Search Results (22)

This review examines the feasibility of electrochemical synthesis of poly-L-arginine (PArg) using repetitive cyclic voltammetry in neutral aqueous phosphate-buffered saline. Previous studies on electrochemical deposition of PArg onto different carbonaceous electrode materials are discussed with respect to the already reported mechanistic models. Some controversial interpretations are of interest, predominantly the formation of peptide bonds during the electropolymerisation of L-arginine. Several alternative anodic pathways are considered via the possibilities and limitations of ways of attaching L-arginine molecules to the electrode surface. Furthermore, the role of oxygen-containing surface groups is discussed, as this aspect has been largely overlooked in the context of L-arginine deposition, despite the O-terminating character of the electrode surface and its effect on the reactivity of the nucleophilic guanidine group in L-arginine. Also, the application of extremely high potentials around +2 V vs. Ag/AgCl/3 mol L⁻¹ KCl is considered, as it can lead to the generation of reactive oxygen species that may interfere with or even govern the entire deposition process. Thus, the absence of such considerations may raise doubts about the peptide nature of the electrochemically assisted polymerisation of this basic amino acid. Finally, it seems that the identity of the electrochemically synthesised PArg does not correspond to that of this polymer prepared by conventional methods, such as solid-phase peptide synthesis, solution-phase synthesis, or N-carboxy-anhydride polymerisation, and therefore the whole process remains unproved. Full article

Vitamins are crucial micro-nutrients for overall well-being, making continuous monitoring essential. There are demands to provide an alternative detection, especially using a portable detection or a point-of-care-testing (POCT) device. One promising approach is employing an in situ electro-polymerised MIP (eMIP), which offers a straightforward polymerisation technique on screen-printed electrodes (SPEs). Here, we report a review based on three databases (PubMed, Scopus, and Web of Science) from 2014 to 2024 using medical subject heading (MeSH) terms “electrochemical polymerisation” OR “electropolymerisation” crossed with the terms “molecularly imprinted polymer” AND “vitamin A” OR “vitamin D” OR “vitamin E” OR “vitamin K” OR “fat soluble vitamin” OR “vitamin B” OR “vitamin C” OR “water soluble vitamin”. The resulting 12 articles covered the detection of vitamins in ascorbic acid, riboflavin, cholecalciferol, calcifediol, and menadione using monomers of catechol (CAT), 3,4-ethylenedioxythiophene (EDOT), o-aminophenol (oAP), o-phenylenediamine (oPD), pyrrole, p-aminophenol (pAP), p-phenylenediamine (pPD), or resorcinol (RES), using common bare electrodes including graphite rod electrode (GRE), glassy carbon electrode (GCE), gold electrode (GE), and screen-printed carbon electrode (SPCE). The most common electrochemical detections were differential pulse voltammetry (DPV) and linear sweep voltammetry (LSV). The imprinting factor (IF) of the eMIP-modified electrodes were from 1.6 to 21.0, whereas the cross-reactivity was from 0.0% to 29.9%. Several types of food and biological samples were tested, such as supplement tablets, poultry and pharmaceutical drugs, soft drinks, beverages, milk, infant formula, human and calf serum, and human plasma. However, more discoveries and development of detection methods needs to be performed, especially for the vitamins that have not been studied yet. This will allow the improvement in the application of eMIPs on portable-based detection and POCT devices. Full article

The detection of glucose is crucial for diagnosing diseases such as diabetes and enables timely medical intervention. In this study, a disposable enzymatic screen-printed electrode electrochemical biosensor enhanced with machine learning (ML) for quantifying glucose in serum is presented. The platinum working surface was modified by chemical adsorption with biographene (BGr) and glucose oxidase, and the enzyme was encapsulated in polydopamine (PDP) by electropolymerisation. Electrochemical characterisation and morphological analysis (scanning and transmission electron microscopy) confirmed the modifications. Calibration curves in Cormay serum (CS) and selectivity tests with chronoamperometry were used to evaluate the biosensor’s performance. Non-linear ML regression algorithms for modelling glucose concentration and calibration parameters were tested to find the best-fit model for accurate predictions. The biosensor with BGr and enzyme encapsulation showed excellent performance with a linear range of 0.75–40 mM, a correlation of 0.988, and a detection limit of 0.078 mM. Of the algorithms tested, the decision tree accurately predicted calibration parameters and achieved a coefficient of determination above 0.9 for most metrics. Multilayer perceptron models effectively predicted glucose concentration with a coefficient of determination of 0.828, demonstrating the synergy of biosensor technology and ML for reliable glucose detection. Full article

