Search results for: microfluidic paper-based electrochemical biosensors

Authors: Aniela Pop, Ianina Birsan, Corina Orha, Rodica Pode, Florica Manea

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Carbon nanofiber-epoxy composite electrode has been investigated through voltammetric and amperometric techniques in order to detect parabens from aqueous solutions. The occurrence into environment as emerging pollutants of these preservative compounds has been extensively studied in the last decades, and consequently, a rapid and reliable method for their quantitative quantification is required. In this study, methylparaben (MP) and propylparaben (PP) were chosen as representatives for paraben class. The individual electrochemical detection of each paraben has been successfully performed. Their electrochemical oxidation occurred at the same potential value. Their simultaneous quantification should be assessed electrochemically only as general index of paraben class as a cumulative signal corresponding to both MP and PP from solution. The influence of pH on the electrochemical signal was studied. pH ranged between 1.3 and 9.0 allowed shifting the detection potential value to smaller value, which is very desired for the electroanalysis. Also, the signal is better-defined and higher sensitivity is achieved. Differential-pulsed voltammetry and square-wave voltammetry were exploited under the optimum pH conditions to improve the electroanalytical performance for the paraben detection. Also, the operation conditions were selected, i.e., the step potential, modulation amplitude and the frequency. Chronomaprometry application as the easiest electrochemical detection method led to worse sensitivity, probably due to a possible fouling effect of the electrode surface. The best electroanalytical performance was achieved by pulsed voltammetric technique but the selection of the electrochemical technique is related to the concrete practical application. A good reproducibility of the voltammetric-based method using carbon nanofiber-epoxy composite electrode was determined and no interference effect was found for the cation and anion species that are common in the water matrix. Besides these characteristics, the long life-time of the electrode give to carbon nanofiber-epoxy composite electrode a great potential for practical applications.

Keywords: carbon nanofiber-epoxy composite electrode, electroanalysis, methylparaben, propylparaben

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Authors: A. Guellati, F-M Lounis, N. Guemras, K. Daoud

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Micro droplet formation is considered as a growing emerging area of research due to its wide-range application in chemistry as well as biology. The mechanism of micro droplet formation using two immiscible liquids running through a T-junction has been widely studied. We believe that the flow of these two immiscible phases can be of greater important factor that could have an impact on out-flow hydrodynamic behavior, the droplets generated and the size of the droplets. In this study, the type of the capillary tubes used also represents another important factor that can have an impact on the generation of micro droplets. The tygon capillary tubing with hydrophilic inner surface doesn't allow regular out-flows due to the fact that the continuous phase doesn't adhere to the wall of the capillary inner surface. Teflon capillary tubing, presents better wettability than tygon tubing, and allows to obtain steady and regular regimes of out-flow, and the micro droplets are homogeneoussize. The size of the droplets is directly dependent on the flows of the continuous and dispersed phases. Thus, as increasing the flow of the continuous phase, to flow of the dispersed phase stationary, the size of the drops decreases. Inversely, while increasing the flow of the dispersed phase, to flow of the continuous phase stationary, the size of the droplet increases.

Keywords: microfluidic system, micro droplets generation, t-junction, fluids engineering

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Authors: Renée M. Ripken, Johannes G. E. Gardeniers, Séverine Le Gac

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Controlling the multiphase behavior of aqueous biomass mixtures is essential when working in the biomass conversion industry. Here, the vapor/liquid equilibria (VLE) of ethylene glycol, glycerol, and xylitol were studied for temperatures between 25 and 200 °C and pressures of 1 to 10 bar. These experiments were performed in a microfluidic platform, which exhibits excellent heat transfer properties so that equilibrium is reached fast. Firstly, the saturated vapor pressure as a function of the temperature and the substrate mole fraction of the substrate was calculated using AspenPlus with a Redlich-Kwong-Soave Boston-Mathias (RKS-BM) model. Secondly, we developed a high-pressure and high-temperature microfluidic set-up for experimental validation. Furthermore, we have studied the multiphase flow pattern that occurs after the saturation temperature was achieved. A glass-silicon microfluidic device containing a 0.4 or 0.2 m long meandering channel with a depth of 250 μm and a width of 250 or 500 μm was fabricated using standard microfabrication techniques. This device was placed in a dedicated chip-holder, which includes a ceramic heater on the silicon side. The temperature was controlled and monitored by three K-type thermocouples: two were located between the heater and the silicon substrate, one to set the temperature and one to measure it, and the third one was placed in a 300 μm wide and 450 μm deep groove on the glass side to determine the heat loss over the silicon. An adjustable back pressure regulator and a pressure meter were added to control and evaluate the pressure during the experiment. Aqueous biomass solutions (10 wt%) were pumped at a flow rate of 10 μL/min using a syringe pump, and the temperature was slowly increased until the theoretical saturation temperature for the pre-set pressure was reached. First and surprisingly, a significant difference was observed between our theoretical saturation temperature and the experimental results. The experimental values were 10’s of degrees higher than the calculated ones and, in some cases, saturation could not be achieved. This discrepancy can be explained in different ways. Firstly, the pressure in the microchannel is locally higher due to both the thermal expansion of the liquid and the Laplace pressure that has to be overcome before a gas bubble can be formed. Secondly, superheating effects are likely to be present. Next, once saturation was reached, the flow pattern of the gas/liquid multiphase system was recorded. In our device, the point of nucleation can be controlled by taking advantage of the pressure drop across the channel and the accurate control of the temperature. Specifically, a higher temperature resulted in nucleation further upstream in the channel. As the void fraction increases downstream, the flow regime changes along the channel from bubbly flow to Taylor flow and later to annular flow. All three flow regimes were observed simultaneously. The findings of this study are key for the development and optimization of a microreactor for hydrogen production from biomass.

