Incorporation of Bismuth(III) Oxide Nanoparticles into Carbon Ceramic Composite: Electrode Material with Improved Electroanalytical Performance in 4-Chloro-3-Methylphenol Determination.

In this study, a carbon ceramic electrode (CCE) with improved electroanalytical performance was developed by bulk-modifying it with bismuth(III) oxide nanoparticles (Bi-CCE). Characterization of the Bi-CCE was conducted employing atomic force microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy, cyclic voltammetry (CV), and electrochemical impedance spectroscopy. Comparative analysis was conducted using an unmodified CCE. The findings proved that the incorporation of Bi2O3 nanoparticles into the CCE significantly altered the morphology and topography of the ceramic composite, and it improved the electrochemical properties of CCE. Notably, the Bi-CCE demonstrated a prolonged operational lifespan of at least three months, and there was a high reproducibility of the electrode preparation procedure. The developed Bi-CCE was effectively employed to explore the electrochemical behavior and quantify the priority environmental pollutant 4-chloro-3-methylphenol (PCMC) using CV and square-wave voltammetry (SWV), respectively. Notably, the developed SWV procedure utilizing Bi-CCE exhibited significantly enhanced sensitivity (0.115 µA L mol-1), an extended linearity (0.5-58.0 µmol L-1), and a lower limit of detection (0.17 µmol L-1) in comparison with the unmodified electrode. Furthermore, the Bi-CCE was utilized effectively for the detection of PCMC in a river water sample intentionally spiked with the compound. The selectivity toward PCMC determination was also successfully assessed.

Fabrication and Characterization of an Electrochemical Platform for Formaldehyde Oxidation, Based on Glassy Carbon Modified with Multi-Walled Carbon Nanotubes and Electrochemically Generated Palladium Nanoparticles.

This study outlines the fabrication process of an electrochemical platform utilizing glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNTs) and palladium nanoparticles (PdNPs). The MWCNTs were applied on the GCE surface using the drop-casting method and PdNPs were produced electrochemically by a potentiostatic method employing various programmed charges from an ammonium tetrachloropalladate(II) solution. The resulting GCEs modified with MWCNTs and PdNPs underwent comprehensive characterization for topographical and morphological attributes, utilizing atomic force microscopy and scanning electron microscopy along with energy-dispersive X-ray spectrometry. Electrochemical assessment of the GCE/MWCNTs/PdNPs involved cyclic voltammetry (CV) and electrochemical impedance spectroscopy conducted in perchloric acid solution. The findings revealed even dispersion of PdNPs, and depending on the electrodeposition parameters, PdNPs were produced within four size ranges, i.e., 10-30 nm, 20-40 nm, 50-60 nm, and 70-90 nm. Additionally, the electrocatalytic activity toward formaldehyde oxidation was assessed through CV. It was observed that an increase in the size of the PdNPs corresponded to enhanced catalytic activity in the formaldehyde oxidation reaction on the GCE/MWCNTs/PdNPs. Furthermore, satisfactory long-term stability over a period of 42 days was noticed for the GCE/MWCNTs/PDNPs(100) material which demonstrated the best electrocatalytic properties in the electrooxidation reaction of formaldehyde.

The Composite Material of (PEDOT-Polystyrene Sulfonate)/Chitosan-AuNPS-Glutaraldehyde/as the Base to a Sensor with Laccase for the Determination of Polyphenols.