This study explores the enhancement of Carbon Fibre Reinforced Polymers (CFRPs) for automotive applications through the integration of modified carbon fibres (CF) and epoxy matrices. The research emphasizes the use of block copolymers (BCPs) and electropolymerisation techniques to improve mechanical properties and interfacial adhesion. Incorporating 2.5 wt.% D51N BCPs in the epoxy matrix led to a 64% increase in tensile strength and a 51.4% improvement in interlaminar fracture toughness. The electropolymerisation of CFs further enhanced interlaminar shear strength by 23.2%, reflecting a substantial enhancement in fibre–matrix interaction. A novel out-of-autoclave manufacturing process for an energy absorber prototype was developed, achieving significant reductions in production time and cost while maintaining performance. Compression tests demonstrated that the modified materials attained an energy absorption rate of 93.3 J/mm, comparable to traditional materials. These results suggest that the advanced materials and manufacturing processes presented in this study are promising for the development of lightweight, high-strength automotive components, meeting rigorous performance and safety standards. This research highlights the potential of these innovations to contribute significantly to the advancement of materials used in the automotive industry. Full article

Herein, chemometric-assisted synthesis of electrochemical sensors based on electropolymerised ion-imprinted polymeric (e-IIP) films was explored. Co(II)-IIPs sensors were prepared by performing electropolymerisation procedures of polymerisation mixtures comprising varying concentrations of an electroactive o-aminophenol (o-AP) monomer and Co(II) ions, respectively, according to the Taguchi L9 experimental design, exploiting the simultaneous evaluation of other controlled parameters during electrosynthesis. Each e-IIP developed from Taguchi runs was compared with the respective non-imprinted polymer (NIP) films and fitted according to Langmuir–Freudlich isotherms. Distinctive patterns of low and high-affinity films were screened based on the qualities and properties of the developed IIPs in terms of binding kinetics (KD), imprinting factor, and the heterogeneity index of produced cavities. These results can provide a generic protocol for chemometric-assisted synthesis of e-IIPs based on poly-o-AP, providing highly stable, reproducible, and high-affinity imprinted polymeric films for monitoring purposes. Full article

Polypyrrole films are commonly prepared as conductive electrode surfaces for a variety of applications. Recently, there has been increasing interest in improving the adhesive properties and biocompatibility of polypyrrole electrodes via the incorporation of bioinspired polydopamine within the polymer scaffold. However, very little is currently known about the structural effects of polydopamine incorporation during the electropolymerisation of hybrid films. In this work, we combine electrochemical quartz crystal microbalance studies, fundamental electrochemical characterisation, atomic force microscopy, and a suite of spectroscopic techniques in order to correlate changes in the structure and performance of polypyrrole–polydopamine films to the structural modifications of the nanostructure induced by polydopamine incorporation. The results indicate that polydopamine incorporation greatly increases the rate of hybrid film deposition, as well as improving adhesion, surface homogeneity, and wettability, with no compromise in charge transfer properties. Polydopamine incorporation is strongly suggested to occur in non-connected domains within a predominantly polypyrrole-like scaffold. We propose a two-step model of co-polymerisation and the subsequent surface adhesion of hybrid films. Results are expected to be of broad general interest to researchers utilizing polypyrrole and polydopamine to prepare tailor-made electrodes for biosensing and catalysis. Full article