Keywords: biomass conversion, high pressure and high temperature microfluidics, multiphase, phase diagrams, superheating

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Authors: Okba Belahssen, Lazhar Torchane, Said Benramache, Abdelouahed Chala

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This paper presents corrosion behavior of the plasma-nitrided 32CrMoV13 steel. Different kinds of samples were tested: non-treated, plasma nitrided samples. The structure of layers was determined by X-ray diffraction, while the morphology was observed by scanning electron microscopy (SEM). The corrosion behavior was evaluated by electrochemical techniques (potentiodynamic curves and electrochemical impedance spectroscopy). The corrosion tests were carried out in acid chloride solution (HCl 1M). Experimental results showed that the nitrides ε-Fe2−3N and γ′-Fe4N present in the white layer are nobler than the substrate but may promote, by galvanic effect, a localized corrosion through open porosity. The better corrosion protection was observed for nitrided sample.

Keywords: plasma-nitrided, 32CrMoV13 steel, corrosion, EIS

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Authors: M. Kowalski, M. Brodowski, K. Dziabowska, E. Czaczyk, W. Bialobrzeska, N. Malinowska, S. Zoledowska, R. Bogdanowicz, D. Nidzworski

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Boron-doped-carbon nanowall (BCNW) electrodes are recently in much interest among scientists. BCNWs are good candidates for biosensor purposes as they possess interesting electrochemical characteristics like a wide potential range and the low difference between redox peaks. Moreover, from technical parameters, they are mechanically resistant and very tough. The production process of the microwave plasma-enhanced chemical vapor deposition (MPECVD) allows boron to build into the structure of the diamond being formed. The effect is the formation of flat, long structures with sharp ends. The potential of these electrodes was checked in the biosensing field. The procedure of simple carbon electrodes modification by antibodies was adopted to BCNW for specific antigen recognition. Surface protein D deriving from H. influenzae pathogenic bacteria was chosen as a target analyte. The electrode was first modified with the aminobenzoic acid diazonium salt by electrografting (electrochemical reduction), next anti-protein D antibodies were linked via 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride/N-hydroxysuccinimide (EDC/NHS) chemistry, and free sites were blocked by BSA. Cyclic voltammetry measurements confirmed the proper electrode modification. Electrochemical impedance spectroscopy records indicated protein detection. The sensor was proven to detect protein D in femtograms. This work was supported by the National Centre for Research and Development (NCBR) TECHMATSTRATEG 1/347324/12/NCBR/ 2017.

Keywords: anti-protein D antibodies, boron-doped carbon nanowall, impedance spectroscopy, Haemophilus influenzae.

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Authors: Md. Danish Eqbal, Venkat Gundabala

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Microparticles and microcapsules are basically used as a carrier for cells, tissues, drugs, and chemicals. Due to its biocompatibility, non-toxicity and biodegradability, alginate based microparticles have numerous applications in drug delivery, tissue engineering, organ repair and transplantation, etc. The production of uniform monodispersed microparticles was a challenge for the past few decades. However, emergence of microfluidics has provided controlled methods for the generation of the uniform monodispersed microparticles. In this work, we present a successful method for the generation of both microparticles and microcapsules (single and double core) using merging approach of two droplets, completely inside the microfluidic device. We have fabricated hybrid glass- PDMS (polydimethylsiloxane) based microfluidic device which has coflow geometry as well as the T junction channel. Coflow is used to generate the single as well as double oil-alginate emulsion in oil and T junction helps to form the calcium chloride droplets in oil. The basic idea is to match the frequency of the alginate droplets and calcium chloride droplets perfectly for controlled generation. Using the merging of droplets technique, we have successfully generated the microparticles and the microcapsules having single core as well as double and multiple cores. The cores in the microcapsules are very stable, well separated from each other and very intact as seen through cross-sectional confocal images. The size and the number of the cores along with the thickness of the shell can be easily controlled by controlling the flowrate of the liquids.

Keywords: double-core, droplets, microcapsules, microparticles

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Authors: Sachin Saxena, Manju Srivastava

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The present study describes a stable, highly sensitive and selective analytical sensor. Fe-BTC was synthesized at room temperature using the noble Iron-trimesate system. The high surface area of as synthesized Fe-BTC proved MOFs as ideal modifiers for glassy carbon electrode. The characterization techniques such as TGA, XRD, FT-IR, BET (BET surface area= 1125 m2/gm) analysis explained the electrocatalytic behaviour of Fe-BTC towards these two drugs. The material formed is cost effective and exhibit higher catalytic behaviour towards analyte systems. The synergism between synthesized Fe-BTC and electroanalytical techniques helped in developing a highly sensitive analytical method for studying the redox fate of ARP and RZ, respectively. Cyclic voltammetry of ferricyanide system proved Fe-BTC/GCE with an increase in 132% enhancement in peak current value as compared to that of GCE. The response characteristics of cyclic voltammetry (CV) and square wave voltammetry (SWV) revealed that the ARP and RZ could be effectively accumulated at Fe-BTC/GCE. On the basis of the electrochemical measurements, electrode dynamics parameters have been evaluated. Present study opens up new field of applications of MOFs modified GCE for drug sensing.

