Search Results (43)

Much progress has been made in the determination of As (III), while numerous electrochemical sensors based on metal nanomaterials with significant sensitivity and precision have been developed. However, further research is still required to achieve rapid detection and avoid interference from other metal ions (especially copper ions). In this study, bimetallic AuPt nanoparticles are electrochemically modified with screen printing electrodes. What’s more, L-cysteine also self-assembles with AuNPs through Au-S bond to enhance the electrochemical performance. To overcome the interference of Cu (II) in the sensing process, the reduced iron powder was chosen to remove Cu (II) and other oxidizing organics in aqueous solutions. The lowest detectable amount is 0.139 ppb, a linear range of 1~50 ppb with superlative stability by differential pulse anodic stripping voltammetry. Fortunately, the reduced iron powder could eliminate the Cu (II) with no effect on the As (III) signal. Full article

Copper is an essential element in living organisms and is crucial in marine ecosystems. However, excessive concentrations can lead to seawater pollution and pose a risk of toxicity to marine organisms, as it is a heavy metal. In addition, it can enter the human body through the food chain, potentially endangering human health. Consequently, there is increasing focus on the rapid and highly sensitive detection of copper ions (Cu²⁺). We prepared a graphite carbon electrode modified with graphitised multi-walled carbon nanotubes/copper(II) ion carrier IV (GMWCNT/copper(II) ion carrier IV/glassy carbon electrode (GCE)) using a drop-coating method. Scanning electron microscopy (SEM) analysis revealed that the composite material film possessed a large surface area. Incorporating this composite material significantly enhanced the adsorption capacity for ions on the electrode surface and greatly improved conductivity. Differential pulse anodic stripping voltammetry (DPASV) was employed to quantify copper levels in seawater. Under optimal experimental conditions, a strong linear relationship was observed between the Cu²⁺ response peak current and its concentration within a range of 50–500 µg L⁻¹, with a correlation coefficient of 0.996. The GMWCNT/copper(II) ion carrier IV/GCE exhibited excellent stability and reproducibility, achieving a low detection limit for Cu²⁺ at 0.74 µg L⁻¹ when applied to copper detection in seawater. Furthermore, spiked recovery rates ranging from 98.6% to 102.8% demonstrated the method’s high sensitivity, convenient operation, and practical value for real-world applications in detecting Cu²⁺ levels in seawater. Full article

Electrochemical (EC) detection is a powerful tool supporting simple, low-cost, and rapid analysis. Although screen printing is commonly used to mass fabricate disposable EC chips, its mask is relatively expensive. In this research, we demonstrated a method for fabricating three-electrode EC chips using 3D printing of relatively high-viscosity paste. The electrodes consisted of two layers, with carbon paste printed over silver/silver chloride paste, and the printed EC chips were baked at 70 °C for 1 h. Engineering challenges such as bulging of the tubing, clogging of the nozzle, dripping, and local accumulation of paste were solved by material selection for the tube and nozzle, and process optimization in 3D printing. The EC chips demonstrated good reversibility in redox reactions through cyclic voltammetry tests, and reliably detected heavy metal ions Pb(II) and Cd(II) in solutions using differential pulse anodic stripping voltammetry measurements. The results indicate that by optimizing the 3D printing of paste, EC chips can be obtained by maskless and flexible 3D printing techniques in lieu of screen printing. Full article

This work presents coal analyses for heavy metal content (Tl, Cu, Zn, Cd, Fe). The tested coal samples came from a Russian deposit in the Kuzbass Basin (Novosibirsk and Kemerovo Oblasts, near Kazakhstan) and from Poland. The concentration of thallium in coal was determined using DPASV—differential pulse anodic stripping voltammetry—and other metals were examined with FAAS, i.e., flame atomic absorption spectrometry. The study confirmed the presence of thallium in the tested coal sample. The coal samples from outside the European Union contained four times more thallium (the maximum content of thallium in coal has been determined to be 0.636 mg·kg⁻¹) than the samples of Polish coal (where the maximum content of thallium was 0.055 mg·kg⁻¹). Cadmium concentration was on average 1.99 mg·kg⁻¹ in the samples from outside the European Union, and 1.2 mg·kg⁻¹ in the samples of Polish coal. Zinc concentration in the samples from outside the European Union was on average 11.27 mg·kg⁻¹, and in the samples of Polish coal approx. 7 mg·kg⁻¹. In addition, iron concentration in all coal samples was determined as 14.96 mg·kg⁻¹, whereas copper concentration in the samples from outside the European Union averaged as 3.96 mg·kg⁻¹. The obtained results do not show any correlation between the presence of thallium and the presence of other metals. It is worth noting that heavy metals pose a threat to living organisms due to their persistence and bioaccumulation, particularly in the context of dust emissions to the atmosphere. Full article