Lithium–sulphur batteries (LiSBs) have garnered significant attention as the next-generation energy storage device because of their high theoretical energy density, low cost, and environmental friendliness. However, the undesirable “shuttle effect” by lithium polysulphides (LPSs) severely inhibits their practical application. To alleviate the shuttle effect, conductive polymers have been used to fabricate LiSBs owing to their improved electrically conducting pathways, flexible mechanical properties, and high affinity to LPSs, which allow the shuttle effect to be controlled. In this study, the applications of various conductive polymers prepared via the simple yet sophisticated electropolymerisation (EP) technology are systematically investigated based on the main components of LiSBs (cathodes, anodes, separators, and electrolytes). Finally, the potential application of EP technology in next-generation batteries is comprehensively discussed. Full article

This paper contains a comprehensive study regarding the synthesis and physicochemical properties of new hexasubstitued benzene derivatives. In this work, three compounds of this type (including two electropolymerisable monomers) were synthesized in a one-step reaction with good yields ranging from 34% to 56%. A thermal investigation shows that this type of compound is stable up to 360 °C (10% weight loss temperature). The influence of the substituents in the first and second position of the central benzene on the stability, luminescence, and (spectro)electrochemical behavior was thoroughly studied with the aid of theoretical calculations. In each case, strong blue shifting of the π-π* transition (according to 1,4-disubstitued analogs) was observed, proving this moieties’ orthogonal orientation. In the case of derivatives with a Bt-core-Bt formula (where Bt = 2,2′-bithiophene-5-yl), an electrochemical oxidation process transformed them into conducting polymers. The polymer presents extraordinary stability during multiple p-doping; thus, spectroelectrochemical measurements of polymeric films were also performed. Full article

This work summarizes the electrochemical response of a salicylic acid-based carbon electrode for use as a novel solid-state reference electrode in a redox-based pH sensor. This novel reference produces a pH insensitive response over a range of pH 3–10 in solutions with low buffer concentrations, different compositions, conductivities, and ionic strengths is produced. The pH of the local environment is shown to be determined by the chemistry and the electrochemical response of the redox active species on the surface of the electrode; the local pH can be controlled by the electropolymerized salicylic acid moieties due to the acid concentration on the surface, avoiding any perturbation in environmental pH and leading to a stable novel reference system. Sensitivities of −7.1 mV/pH unit, −2.4 mV/pH unit, −0.2 mV/pH unit, and 2.5 mV/pH units were obtained for different food medias, hydroponic solution, seawater, and cell-culture media, respectively, confirming its ability to control the local pH of the electrode. This reference system is paired with a new pH sensing element based on electropolymerized flavanone to provide a calibration free, pH sensitive sensor to effectively and accurately measure the pH of various media with high viscosity, low conductivity, low/high buffer concentration or cell-culture environment, presenting a maximum error of +/−0.03 pH units. Full article

The present study focuses on the effect of two novel carbon fibre surface treatments, electropolymerisation of methacrylic acid and air pressure plasma, on the mechanical properties and structural integrity of carbon-fibre-reinforced composites under operational conditions. Extensive mechanical testing was applied, both in nano- and macro-scale, to assess the performance of the composites and the interphase properties after ultraviolet/humidity weathering. The results of the mechanical assessment are supported by structure, surface, and chemistry examination in order to reveal the failure mechanism of the composites. Composites with the electropolymerisation treatment exhibited an increase of 11.8% in interlaminar shear strength, while APP treatment improved the property of 23.9%, rendering both surface treatments effective in increasing the fibre-matrix adhesion. Finally, it was proven that the developed composites can withstand operational conditions in the long term, rendering them suitable for a wide variety of structural and engineering applications. Full article

Conjugated polymers are widely used in the development of sensors, but even though they are sensitive and robust, they typically show limited selectivity, being cross-sensitive to many substances. In turn, molecular imprinting is a method involving modification of the microstructure of the surface to incorporate cavities, whose shape matches that of the “template”—the analyte to be detected, resulting in high selectivity. The primary goal of this review is to report on and briefly explain the most relevant recent developments related to sensors utilising molecularly imprinted polypyrrole layers and their applications, particularly regarding the detection of bioactive substances. The key approaches to depositing such layers and the most relevant types of analytes are highlighted, and the various trends in the development of this type of sensors are explored. Full article