Keywords: MOFs, anti-psychotic, electrochemical sensor, anti-migraine drugs

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Authors: Shamima Akhter, Samira Bagheri, M. Shalauddin, Wan Jefrey Basirun

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In the present study, a nanocomposite of f-MWCNTs-Chitosan was prepared by the immobilization of Co(II) transition metal through self-assembly method and used for the simultaneous voltammetric determination of paracetamol (PA). The composite material was characterized by field emission scanning electron microscopy (FESEM) and energy dispersive X-Ray analysis (EDX). The electroactivity of cobalt immobilized f-MWCNTs with excellent adsorptive polymer chitosan was assessed during the electro-oxidation of paracetamol. The resulting GCE modified f-MWCNTs/CTS-Co showed electrocatalytic activity towards the oxidation of PA. The electrochemical performances were investigated using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and differential pulse voltammetry (DPV) methods. Under favorable experimental conditions, differential pulse voltammetry showed a linear dynamic range for paracetamol solution in the range of 0.1 to 400µmol L⁻¹ with a detection limit of 0.01 µmol L⁻¹. The proposed sensor exhibited significant selectivity for the paracetamol detection. The proposed method was successfully applied for the determination of paracetamol in commercial tablets and human serum sample.

Keywords: nanomaterials, paracetamol, electrochemical technique, multi-wall carbon nanotube

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Authors: P. Mirahmadpour, M. H. Banitaba, D. Nematollahi

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The chemistry of coordination polymers in recent years has grown exponentially not only because of their interesting architectures but also due to their various technical applications in many fields including ion exchange, chemical catalysis, small molecule separations, and drug release. The use of bridging ligands for the controlled self-assembly of one, two or three dimensional metallo-supramolecular species is the subject of serious study in last decade. Numerous different synthetic methods have been offered for the preparation of coordination polymers such as (a) diffusion from the gas phase, (b) slow diffusion of the reactants into a polymeric matrix, (c) evaporation of the solvent at ambient or reduced temperatures, (d) temperature controlled cooling, (e) precipitation or recrystallisation from a mixture of solvents and (f) hydrothermal synthesis. The electrosynthetic process suggested several advantages over conventional approaches. A general advantage of electrochemical synthesis is that it allows synthesis under milder conditions than typical solvothermal or microwave synthesis. In this work we have introduced a simple electrochemical method for growing metal coordination polymers based on copper with a flexible 2,2’-thiodiacetic acid (TDA) and rigid 1,2,4,5-benzenetetracarboxylate (BTC) ligands. The structure of coordination polymers were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), elemental analysis, thermal gravimetric (TG) and differential thermal analyses (DTA). The single-crystal X-ray diffraction analysis revealed that different conformations of the ligands and different coordination modes of the carboxylate group as well as different coordination geometries of the copper atoms. Electrochemical synthesis of coordination polymers has different advantages such as faster synthesis at lower temperature in compare with conventional chemical methods and crystallization of desired materials in a single synthetic step.

Keywords: 1, 2, 4, 5-benzenetetracarboxylate, coordination polymer, copper, 2, 2’-thiodiacetic acid

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Authors: M. Said Ahmed, M. Lebrini, J. Pellé, S. Rioual, B. Lescop, C. Roos

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The corrosion behavior of copper exposed in a marine atmosphere polluted and unpolluted by gases, mainly hydrogen sulphide (H2S), from the decomposition of Sargassum algae was studied using the mass loss method and electrochemical measurements. MEB/EDX and XRD were also used for the observation of morphology and surface analysis. To study the impact of this on copper corrosion, four sites more or less impacted by Sargassum algae strandings were selected. The samples were exposed for up to six months. The mass loss results showed that the average corrosion rate of copper was 528 µm/year for the site most affected by Sargassum algae and 9.4 µm/year for the least impacted site after three months of exposure, implying that the presence of Sargassum algae caused an important copper degradation. The morphological structures and properties of the corrosion products obtained at the impacted and non-impacted sites differed significantly. In the absence of Sargassum algae, we obtained mainly Cu2O and Cu2Cl(OH)3. Whereas in the atmosphere with Sargassum algae, CuS product is the main corrosion product obtained. Electrochemical analyses showed that the protection offered by the corrosion product layer was more important and improved with time for the non-impacted sites, whereas on the impacted sites, this protection deteriorated.

Keywords: atmospheric-corrosion, sargassum algae, copper, electrochemical techniques, SEM/EDX and XRD

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Authors: Mao Li, Yuguang Ma, Katsuhiko Ariga

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The performance of functional materials is governed by their ability to interact with surrounding environments in a well-defined and controlled manner. Layer-by-Layer (LbL) assembly is one of the most widely used technologies for coating both planar and particulate substrates in a diverse range of fields, including optics, energy, catalysis, separations, and biomedicine. Herein, we introduce electrochemical-coupling layer-by-layer assembly as a novel fabrication methodology for preparing layered thin films. This assembly method not only determines the process properties (such as the time, scalability, and manual intervention) but also directly control the physicochemical properties of the films (such as the thickness, homogeneity, and inter- and intra-layer film organization), with both sets of properties linked to application-specific performance.

Keywords: layer by layer assembly, electropolymerization, carbazole, optical thin film, electronics

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Authors: J. Tomilla Ajayi, Werner E. Van Zyl

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This work presents an overview of the reaction of 2, 4-diferrocenyl-1, 3-dithiadiphosphetane-2, 4-disulfide (Ferrocenyl Lawesson’s reagent) with water to produce the non-symmetric, ferocenyl dithiophosphonic acid respectively in high yields. These acids were readily deprotonated by anhydrous Ammonia to yield the corresponding ammonium salt NH4S2PFcOH. These were complex to Ni (II) in molar ratio 1:1 and 1:2. The resulting complex from the reaction formed same compound with different isomers (Cis and Trans) and also compound with multimetallic coordination. Quality X-ray crystals were formed from THF/Ether. The compounds were characterized by 1H, 31P NMR, and FTIR. Bulk purity were confirmed by either ESI-MS or elemental analysis and The XRD images were obtained using single crystal X-ray crystallographic studies. The electrochemical investigation of the Compounds were carried out using cyclic voltammetry.