The described research aimed to develop the properties of the conductive composite /poly(3,4-ethylenedioxy-thiophene-poly(4-lithium styrenesulfonic acid)/chitosan-AuNPs-glutaraldehyde/ (/PEDOT-PSSLi/chit-AuNPs-GA/) and to develop an electrochemical enzyme sensor based on this composite material and glassy carbon electrodes (GCEs). The composite was created via electrochemical production of an /EDOT-PSSLi/ layer on a glassy carbon electrode (GCE). This layer was covered with a glutaraldehyde cross-linked chitosan and doped with AuNPs. The influence of AuNPs on the increase in the electrical conductivity of the chitosan layers and on facilitating the oxidation of polyphenols in these layers was demonstrated. The enzymatic sensor was obtained via immobilization of the laccase on the surface of the composite, with glutaraldehyde as the linker. The investigation of the surface morphology of the GCE/PEDOT-PSSLi/chit-AuNPs-GA/Laccase sensor was carried out using SEM and AFM microscopy. Using EDS and Raman spectroscopy, AuNPs were detected in the chitosan layer and in the laccase on the surface of the sensor. Polyphenols were determined using differential pulse voltammetry. The biosensor exhibited catalytic activity toward the oxidation of polyphenols. It has been shown that laccase is regenerated through direct electron transfer between the sensor and the enzyme. The results of the DPV tests showed that the developed sensor can be used for the determination of polyphenols. The peak current was linearly proportional to the concentrations of catechol in the range of 2-90 µM, with a limit of detection (LOD) of 1.7 µM; to those of caffeic acid in the range of 2-90 µM, LOD = 1.9 µM; and to those of gallic acid in the range 2-18 µM, LOD = 1.7 µM. Finally, the research conducted in order to determine gallic acid in a natural sample, for which white wine was used, was described.

Selected Spectroscopic Techniques for Surface Analysis of Dental Materials: A Narrative Review.

The presented work focuses on the application of spectroscopic methods, such as Infrared Spectroscopy (IR), Fourier Transform Infrared Spectroscopy (FT-IR), Raman spectroscopy, Ultraviolet and Visible Spectroscopy (UV-Vis), X-ray spectroscopy, and Mass Spectrometry (MS), which are widely employed in the investigation of the surface properties of dental materials. Examples of the research of materials used as tooth fillings, surface preparation in dental prosthetics, cavity preparation methods and fractographic studies of dental implants are also presented. The cited studies show that the above techniques can be valuable tools as they are expanding the research capabilities of materials used in dentistry.

Cytotoxic effect, generation of reactive oxygen/nitrogen species and electrochemical properties of Cu(ii) complexes in comparison to half-sandwich complexes of Ru(ii) with aminochromone derivatives.

This paper describes the synthesis of new 6-aminoflavone (6AFl (3)) and 6-aminochromone (6AC (4)) complexes with Cu(ii) and Ru(ii) ions ([Cu(6AC)2Cl2] (3a), [Cu(6AFl)2Cl2] (4a), [Ru(p-cymene)(6AC)Cl2] (4b)) and comparison of their properties with the previously described 7-aminoflavone (7AFl (1)) and 7-amino-2-methylchromone (7A2MC (2)) analogues. The cytotoxic effect of all these complexes against two human leukaemia cell lines (HL-60 and NALM-6), melanoma WM-115 cells and COLO205 cells, is determined. The cytotoxicity of copper(ii) complexes, especially [Cu(6AFl)2Cl2] (3a) was higher than ruthenium(ii) complexes with the same ligands. Their cytotoxic potency was also stronger in comparison to the referential agents like cisplatin. The pro-oxidative properties were determined for the most active complexes and their ability to generate ROS (reactive oxygen species)/RNS (reactive nitrogen species) in cancer cells was confirmed. The type of ligand and the chemical structure of the tested complexes had an influence on the level of ROS/RNS generated in cancer cells. The redox properties of the copper complex compounds were evaluated by cyclic voltammetry, and compared with the data for Ru(ii) complexes. The reduction and oxidation processes of Ru(iii)/Ru(ii) and Cu(ii)/Cu(i) were described as quasi-reversible.

Synthesis and characterization of the thermally reduced graphene oxide in argon atmosphere, and its application to construct graphene paste electrode as a naptalam electrochemical sensor.