Bisphenol A is one of the most widely used industrial compounds. Over the years, it has raised severe concern as a potential hazard to the human endocrine system and the environment. Developing robust and easy-to-use sensors for bisphenol A is important in various areas, such as controlling and monitoring water purification and sewage water systems, food safety monitoring, etc. Here, we report an electrochemical method to fabricate a bisphenol A (BPA) sensor based on a modified Au nanoparticles/multiwalled carbon nanotubes composite electrocatalyst electrode (AuCu-UPD/MWCNTs/GCE). Firstly, the Au-Cu alloy was prepared via a convenient and controllable Cu underpotential/bulk Au co-electrodeposition on a multiwalled modified carbon nanotubes glassy carbon electrode (GCE). Then, the AuCu-UPD/MWCNTs/GCE was obtained via the electrochemical anodic stripping of Cu underpotential deposition (UPD). Our novel prepared sensor enables the high-electrocatalytic and high-performance sensing of BPA. Under optimal conditions, the modified electrode showed a two-segment linear response from 0.01 to 1 µM and 1 to 20 µM with a limit of detection (LOD) of 2.43 nM based on differential pulse voltammetry (DPV). Determination of BPA in real water samples using Au_Cu-UPD/MWCNTs/GCE yielded satisfactory results. The proposed electrochemical sensor is promising for the development of a simple, low-cost water quality monitoring system for the detection of BPA in ambient water samples. Full article

The high-performance determination of heavy metal ions (Cd²⁺) in water sources is significant for the protection of public health and safety. We have developed a novel sensor of nanograss boron and nitrogen co-doped diamond (NGBND) to detect Cd²⁺ using a simple method without any masks or reactive ion etching. The NGBND electrode is constructed based on the co-doped diamond growth mode and the removal of the non-diamond carbon (NDC) from the NGBND/NDC composite. Both the enlarged surface area and enhanced electrochemical performance of the NGBND film are achievable. Scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, cyclic voltammetry, electrochemical impedance spectroscopy, and differential pulse anodic stripping voltammetry (DPASV) were used to characterize the NGBND electrodes. Furthermore, we used a finite element numerical method to research the current density near the tip of NGBND. The NGBND sensor exhibits significant advantages for detecting trace Cd²⁺ via DPASV. A broad linear range of 1 to 100 μg L⁻¹ with a low detection limit of 0.28 μg L⁻¹ was achieved. The successful application of this Cd²⁺ sensor indicates considerable promise for the sensitive detection of heavy metal ions. Full article

Nano-needle boron-doped diamond (NNBDD) films increase their performance when used as electrodes in the determination of Pb²⁺. We develop a simple and economical route to produce NNBDD based on the investigation of the diamond growth mode and the ratio of diamond to non-diamond carbon without involving any templates. An enhancement in surface area is achievable for NNBDD film. The NNBDD electrodes are characterized through scanning electron microscopy, Raman spectroscopy, X-ray diffraction, cyclic voltammetry, electrochemical impedance spectroscopy, and differential pulse anodic stripping voltammetry (DPASV). Furthermore, we use a finite-element numerical method to research the prospects of tip-enhanced electric fields for sensitive detection at low Pb²⁺ concentrations. The NNBDD exhibits significant advantages and great electrical conductivity and is applied to detect trace Pb²⁺ through DPASV. Under pre-deposition accumulation conditions, a wide linear range from 1 to 80 µgL⁻¹ is achieved. A superior detection limit of 0.32 µgL⁻¹ is achieved for Pb²⁺, which indicates great potential for the sensitive detection of heavy metal ions. Full article