Keywords: ferrocenyl, dithiophosphonate, isomer, coordination

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Authors: Dessie Tibebe, Muluken Asmare, Marye Mulugeta, Yezbie Kassa, Zerubabel Moges, Dereje Yenealem, Tarekegn Fentie, Agmas Amare

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The performance of electrocoagulation (EC) using Aluminium electrodes for the treatment of effluent-containing chromium metal using a fixed bed electrochemical batch reactor was studied. In the present work, the efficiency evaluation of EC in removing physicochemical and heavy metals from real industrial tannery wastewater in the Amhara region, collected from Bahirdar, Debre Brihan, and Haik, was investigated. The treated and untreated samples were determined by AAS and ICP OES spectrophotometers. The results indicated that selected heavy metals were removed in all experiments with high removal percentages. The optimal results were obtained regarding both cost and electrocoagulation efficiency with initial pH = 3, initial concentration = 40 mg/L, electrolysis time = 30 min, current density = 40 mA/cm2, and temperature = 25oC favored metal removal. The maximum removal percentages of selected metals obtained were 84.42% for Haik, 92.64% for Bahir Dar and 94.90% for Debre Brihan. The sacrificial electrode and sludge were characterized by FT-IR, SEM and XRD. After treatment, some metals like chromium will be used again as a tanning agent in leather processing to promote a circular economy.

Keywords: electrochemical, treatment, aluminum, tannery effluent

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Authors: Mulatu Kassie Birhanu

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Electrochemical reduction of CO₂ is an emerging and current issue for its conversion in to valuable product upon minimization of its atmospheric level for contribution of maintaining within the range of permissible limit. Among plenty of electro-catalysts gold and copper are efficient and effective catalysts, which are synthesized and applicable for this research work. The two metal catalysts were prepared in inert environment with different compositions through co-reduction process from their corresponding precursors and then by adding multi-walled carbon nano-tube as a supporter and enhanced the conductivity. The catalytic performance of CO₂ reduction for each composition was performed and resulted an outstanding catalytic activity with generation of high current density (70 mA/cm² at 0.91V vs. RHE) and relatively small onset potential. The catalytic performance, compositions, morphologies, structure and geometric arrangements were evaluated by electrochemical analysis (LSV, impedance, chronoamperometry & tafel plot), EDS, SEM and XAS respectively. The composite metals showed better selectivity of products and faradaic efficiencies due to the synergetic effects of the combined nano-particles in addition to the impact of grain size in reduction of CO₂. Carbon monoxide, hydrogen, formate and ethanol are the reduction products, which are detected and quantifiable by chromatographic techniques considering their physical state of each product.

Keywords: carbondioxide, faradaic efficiency, electrocatalyst, current density

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Authors: Chia-Ting Chang, Chia-Yu Lin

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We report on the decisive role of iron phosphate (FePO₄), formed in-situ during the electrochemical characterization, played in the electrocatalytic activity, especially its oxygen tolerance of iron oxides towards H₂O₂ reduction. Iron oxides studied including, Nanorod arrays (NRs) of β-FeOOH, γ-Fe₂O₃, α-Fe₂O₃, α-Fe₂O₃ nanosheets (α-Fe₂O₃NS), α-Fe₂O₃ nanoparticles (α-Fe₂O₃NP), were synthesized using chemical bath deposition. The nanostructure was controlled simply by adjusting the composition of precursor solution and reaction duration for CBD process, whereas the crystal phase was controlled by adjusting the annealing temperature. It was found that iron phosphate (FePO₄) was deposited in-situ onto the surface of this nanostructured α-Fe₂O₃ during the electrochemical pretreatment in the phosphate electrolyte, and both FePO₄ and α-Fe₂O₃ showed the activity in catalysing the electrochemical reduction of H₂O₂. In addition, the interaction/compatibility between deposited FePO₄ and iron oxides has a decisive effect on the overall electrocatalytic activity of the resultant electrodes; FePO₄ only showed synergetic effect on the overall electrocatalytic activity of α-Fe₂O₃NR and α-Fe2O₃NS. Both α-Fe₂O₃NR and α-Fe₂O₃NS showed two reduction peaks in phosphate electrolyte containing H₂O₂, one being pH-dependent and related to the electrocatalytic properties of FePO₄, and the other one being pH-independent and only related to the intrinsic electrocatalytic properties of α-Fe₂O₃NR and α-Fe₂O₃NS. However, all iron oxides showed only one pH-independent reductive peak in non-phosphate electrolyte containing H₂O₂. The synergesitic catalysis exerted by FePO₄ with α-Fe₂O₃NR or α-Fe₂O₃NS providing additional oxygen-insensitive active site for H₂O₂ reduction, which allows their applications to electrochemical detection of H₂O₂ without the interference of O₂ involving in oxidase-catalyzed chemical processes.

