The Alternative Voltammetric Method for the Determination of Nicotine and Its Metabolite Nicotine N-Oxide

In the present paper, for the first time, the electrochemical behaviour of nicotine metabolite nicotine N-oxide (NNO) on static mercury dropping electrode (SMDE) and mercury meniscus modified silver solid amalgam electrode (m-AgSAE) has been reported. Nicotine N-oxide is reduced forming one peak at the potential -0.78 V on SDME and -0.86 V on m-AgSAE in Britton-Robinson buffer medium at pH 4.5 using cyclic voltammetry (CV). One electron and one proton take part in the reaction of NNO reduction. Calibration graphs for NNO determination using linear sweep voltammetry (LSV) on SDME and square-wave voltammetry (SWV) and differential pulse voltammetry (DPV) on m-AgSAE were obtained. Limit of detection (LOD) is 0.13 μM on SDME, and 0.16 μM (SWV) and 0.29 μM (DPV) on m-AgSAE. Since NNO can be used as an analytical form for nicotine voltammetric determination, so the developed methods were applied for the analysis of pharmaceutical preparations, and the recoveries from 97.3 to 104.6 % were achieved. Also, the elaborated methods were used in the analysis of biological fluids, and tobacco products. The obtained results were compared to those indicated in the certificates of drugs analysis, and to the results, obtained by reference methods (HPLC and GC).

Study of the Electrochemical Dissolution Behavior of Nitinol Shape Memory Alloy in Different Electrolytes for Micro-ECM Process

Nickel-Titanium alloy (Nitinol) is an excellent shape memory alloy (SMA) for Micro electro-mechanical systems (MEMS) particularly in biomedical applications owing to its three excellent features like shape memory effect (SME), superelasticity, and biocompatibility. The fabrication of micro features on Nitinol SMAs through conventional machining has been challenging due to its temperature-dependent material transformation properties. Micro electrochemical machining (micro-ECM), a nonconventional machining method for conductive material irrespective of strength and hardness has the potential for microfeature fabrication on Nitinol. This study presents the investigation on electrochemical dissolution behavior of Nitinol in different electrolytes for micro-ECM. The influence of electrolytes on the nature of dissolution of Nitinol has been studied by fabricating microchannels in three levels of parameters containing applied voltage and electrolyte concentration. The first three electrolytes were all aqueous neutral electrolytes i.e. sodium chloride (NaCl), sodium nitrate (NaNO3), and sodium bromide (NaBr). For profound analysis of dissolution behavior and its influence on machining performance, potentiodynamic polarization (PDP) tests of Nitinol were performed in aqueous NaCl, aqueous NaNO3, and aqueous NaBr solutions. The PDP tests that are conducted here are cyclic voltammetry (CV) and linear sweep voltammetry (LSV). The three aqueous solutions were utilized for microchannel fabrication in Nitinol through micro ECM in three levels of parameters out of which aqueous NaNO3 was successful in fabricating microchannel. Then nonaqueous electrolyte of ethylene glycol-based NaNO3 has been used to fabricate microchannels with lower depth overcut (DOC), width overcut (WOC), and length overcut (LOC) with respect to aqueous NaNO3 electrolyte.

Preparation and Characterization of Multi-doped Porous Carbon Nanofibers from Carbonization in Different Atmospheres and Their Oxygen Electrocatalytic Properties Research

Recently, electrocatalysts for oxygen reduction reactions (ORRs) as well as oxygen evolution reactions (OERs) hinged on electrospun nanofiber composites have attracted wide research attention. Transition metal elements and heteroatomic doping are important methods used to enhance their catalytic performances. Lately, the construction of electrocatalysts based on metal-organic framework (MOF) electrospun nanofibers has become a research hotspot. In this work, bimetallic NixCoy-ZIF nanocrystals were synthesized in an aqueous solution, followed by NixCoy-ZIF/PAN electrospun nanofiber precursors, which were prepared by a simple electrospinning method. Bimetal (Ni-Co) porous carbon nanofiber catalysts doped with nitrogen, oxygen, and sulfur elements were obtained at high-temperature carbonization treatment in different atmospheres (Ar, Air, and H2S), respectively. The morphological properties, structures, and composition were characterized by SEM, TEM, SAED, XRD, and XPS. Also, the specific surface area of materials and their pore size distribution was characterized by BET. Linear sweep voltammetry curves investigated catalyst performances towards oxygen reduction and evolution reactions. Importantly, Ni1Co2-ZIFs/PAN-Ar yielded the best ORR activity, whereas Ni1Co1-ZIFs/PAN-Air exhibited the best OER performance. This work provides significant guidance for the preparation and characterization of multi-doped porous carbon nanofibers carbonized in different atmospheres.