Polyaniline (PANI) is a conducting polymer, widely used in gas-sensing applications. Due to its classification as a semiconductor, PANI is also used to detect reducing ammonia gas (NH₃), which is a well-known and studied topic. However, easier, cheaper and more straightforward procedures for sensor fabrication are still the subject of much research. In the presented work, we describe a novel, more controllable, synthesis approach to creating NH₃ PANI-based receptor elements. The PANI was electrochemically deposited via cyclic voltammetry (CV) on screen-printed electrodes (SPEs). The morphology, composition and surface of the deposited PANI layer on the Au electrode were characterised with electron microscopy, Fourier-transform infrared spectroscopy and profilometry. Prior to the gas-chamber measurement, the SPE was suitably modified by Au sputtering the individual connections between the three-electrode system, thus showing a feasible way of converting a conventional three-electrode electrochemical SPE system into a two-electrode NH₃-gas detecting system. The feasibility of the gas measurements’ characterisation was improved using the gas analyser. The gas-sensing ability of the PANI-Au-SPE was studied in the range 32–1100 ppb of NH₃, and the sensor performed well in terms of repeatability, reproducibility and sensitivity. Full article

Our contribution focuses on a correlative study of polyaniline (PANI) electropolymerisation and UV/VIS spectroscopy. PANI was prepared via electro-oxidation using a potentiodynamic method on commercial gold screen-printed electrodes (Au-SPE). By using an in-situ spectroelectrochemical method, the development of the polymer was observed from monomer, monomer oxidation to final polymer formation and its transformations between the oxidation forms. The results confirm the spontaneous doping of the polymer during the polymerisation, the instability of leucoemeraldine form in air and its two-stage oxidation to emeraldine form. The final conductive PANI deposited on Au-SPE will be used as sensor element for the detection of toxic organic compounds. Full article

Preliminary results on an electrosynthesized ion imprinted polymeric film (IIP-film) for Cd(II) ions determination in sensor development are here reported. The sensor was prepared by electropolymerization of 4-aminophenylacetic acid (4-APA) monomer in presence of Cd(II) ions, which acts as the template. The screen-printed carbon electrodes (SPCE) were used as transducer during sensor development, whereas the cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were selected as the electrochemical methods for the synthesis and Cd(II) ions sensing, respectively. The incubation of the developed sensor in NaOH 250 mM involved into remove the template and the formation of specific recognition cavities into the polymer. A multivariate optimization based on central composite design (CCD) was employed to study the effect of three independent parameters on electrochemical performances of the sensor. The electrochemical characterization of sensors was performed in ferrocyanide-ferricyanide redox couple and in KCl 0.1 M, the latter revealing redox properties from the polymeric film. The performances of sensors and the control (non-imprinted film, NIP) was observed in sodium acetate buffer (100 mM, pH = 5) over the Cd(II) concentration range 0.1–10 µM. Full article

Carbon Fibres (CFs) are widely used in textile-reinforced composites for the construction of lightweight, durable structures. Since their inert surface does not allow effective bonding with the matrix material, the surface treatment of fibres is suggested to improve the adhesion between the two. In the present study, different surface modifications are compared in terms of the mechanical enhancement that they can offer to the fibres. Two main advanced technologies have been investigated; namely, plasma treatment and electrochemical treatment. Specifically, active screen plasma and low-pressure plasma were compared. Regarding the electrochemical modification, electrochemical oxidation and electropolymerisation of monomer solutions of acrylic and methacrylic acids, acrylonitrile and N-vinyl pyrrolidine were tested for HTA-40 CFs. In order to assess the effects of the surface treatments, the morphology, the physicochemical properties, as well as the mechanical integrity of the fibres were investigated. The CF surface and polymeric matrix interphase adhesion in composites were also analysed. The improvement of the carbon fibre’s physical–mechanical properties was evident for the case of the active screen plasma treatment and the electrochemical oxidation. Full article