Keywords: H₂O₂ reduction, Iron oxide, iron phosphate, O₂ tolerance

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Authors: Mahfouz Saeed

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Cu₂(ZnSn)(S)₄ (CTZS) offers potential advantages over CuInGaSe₂ (CIGS) as solar thin film because to its higher band gap. Preparing such photovoltaic materials by electrochemical techniques is particularly attractive due to the lower processing cost and the high throughput of such techniques. Several recent publications report CTZS electroplating; however, the electrochemical process still facing serious challenges such as a sulfur atomic ration which is about 50% of the total alloy. We introduce in this work an improved electrolyte composition which enables the direct electrodeposition of CTZS from a single bath. The electrolyte is significantly more dilute in comparison to common baths described in the literature. The bath composition we introduce is: 0.0032 M CuSO₄, 0.0021 M ZnSO₄, 0.0303 M SnCl₂, 0.0038 M Na₂S₂O₃, and 0.3 mM Na₂S₂O3. PHydrion is applied to buffer the electrolyte to pH=2, and 0.7 M LiCl is applied as supporting electrolyte. Electrochemical process was carried at a rotating disk electrode which provides quantitative characterization of the flow (room temperature). Comprehensive electrochemical behavior study at different electrode rotation rates are provided. The effects of agitation on atomic composition of the deposit and its adhesion to the molybdenum back contact are discussed. The post treatment annealing was conducted under sulfur atmosphere with no need for metals addition from the gas phase during annealing. The potential which produced the desired atomic ratio of CTZS at -0.82 V/NHE. Smooth deposit, with uniform composition across the sample surface and depth was obtained at 500 rpm rotation speed. Final sulfur atomic ratio was adjusted to 50.2% in order to have the desired atomic ration. The final composition was investigated using Energy-dispersive X-ray spectroscopy technique (EDS). XRD technique used to analyze CTZS crystallography and thickness. Complete and functional CTZS PV devices were fabricated by depositing all the required layers in the correct order and the desired optical properties. Acknowledgments: Case Western Reserve University for the technical help and for using their instruments.

Keywords: photovoltaic, CTZS, thin film, electrochemical

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Authors: Xinyong Li

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A new coupling system was constructed by combining photo-electrochemical cell with eletro-fenton cell (PEC-EF). The electrode material in this system was derived from MnyFe₁₋yCo Prussian-Blue-Analog (PBA). Mn₀.₄Fe₀.₆Co₀.₆₇-N@C spin-coated on carbon paper behaved as the gas diffusion cathode and Mn₀.₄Fe₀.₆Co₀.₆₇O₂.₂ spin-coated on fluorine-tin oxide glass (FTO) as anode. The two separated cells could degrade Sulfamethoxazole (SMX) simultaneously and some coupling mechanisms by PEC and EF enhancing the degradation efficiency were investigated. The continuous on-site generation of H₂O₂ at cathode through an oxygen reduction reaction (ORR) was realized over rotating ring-disk electrode (RRDE). The electron transfer number (n) of the ORR with Mn₀.₄Fe₀.₆Co₀.₆₇-N@C was 2.5 in the selected potential and pH range. The photo-electrochemical properties of Mn₀.₄Fe₀.₆Co₀.₆₇O₂.₂ were systematically studied, which displayed good response towards visible light. The photo-induced electrons at anode can transfer to cathode for further use. Efficient photo-electro-catalytic performance was observed in degrading SMX. Almost 100% SMX removal was achieved in 120 min. This work not only provided a highly effective technique for antibiotic treatment but also revealed the synergic effect between PEC and EF.

Keywords: Electro-Fenton, photo-electrochemical, synergic effect, sulfamethoxazole

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Authors: O. Tovide, N. Jahed, N. Mohammed, C. E. Sunday, H. R. Makelane, R. F. Ajayi, K. M. Molapo, A. Tsegaye, M. Masikini, S. Mailu, A. Baleg, T. Waryo, P. G. Baker, E. I. Iwuoha

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A graphenated–polyaniline (GR-PANI) nanocomposite sensor was constructed and used for the determination of anthracene. The direct electro-oxidation behavior of anthracene on the GR-PANI modified glassy carbon electrode (GCE) was used as the sensing principle. The results indicate thatthe response profile of the oxidation of anthracene on GR-PANI-modified GCE provides for the construction of sensor systems based onamperometric and potentiometric signal transductions. A dynamic linear range of 0.12- 100 µM anthracene and a detection limit of 0.044 µM anthracene were established for the sensor system.

Keywords: electrochemical sensors, environmental pollutants, graphenated-polymers, polyaromatic hydrocarbon

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Authors: Behnoush Dousti, Ye Choi, Gil S. Lee

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Microsupercapacitors (MScs) are known as the future of miniaturized energy sources that can be coupled to a battery to deliver stable and constant energy to microelectronics. Among all their counterparts, electrochemical microsupercapacitor have drawn the most research attention due to their higher power density and long cycle life. Designing the microstructure and choosing the electroactive materials are two significant factors that greatly affect the performance of the device. Here, we report successful fabrication and characterization of a microsupercapacitor with interdigitated structure based on Carbon nanotube sheets (CNT sheet). Novel structure of highly aligned CNT sheet as the electrode materials which also offers excellent conductivity and large surface area along with doping with nitrogen, enabled us to develop a device with serval order of magnitude higher electrochemical performance than the pristine CNT in aqueous electrolyte including high specific capacitance and rate capabilities and excellent cycle life over 10000 cycles. Geometric parameters such as finger width and gap size were also studied and it was shown the device performance is much depended on them. Results of this study confirms the potential of CNT sheet for future energy storage devices.

Keywords: carbon nanotube, energy storage systems, microsupercapacitor, nitrogen doping

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Authors: D. Baratian, A. Cavalli, D. van den Ende, F. Mugele

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The morphology of liquid bridges inside complex geometries is the subject of interest for many years. These efforts try to find stable liquid configuration considering the boundary condition and the physical properties of the system. On the other hand precise manipulation of droplets is highly significant in many microfluidic applications. The liquid configuration in a complex geometry can be switched by means of external stimuli. We show manipulation of droplets in a wedge structure. The profile and position of a drop in a wedge geometry has been calculated analytically assuming negligible contact angle hysteresis. The characteristic length of liquid bridge and its interfacial tension inside the surrounding medium along with the geometrical parameters of the system determine the morphology and equilibrium position of drop in the system. We use electrowetting to modify one the governing parameters to manipulate the droplet. Electrowetting provides the capability to have precise control on the drop position through tuning the voltage and consequently changing the contact angle. This technique is employed to tune drop displacement and control its position inside the wedge. Experiments demonstrate precise drop movement to its predefined position inside the wedge geometry. Experimental results show promising consistency as it is compared to our geometrical model predictions. For such a drop manipulation, appealing applications in microfluidics have been considered.

