2Ni, Mg1.9C0.1Ni and Mg2C0.1Ni0.9. The structures and morphologies of the milled products were studied by XRD, SEM and HRTEM. Their electrochemical hydrogen storage characteristics were investigated in 6 M KOH solution. X-Ray diffraction, scanning and transmission electron microscopy of the milled products showed the formation of Mg2Ni-based nano-crystallites after 5, 15 and 30 h of milling using the initial powder mixtures of Mg1.9C0.1Ni, Mg2Ni and Mg2C0.1Ni0.9, respectively. It was found that partial substitution of C for Mg has beneficial effect on the formation kinetic of nano-crystalline Mg2Ni. Contrary to this, partial substitution of C for Ni was resulted in retardation of formation kinetic of nano-crystalline Mg2Ni. In addition, the negative electrode made from Mg1.9C0.1Ni ternary milled product after 30 hour of milling exhibited the highest initial discharge capacity and longest discharge life. Thus, partial substitution of C for Mg is beneficial to electrode properties of the Mg2Ni-based crystallites. The relation between the discharge capacity and cycling number of mechanically alloyed products was proposed on the basis of the fact that the degradation of discharge capacity was mainly caused by the oxidation of magnesium and nickel. The experimental data fitted the deduced equation well.

Keywords: Mg2Ni, hydrogen absorbing materials, electrochemical properties, nano-crystalline, amorphous, mechanical alloying, carbon

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Authors: Samaneh Nabavi, Hadi Shirzad, Arash Ghoorchian, Maryam Shanesaz, Reza Naderi

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Morphine (MO), the most effective painkiller, is considered the reference by which analgesics are assessed. It is very necessary for the biomedical applications to detect and maintain the MO concentrations in the blood and urine with in safe ranges. To date, there are many expensive techniques for detecting MO. Recently, many electrochemical sensors for direct determination of MO were constructed. The molecularly imprinted polymer (MIP) is a polymeric material, which has a built-in functionality for the recognition of a particular chemical substance with its complementary cavity.This paper reports a sensor for MO using a combination of a molecularly imprinted polymer (MIP) and differential-pulse voltammetry (DPV). Electropolymerization of MO doped polypyrrole yielded poor quality, but a well-doped, nanostructure and increased impregnation has been obtained in the pH=12. Above a pH of 11, MO is in the anionic forms. The effect of various experimental parameters including pH, scan rate and accumulation time on the voltammetric response of MO was investigated. At the optimum conditions, the concentration of MO was determined using DPV in a linear range of 7.07 × 10−6 to 2.1 × 10−4 mol L−1 with a correlation coefficient of 0.999, and a detection limit of 13.3 × 10-8 mol L−1, respectively. The effect of common interferences on the current response of MO namely ascorbic acid (AA) and uric acid (UA) is studied. The modified electrode can be used for the determination of MO spiked into urine samples, and excellent recovery results were obtained. The nanostructured polypyrrole films were characterized by field emission scanning electron microscopy (FESEM) and furrier transforms infrared (FTIR).

Keywords: morphine detection, sensor, polypyrrole, nanostructure, molecularly imprinted polymer

Procedia PDF Downloads 396