Mercuric ion (Hg²⁺) in aqueous media is extremely toxic to the environment and organisms. Therefore, the ultra-trace electrochemical determination of Hg²⁺ in the environment is of critical importance. In this work, a new electrochemical Hg²⁺ sensing platform based on porous activated carbon (BC/Cu₂O) modified with cuprous oxide was developed using a simple impregnation pyrolysis method. Differential pulse anodic stripping voltammetry (DPASV) was used to investigate the sensing capability of the BC/Cu₂O electrode towards Hg²⁺. Due to the excellent conductivity and large specific surface area of BC, and the excellent catalytic activity of Cu₂O nanoparticles, the prepared BC/Cu₂O electrode exhibited excellent electrochemical activity. The high sensitivity of the proposed system resulted in a low detection limit of 0.3 ng·L⁻¹ and a wide linear response in the ranges from 1.0 ng·L⁻¹ to 1.0 mg·L⁻¹. In addition, this sensor was found to have good accuracy, acceptable precision, and reproducibility. All of these results show that the BC/Cu₂O composite is a promising material for Hg²⁺ electrochemical detection. Full article

Three novel dibenzo-18-crown-6 aldimines were successfully synthesised and structurally characterised via various spectroscopic methods (¹H,¹³H NMR, FT-IR) and their solution phase lead binding behaviours probed via absorption spectroscopy, the results are supported by Density Functional Theoretical (DFT) modelling. These methods revealed that the asymmetric nature of these compounds is such that at equilibrium the ether cavity adopts an open configuration where the constituent oxygen atoms exhibit a highly negative electrostatic potential; hence, they spontaneously (ΔG~−58 kJ mol⁻¹) interact/bind aqueous lead ions to form stable 2:1 metal–ligand complexes. As indicated by cyclic and square voltammetry studies, all compounds are redox active and polymerise relatively easily onto a platinum surface to form a multi-layered lead Ion-selective Membrane (ISM), the structure of which is confirmed by Scanning Electron Microscopy (SEM) and Electrochemical Impedance Spectroscopy (EIS). These novel Ion-selective Electrodes (ISEs), as characterised by Differential Pulse Anodic Stripping Voltammetry (D PASV), allow selective electrochemical detection and quantification of lead at concentrations as low as 10 ppm, over a range of 15–60 ppm, with only minimal interference from mercury(II) and aluminium(III) ions at a 1:1 analyte-interferent ratio. Full article

The presence of heavy metals in craft beers can endanger human health if the total metal content exceeds the exposure limits recommended by sanitary standards; in addition, they can cause damage to the quality of the beer. In this work, the concentration of Cd(II), Cu(II), and Fe(III) was determined in 13 brands of craft beer with the highest consumption in Quito, Ecuador, by differential pulse anodic stripping voltammetry (DPASV), using as boron-doped diamond (BDD) working electrode. The BDD electrode used has favorable morphological and electrochemical properties for the detection of metals such as Cd(II), Cu(II), and Fe(III). A granular morphology with microcrystals with an average size between 300 and 2000 nm could be verified for the BDD electrode using a scanning electron microscope. Double layer capacitance of the BDD electrode was 0.01412 μF cm⁻², a relatively low value; Ip_ox/Ip_red ratios were 0.99 for the potassium ferro-ferricyanide system in BDD, demonstrating that the redox process is quasi-reversible. The figures of merit for Cd(II), Cu(II), and Fe(III) were; DL of 6.31, 1.76, and 1.72 μg L⁻¹; QL of 21.04, 5.87, and 5.72 μg L⁻¹, repeatability of 1.06, 2.43, and 1.34%, reproducibility of 1.61, 2.94, and 1.83% and percentage of recovery of 98.18, 91.68, and 91.68%, respectively. It is concluded that the DPASV method on BDD has acceptable precision and accuracy for the quantification of Cd(II), Cu(II), and Fe(III), and it was verified that some beers did not comply with the permissible limits of food standards. Full article

Recently, nanotechnology and nanoparticles (NPs) such as AgNPs and AuNPs have become important in analytical chemistry due to their great potential to improve the performance of electrochemical sensors. In this work, Ag and Au nanoparticles have been synthesized using a green route in which a grape stalk waste extract is used as a reducing agent to obtain metallic nanoparticles. These NPs were used to customize the surface of commercial screen-printed electrodes (SPCNFEs). The spin-coating method was used to modify commercial SPCNFEs under a nitrogen atmosphere. The resulting electrodes were used in a determination study of Cd(II), Pb(II), and U(VI) with differential pulse anodic stripping voltammetry (DPASV). The customized green AgNPs and AuNPs electrodes presented higher sensitivity and electroanalytical performance than the non-modified SPCNFE. The results showed that the best analytical parameters were obtained with the green, silver nanoparticle SPCNFEs, with a LOD of 0.12 μg L⁻¹ for Pb(II), which is a lower value compared to the most restrictive regulation guidelines. Additionally, the U(VI) ion was successfully determined using the developed G-AgNPs-SPCNFE in spiked tap water, showing comparable results with the ICP-MS technique. Full article