Keywords: liquid bridges, microfluidics, drop manipulation, wetting, electrowetting, capillarity

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Authors: Z. Yousefniayejahr, S. Bolognini, A. Bonini, C. Campobasso, N. Poma, F. Vivaldi, M. Di Luca, A. Tavanti, F. Di Francesco

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Pathogenic bacteria represent a threat to healthcare systems and the food industry, because their rapid detection remains challenging. Electrochemical biosensors are gaining prominence as a novel technology for the detection of pathogens due to intrinsic features such as low cost, rapid response time, and portability, which make them a valuable alternative to traditional methodologies. These sensors use biorecognition elements that are crucial for the identification of specific bacteria. In this context, bacteriophages are promising tools for their inherent high selectivity towards bacterial hosts, which is of fundamental importance when detecting bacterial pathogens in complex biological samples. In this study, we present the development of a low-cost and portable sensor based on the Zeno phage for the rapid detection of Staphylococcus aureus. Screen-printed gold electrodes functionalized with the Zeno phage were used, and electrochemical impedance spectroscopy was applied to evaluate the change of the charge transfer resistance (Rct) as a result of the interaction with S. aureus MRSA ATCC 43300. The phage-based biosensor showed a linear range from 101 to 104 CFU/mL with a 20-minute response time and a limit of detection (LOD) of 6 CFU/mL under physiological conditions. The biosensor’s ability to recognize various strains of staphylococci was also successfully demonstrated in the presence of clinical isolates collected from different geographic areas. Assays using S. epidermidis were also carried out to verify the species-specificity of the phage sensor. We only observed a remarkable change of the Rct in the presence of the target S. aureus bacteria, while no substantial binding to S. epidermidis occurred. This confirmed that the Zeno phage sensor only targets S. aureus species within the genus Staphylococcus. In addition, the biosensor's specificity with respect to other bacterial species, including gram-positive bacteria like Enterococcus faecium and the gram-negative bacterium Pseudomonas aeruginosa was evaluated, and a non-significant impedimetric signal was observed. Notably, the biosensor successfully identified S. aureus bacterial cells in a complex matrix such as a nasal swab, opening the possibility of its use in a real-case scenario. We diluted different concentrations of S. aureus from 108 to 100 CFU/mL with a ratio of 1:10 in the nasal swap matrices collected from healthy donors. Three different sensors were applied to measure various concentrations of bacteria. Our sensor indicated high selectivity to detect S. aureus in biological matrices compared to time-consuming traditional methods, such as enzyme-linked immunosorbent assay (ELISA), polymerase chain reaction (PCR), and radioimmunoassay (RIA), etc. With the aim to study the possibility of using this biosensor to address the challenge associated with pathogen detection, ongoing research is focused on the assessment of the biosensor’s analytical performances in different biological samples and the discovery of new phage bioreceptors.

Keywords: electrochemical impedance spectroscopy, bacteriophage, biosensor, Staphylococcus aureus

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Authors: Amirhossein Hasani, Shamin Houshmand Sharifi

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In this work, we investigate humidity sensing behavior of the graphene oxide with porous silicon substrate. By evaporation method, aluminum interdigital electrodes have been deposited onto porous silicon substrate. Then, by drop-casting method graphene oxide solution was deposited onto electrodes. The porous silicon was formed by electrochemical etching. The experimental results showed that using porous silicon substrate, we obtained two times larger sensitivity and response time compared with the results obtained with silicon substrate without porosity.

Keywords: graphene oxide, porous silicon, humidity sensor, electrochemical

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Authors: Manuel Salado, Mikel Rincón, Arkaitz Fidalgo, Roberto Fernandez, Senentxu Lanceros-Méndez

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Lithium-ion batteries (LIBs) are a promising technology for energy storage, but they suffer from safety concerns due to the use of flammable organic solvents in their liquid electrolytes. Solid-state electrolytes (SSEs) offer a potential solution to this problem, but they have their own limitations, such as poor ionic conductivity and high interfacial resistance. The aim of this research was to develop a new type of SSE based on metal-organic frameworks (MOFs) and ionic liquids (ILs). MOFs are porous materials with high surface area and tunable electronic properties, making them ideal for use in SSEs. ILs are liquid electrolytes that are non-flammable and have high ionic conductivity. A series of MOFs were synthesized, and their electrochemical properties were evaluated. The MOFs were then infiltrated with ILs to form a quasi-solid gel and solid xerogel SSEs. The ionic conductivity, interfacial resistance, and electrochemical performance of the SSEs were characterized. The results showed that the MOF-IL SSEs had significantly higher ionic conductivity and lower interfacial resistance than conventional SSEs. The SSEs also exhibited excellent electrochemical performance, with high discharge capacity and long cycle life. The development of MOF-IL SSEs represents a significant advance in the field of solid-state electrolytes. The high ionic conductivity and low interfacial resistance of the SSEs make them promising candidates for use in next-generation LIBs. The data for this research was collected using a variety of methods, including X-ray diffraction, scanning electron microscopy, and electrochemical impedance spectroscopy. The data was analyzed using a variety of statistical and computational methods, including principal component analysis, density functional theory, and molecular dynamics simulations. The main question addressed by this research was whether MOF-IL SSEs could be developed that have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. The results of this research demonstrate that MOF-IL SSEs are a promising new type of solid-state electrolyte for use in LIBs. The SSEs have high ionic conductivity, low interfacial resistance, and excellent electrochemical performance. These properties make them promising candidates for use in next-generation LIBs that are safer and have higher energy densities.