New insight into the preparation of sensitive carbon-based electrochemical electrode is provided by examining the properties of thermally reduced graphene oxide (TRGO). In this paper, TRGO was prepared by thermal reduction of graphene oxide (GO) in argon atmosphere, and characterized by Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), and atomic force microscopy (AFM). Results showed that thermal reduction in argon was effective to remove oxygen-containing functional groups in GO, and graphene sheets were obtained. Furthermore, TRGO was used to prepare thermally reduced graphene oxide paste electrode (TRGOPE) which showed excellent conductivity and fast electron transfer kinetics confirmed by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrode was applied to determination of the pesticide naptalam (Nap) in square-wave voltammetric (SWV) mode. The corresponding current at approx. +1.0 V increased linearly with the Nap concentration within two linear dynamic ranges (LDR) of 0.1-1.0 µmol L-1 (LDR1) and 1.0-10.0 µmol L-1 (LDR2). The limits of detection (LOD) and quantification (LOQ) for Nap were calculated as 0.015 µmol L-1 and 0.051 µmol L-1, respectively. In comparison to the carbon paste electrode (CPE) the results showed that the TRGOPE possesses advantages in terms of linearity, sensitivity and detectability.

Improved electroanalytical characteristics for the determination of pesticide metobromuron in the presence of nanomaterials.

In the present work, bare ultra trace graphite electrode (UTGE), UTGE modified with multi-walled carbon nanotubes (UTGE-MWCNTs), and UTGE modified with graphene nanoplatelets (UTGE-GNPs) were considered as working electrodes. For the first time, the UTGEs were modified with MWCNTs and GNPs by simple and fast drop-casting approach (the whole procedures take no more times than ca. 30 min). The comprehensive microscopic and electrochemical characterization of the unmodified and the modified UTGEs was conducted by means of atomic force microscopy (AFM), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV) techniques. The prepared electrodes were further applied for the analytical purposes, and the procedures for the square-wave voltammetric (SWV) determination of pesticide metobromuron (Mbn) using the bare UTGE, the UTGE-MWCNTs, and the UTGE-GNPs were developed. For the first time, this compound was electrochemically investigated. The SWV measurements were performed in Britton-Robinson buffer (B-R) solution at pH 2.0 as a supporting electrolyte. SWV parameters, i.e. amplitude, frequency, and step potential, were optimized. The linear relationships between peak current vs. increasing concentrations of Mbn were defined using the bare UTGE, the UTGE-MWCNTs, and the UTGE-GNPs, and the limits of detection were calculated (0.13, 0.11, 0.048 µmol L-1, respectively). The analytical parameters determined from calibration curves indicate similar sensitivity on all tested electrodes, however, the widest linearity range as well as the lowest LOD and LOQ values were achieved on the UTGE modified with GNPs. The utility of the proposed method with the UTGE-GNPs was verified by the quantitative analysis of Mbn in soil samples with satisfactory results (recovery of 99.1%). Furthermore, the impact of possible interferences was tested and evaluated, and obtained results proved good selectivity of the proposed method.

ß-Cyclodextrins incorporated multi-walled carbon nanotubes modified electrode for the voltammetric determination of the pesticide dichlorophen.

In this work, a glassy carbon electrode modified with ß-cyclodextrins and multi-walled carbon nanotubes (ß-CDs/MWCNTs/GCE) was constructed and applied for the square-wave adsorptive stripping voltammetric (SWAdSV) determination of the pesticide dichlorophen (Dcp). For the first time, this compound was electrochemically investigated. The voltammetric measurements were conducted in phosphate buffer (PBS) at pH 6.5 as a supporting electrolyte, and SWAdSV technique parameters were optimized. A linear calibration curve in the wide concentration range from 5.0 × 10-8molL-1 to 2.9 × 10-6molL-1 was obtained. Excellent analytical performance in terms of limit of detection (LOD) of 1.4 × 10-8molL-1 was achieved. The utility of the proposed method was verified by the quantitative analysis of Dcp in Pilica River water samples with satisfactory results. The characterization of modified electrodes was conducted by means of atomic force microscopy (AFM), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). Moreover, in this work, the dissociation constants (pKa) of Dcp using potentiometric pH titration were estimated. The stoichiometry of the Dcp-ß-CDs inclusion complex formed in solution was determined by proton nuclear magnetic resonance (1H NMR) spectroscopy, and a binding constant (ß2) was estimated from NMR titration studies.