Electroplated core–shell nanowire network electrodes for highly efficient organic light-emitting diodes

In this study, we performed metal (Ag, Ni, Cu, or Pd) electroplating of core–shell metallic Ag nanowire (AgNW) networks intended for use as the anode electrode in organic light-emitting diodes (OLEDs) to modify the work function (WF) and conductivity of the AgNW networks. This low-cost and facile electroplating method enabled the precise deposition of metal onto the AgNW surface and at the nanowire (NW) junctions. AgNWs coated onto a transparent glass substrate were immersed in four different metal electroplating baths: those containing AgNO3 for Ag electroplating, NiSO4 for Ni electroplating, Cu2P2O7 for Cu electroplating, and PdCl2 for Pd electroplating. The solvated metal ions (Ag+, Ni2+, Cu2+, and Pd2+) in the respective electroplating baths were reduced to the corresponding metals on the AgNW surface in the galvanostatic mode under a constant electric current achieved by linear sweep voltammetry via an external circuit between the AgNW networks (cathode) and a Pt mesh (anode). The amount of electroplated metal was systematically controlled by varying the electroplating time. Scanning electron microscopy images showed that the four different metals (shells) were successfully electroplated on the AgNWs (core), and the nanosize-controlled electroplating process produced metal NWs with varying diameters, conductivities, optical transmittances, and WFs. The metal-electroplated AgNWs were successfully employed as the anode electrodes of the OLEDs. This facile and low-cost method of metal electroplating of AgNWs to increase their WFs and conductivities is a promising development for the fabrication of next-generation OLEDs.

Worrisome Exaggeration of Activity of Electrocatalysts Destined for Steady-State Water Electrolysis by Polarization Curves from Transient Techniques

Cyclic and linear sweep voltammetry techniques substantially misjudge the performance of water splitting electrocatalysts due to their transient nature that forbids the interface from reaching a steady-state. This misjudgment leads to the potentially detrimental yet unwittingly falsified data accumulation in the literature that requires immediate attention. Alternatively, sampled-current voltammetry (SCV) constructed from steady-state responses is advised to be widely adopted for screening electrocatalysts that are actually destined for steady-state operations. To show that this exaggeration is universal, a well-characterized activated SS, coprecipitated Co(OH)2, and Pt foil electrodes are studied for OER and HER in 1.0 M KOH. The results urge that it is time to adopt a relatively more precise alternative technique such as SCV.

Spray-Pyrolytic Tunable Structures of Mn Oxides-Based Composites for Electrocatalytic Activity Improvement in Oxygen Reduction

Hybrid nanomaterials based on manganese, cobalt, and lanthanum oxides of different morphology and phase compositions were prepared using a facile single-step ultrasonic spray pyrolysis (USP) process and tested as electrocatalysts for oxygen reduction reaction (ORR). The structural and morphological characterizations were completed by XRD and SEM-EDS. Electrochemical performance was characterized by cyclic voltammetry and linear sweep voltammetry in a rotating disk electrode assembly. All synthesized materials were found electrocatalytically active for ORR in alkaline media. Two different manganese oxide states were incorporated into a Co3O4 matrix, δ-MnO2 at 500 and 600 °C and manganese (II,III) oxide-Mn3O4 at 800 °C. The difference in crystalline structure revealed flower-like nanosheets for birnessite-MnO2 and well-defined spherical nanoparticles for material based on Mn3O4. Electrochemical responses indicate that the ORR mechanism follows a preceding step of MnO2 reduction to MnOOH. The calculated number of electrons exchanged for the hybrid materials demonstrate a four-electron oxygen reduction pathway and high electrocatalytic activity towards ORR. The comparison of molar catalytic activities points out the importance of the composition and that the synergy of Co and Mn is superior to Co3O4/La2O3 and pristine Mn oxide. The results reveal that synthesized hybrid materials are promising electrocatalysts for ORR.