Keywords: energy storage, solid-electrolyte, ionic liquid, metal-organic-framework, electrochemistry, organic inorganic plastic crystal

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Authors: N. Chahmana, I. Zerroual

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The aim of our work is the contribution to the improvement of the performances of the positive plate of the lead acid battery. For that, we synthesized two varieties of PbO2 used in industry, alpha and beta PbO2 by electrochemical way starting from the not formed industrial plates. We studied the kinetics of reduction of the alpha varieties and PbO2 beta on electrode with microcavity in sulphuric medium. The electrochemical study of the powders of α and β-PbO2 was made by cyclic voltamperometry with sweeping of potential by using a traditional assembly with three electrodes. Values of the coefficient of diffusion of the proton in α and β-PbO2 are respectively equal to 0.498*10-8cm2 /s and 0.793*10-8 cm2 /s. During the cycling of the two varieties of PbO2, we obtain a clear increase in the capacity.

Keywords: lead accumulator, α and β - PbO2, synthesis, kinetics, cyclic voltametry, coefficient of diffusion

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Authors: Yilei Xue, Yat-Hing Ham, Wenting Qiu, Wan Chan, Stefan Nagl

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Polydopamine (PDA) is a popular material in biological and medical applications due to its excellent biocompatibility, outstanding physicochemical properties, and facile fabrication. In this project, a new sandwich-structured PDA and silver (Ag) hybrid material named PDA-Ag-PDA was synthesized and characterized layer-by-layer, where silver nanoparticles (Ag NPs) are wrapped in PDA coatings, using SEM, AFM, 3D surface metrology, and contact angle meter. The silver loading capacity is positively proportional to the roughness value of the initial PDA film. This designed film was subsequently integrated within a digital microfluidic (DMF) platform coupling with an oxygen sensor layer for on-chip antibacterial assay. The concentration of E. coli was quantified on DMF by real-time monitoring oxygen consumption during E. coli growth with the optical oxygen sensor layer. The PDA-Ag-PDA coating shows an 99.9% reduction in E. coli population under non-nutritive condition with 1-hour treatment and has a strong growth inhibition of E. coliin nutrient LB broth as well. Furthermore, PDA-Ag-PDA film maintaining a low cytotoxicity effect to human cells. After treating with PDA-Ag-PDA film for 24 hours, 82% HEK 293 and 86% HeLa cells were viable. The SERS enhancement factor of PDA-Ag-PDA is estimated to be 1.9 × 104 using Rhodamine 6G (R6G). Multifunctional PDA-Ag-PDA coating provides an alternative platform to conjugate biomolecules and perform biological applications on DMF, in particular, for the adhesive protein and cell study.

Keywords: polydopamine, silver nanoparticles, digital microfluidic, optical sensor, antimicrobial assay, SERS

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Authors: Boce Zhang

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Strategic innovation of nanotechnology to promote food safety has drawn tremendous attentions among research groups, which includes the need for research support during the implementation of the Food Safety Modernization Act (FSMA) in the United States. There are urgent demands and knowledge gaps to the understanding of a) food-water-bacteria interface as for how pathogens persist and transmit during food processing and storage; b) minimum processing requirement needed to prevent pathogen cross-contamination in the food system. These knowledge gaps are of critical importance to the food industry. However, the lack of knowledge is largely hindered by the limitations of research tools. Our groups recently endeavored two novel engineering systems with biomimetics and microfluidics as a holistic approach to hazard analysis and risk mitigation, which provided unprecedented research opportunities to study pathogen behavior, in particular, contamination, and cross-contamination, at the critical food-water-pathogen interface. First, biomimetically-patterned surfaces (BPS) were developed to replicate the identical surface topography and chemistry of a natural food surface. We demonstrated that BPS is a superior research tool that empowers the study of a) how pathogens persist through sanitizer treatment, b) how to apply fluidic shear-force and surface tension to increase the vulnerability of the bacterial cells, by detaching them from a protected area, etc. Secondly, microfluidic devices were designed and fabricated to study the bactericidal kinetics in the sub-second time frame (0.1~1 second). The sub-second kinetics is critical because the cross-contamination process, which includes detachment, migration, and reattachment, can occur in a very short timeframe. With this microfluidic device, we were able to simulate and study these sub-second cross-contamination scenarios, and to further investigate the minimum sanitizer concentration needed to sufficiently prevent pathogen cross-contamination during the food processing. We anticipate that the findings from these studies will provide critical insight on bacterial behavior at the food-water-cell interface, and the kinetics of bacterial inactivation from a broad range of sanitizers and processing conditions, thus facilitating the development and implementation of science-based food safety regulations and practices to mitigate the food safety risks.