Pencil Graphite Electrodes Decorated with Platinum Nanoparticles as Efficient Electrocatalysts for Hydrogen Evolution Reaction

Platinum-based materials are widely known as the most utilized and advanced catalysts for hydrogen evolution reaction. For this reason, several studies have reported alternative methods of incorporating this metal into more economical electrodes with a carbon-based support material. Herein, we report on the performance of pencil graphite electrodes decorated with electrochemically deposited platinum nanoparticles as efficient electrocatalysts for hydrogen evolution reaction. The electrodeposition of platinum was performed via pulsed current electrodeposition and the effect of current density on the electrocatalytic activity was investigated. The obtained electrodes were characterized using cyclic voltammetry, while the electrocatalytic activity was assessed through linear sweep voltammetry. Field emission scanning electron microscopy and energy-dispersive X-ray spectroscopy were utilised to gain an insight into surface morphology and chemical analysis of platinum nanoparticles. The best performing electrocatalyst, at both low and high current densities, was characterized by the highest exchange current density of 1.98 mA cm−2 and an ultralow overpotential of 43 mV at a current density of 10 mA cm−2. The results show that, at low current densities, performances closest to that of platinum can be achieved even with an ultralow loading of 50 µg cm−2 Pt.

Stable and Efficient Photoinduced Charge Transfer of MnFe2O4/Polyaniline Photoelectrode in Highly Acidic Solution

Tailoring conductive polymers with inorganic photocatalysts, which provide photoinduced electron-hole generation, have significantly enhanced composites leading to excellent photoelectrodes. In this work, MnFe2O4 nanoparticles prepared by a hydrothermal method were combined with polyaniline to prepare mixed (hybrid) slurries, which were cast onto flexible FTO to prepare photoelectrodes. The resulting photoelectrodes were characterized by XRD, FESEM, HRTEM and UV-VIS. The photoelectrochemical performance was investigated by linear sweep voltammetry and chronoamperometry. The photocurrent achieved by MnFe2O4/Polyaniline was 400 μA/cm2 at 0.8 V vs. Ag/AgCl in Na2SO4 (pH = 2) at 100 mW/cm2, while polyaniline alone achieved only 25 μA/cm2 under the same conditions. The best MnFe2O4/Polyaniline displayed an incident photon-to-current conversion efficiency (IPCE) and applied bias photon-to-current efficiency (ABPE) of 60% at 405 nm wavelength, and 0.17% at 0.8 V vs. Ag/AgCl, respectively. High and stable photoelectrochemical performance was achieved for more than 900 s in an acidic environment.

Graphene and Chitosan Composite Film Modified Electrode as a Sensitive Voltammetric Sensor for Tyrosine Detection in Food and Biological Samples

A voltammetric sensor made from a graphene and chitosan modified glassy carbon electrode (GR-CTS/GCE) was fabricated for accurate analysis of tyrosine (Tyr) in both food and biological samples. The surface morphology of the electrode and the properties of the electrode-electrolyte interface were determined by scanning electron microscopy and cyclic voltammetry. Compared with a bare GCE, the synergistic effect of GR and CTS is obvious. The peak current increases 35.6 times. The experimental conditions were optimized by second derivative linear sweep voltammetry (SDLSV) and Tyr was quantitatively analyzed on the electrode. The study shows that the oxidation peak current of Tyr obtained in 0.1 M pH 2.7 phosphate buffer is proportional to its concentration between 0.006-0.8 and 0.8-10.0 μM, with the low detection limit being 4.0 nM (signal/noise = 3). Excellent anti-interference ability was demonstrated by investigating the voltammetric response of Tyr in mixtures containing other biomolecules. In addition, the sensor exhibited good stability and repeatability. Through the detection of Tyr in milk and serum samples, the effectiveness of the sensor was studied, and the results were satisfactory.