Keywords: biomimetic materials, microbial food safety, microfluidic device, nanotechnology

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Authors: William L. Whitehouse, Louisa H. Y. Lo, Andrew B. Kinghorn, Simon C. C. Shiu, Julian. A. Tanner

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C-reactive protein (CRP) is an acute-phase reactant and sensitive indicator for sepsis and other life-threatening pathologies, including systemic inflammatory response syndrome (SIRS). Currently, clinical turn-around times for established CRP detection methods take between 30 minutes to hours or even days from centralized laboratories. Here, we report the development of an electrochemical biosensor using redox probe-tagged DNA aptamers functionalized onto cheap, commercially available screen-printed electrodes. Binding-induced conformational switching of the CRP-targeting aptamer induces a specific and selective signal-ON event, which enables single-step and reagentless detection of CRP in as little as 1 minute. The aptasensor dynamic range spans 5-1000nM (R=0.97) or 5-500nM (R=0.99) in 50% diluted human serum, with a LOD of 3nM, corresponding to 2-orders of magnitude sensitivity under the clinically relevant cut-off for CRP. The sensor is stable for up to one week and can be reused numerous times, as judged from repeated real-time dosing and dose-response assays. By decoupling binding events from the signal induction mechanism, structure-switching electrochemical aptamer-based sensors (SS-EABs) provide considerable advantages over their adsorption-based counterparts. Our work expands on the retinue of such sensors reported in the literature and is the first instance of an SS-EAB for reagentless CRP detection. We hope this study can inspire further investigations into the suitability of SS-EABs for diagnostics, which will aid translational R&D toward fully realized devices aimed at point-of-care applications or for use more broadly by the public.

Keywords: structure-switching, C-reactive protein, electrochemical, biosensor, aptasensor.

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Authors: Sarah Fahad Alajmi, Tamer Ezzat Youssef

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Here, we report a simple method for the direct conversion of 6-Nitro-1H-indole into N-substituted indoles via electrochemical dehydrogenative reaction with halogenated reagents under strongly basic conditions through N–R bond formation. The N-protected indoles have been prepared under moderate and scalable electrolytic conditions. The conduct of the reactions was performed in a simple divided cell under constant current without oxidizing reagents or transition-metal catalysts. The synthesized products have been characterized via UV/Vis spectrophotometry, 1H-NMR, and FTIR spectroscopy. A possible reaction mechanism is discussed based on the N-protective products. This methodology could be applied to the synthesis of various biologically active N-substituted indole derivatives.

Keywords: green chemistry, 1H-indole, heteroaromatic, organic electrosynthesis

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Authors: Maria Sofia Palagonia, Doriano Brogioli, Fabio La Mantia

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In the last decade, lithium has become an important raw material in various sectors, in particular for rechargeable batteries. Its production is expected to grow more and more in the future, especially for mobile energy storage and electromobility. Until now it is mostly produced by the evaporation of water from salt lakes, which led to a huge water consumption, a large amount of waste produced and a strong environmental impact. A new, clean and faster electrochemical technique to recover lithium has been recently proposed: electrochemical ion pumping. It consists in capturing lithium ions from a feed solution by intercalation in a lithium-selective material, followed by releasing them into a recovery solution; both steps are driven by the passage of a current. In this work, a new configuration of the electrochemical cell is presented, used to study and optimize the process of the intercalation of lithium ions through the hydrodynamic condition. Lithium Manganese Oxide (LiMn₂O₄) was used as a cathode to intercalate lithium ions selectively during the reduction, while Nickel Hexacyano Ferrate (NiHCF), used as an anode, releases positive ion. The effect of hydrodynamics on the process has been studied by conducting the experiments at various fluxes of the electrolyte through the electrodes, in terms of charge circulated through the cell, captured lithium per unit mass of material and overvoltage. The result shows that flowing the electrolyte inside the cell improves the lithium capture, in particular at low lithium concentration. Indeed, in Atacama feed solution, at 40 mM of lithium, the amount of lithium captured does not increase considerably with the flux of the electrolyte. Instead, when the concentration of the lithium ions is 5 mM, the amount of captured lithium in a single capture cycle increases by increasing the flux, thus leading to the conclusion that the slowest step in the process is the transport of the lithium ion in the liquid phase. Furthermore, an influence of the concentration of other cations in solution on the process performance was observed. In particular, the capturing of the lithium using a different concentration of NaCl together with 5 mM of LiCl was performed, and the results show that the presence of NaCl limits the amount of the captured lithium. Further studies can be performed in order to understand why the full capacity of the material is not reached at the highest flow rate. This is probably due to the porous structure of the material since the liquid phase is likely not affected by the convection flow inside the pores. This work proves that electrochemical ion pumping, with a suitable hydrodynamic design, enables the recovery of lithium from feed solutions at the lower concentration than the sources that are currently exploited, down to 1 mM.

Keywords: desalination battery, electrochemical ion pumping, hydrodynamic, lithium

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Authors: Lingling Shui, Shuting Xie

Abstract:

As alternatives to electronic devices, optically active structures from responsive nanomaterials offer great opportunity buildup smart functional sensors. Hereby, we report on droplet microfluidics enabled construction and application of photonic microcapsules (PMCs) for colorimetric temperature microsensors, enabling miniaturization for injectable local micro-area sensing and integration for large-area sensing. Monodispersed PMCs are produced by in-situ photopolymerization of hydrogel shells of cholesteric liquid crystal (CLC)-in-water-in-oil double emulsion droplets prepared using microfluidic devices, with controllable physical structures and chemical compositions. Constructed PMCs exhibit thermal responsive structural color according to the selective Bragg reflection of CLC’s periodical helical structures within the microdroplet’s spherical confinement. Constructed PMCs with tunable size and composition have been successfully applied for monitoring the living cell extracellular temperature via co-incubation with cell suspension, and for detecting human body temperature via a flexible device from assembled PMCs. These PMCs could be flexibly applied in either micro-environment or large-area surface, enabling wide applications for precision temperature monitoring biological activities (e.g. cells or organs), optoelectronic devices working conditions (e.g. temperature indicators under extreme conditions), and etc.

Keywords: droplet, microfluidics, assembly, soft materials, microsensor

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