In this paper, graphdiyne (GDY)−modified glassy carbon electrode was prepared and further used for the sensitive and simultaneous detection of three target heavy metal ions of Zn²⁺, Cd²⁺ and Hg²⁺ by codeposition with Bi³⁺ in the mixture solution. GDY−modified electrodes exhibit a larger electrode area and abundant active sites, which is favorable for absorbing more metal ions. Bismuth has low toxicity and can form alloys with zinc, cadmium and mercury. Therefore, three kinds of heavy metal ions can be pre-concentrated with bismuth on the GDY−modified electrode surface, and the following stripping analysis results in high sensitivity and selectivity. By using differential pulse anodic stripping voltammetry, the detection ranges of Zn²⁺, Cd²⁺ and Hg²⁺ were from 2.0 to 100.0 μM with low detection limits of 0.255 μM, 0.367 μM and 0.796 μM, respectively. In addition, the sensor showed excellent repeatability, reproducibility, and stability, which was applied to sensitive analysis of river water samples with satisfactory results. Full article

In this study, an electrochemical sensor for the monitoring of Hg (II) at trace levels by using differential pulse anodic stripping voltammetry has been reported. Basically the electrochemical sensor is a Phanerochaete chrysosporium-based carbon paste electrode. Here, Phanerochaete chrysosporium has played a new vital role in electrochemical detection of heavy metal apart from its known contribution in their removal. Optimal voltammetric response was observed at −0.7 V deposition potential l, 5% biomass concentration ratio (w/w), and neutral pH conditions with 12 min as the accumulation time. Selectivity was evaluated in the presence of different interfering cations. Linear range was observed for 5–50 µgL⁻¹ of metal concentration with a detection limit of 4.4 µgL⁻¹. The equivalence of new and reference analytical methods was statistically assessed in mercury samples collected from chlor-alkali industrial effluent by correlation of results (Pearson’s product-moment correlation), weighted Deming regression analysis, paired comparison test, relative standard deviation (RSD), median relative error (MRE), root mean square error (RMSE), and predicted residual sum of square (PRESS). This work presented a simple, efficient, and promising analytical tool in trace level detection of Hg (II), as compared to previously reported carbon paste electrodes based on biological material. Full article

The use of economic methods to design and fabricate flexible copper sensors decorated with bismuth micro/nanodentrites for the detection of lead and cadmium in sweat is demonstrated. The flexible copper sensors were constructed with simple and cost-effective materials; namely, flexible and adhesive conductive copper tape, adhesive label containing the design of a three-electrode electrochemical system, and nail polish or spray as a protective layer. The flexible copper device consisted of a working electrode decorated with bismuth micro/nanodentrites using an electrodeposition technique, a copper pseudo-reference and copper counter electrodes. Under optimal experimental conditions, the flexible sensing platform showed excellent performance toward the detection of lead and cadmium using differential pulse anodic stripping voltammetry (DPAdSV) in a wide linear range from 2.0 μM to 50 μM with acceptable reproducibility and repeatability, and limits of detection and quantification of 5.36 and 17.9 μM for Cd²⁺ ions and 0.76 μM and 2.5 for Pb²⁺ ions. Studies of addition and recovery in spiked artificial sweat sample were performed, with a recovery of 104.6%. The flexible copper device provides a great opportunity for application in wearable perspiration-based healthcare systems or portable sensors to detect toxic metals in biological samples. Full article

A talc-like magnesium phyllosilicate functionalized with amine groups (TalcNH₂), useful as sensor material in voltammetry stripping analysis, was synthesized by a sol–gel-based processing method. The characterizations of the resulting synthetic organoclay by scanning electron microscopy (SEM), X-ray diffraction, N₂ sorption isotherms (BET method), Fourier transform infrared spectroscopy (FTIR), CHN elemental analysis and UV–Vis diffuse reflectance spectroscopy (UV–Vis-DRS) demonstrated the effectiveness of the process used for grafting of amine functionality in the interlamellar clay. The results indicate the presence of organic moieties covalently bonded to the inorganic lattice of talc-like magnesium phyllosilicate silicon sheet, with interlayer distances of 1568.4 pm. In an effort to use a talc-like material as an electrode material without the addition of a dispersing agent and/or molecular glue, the TalcNH₂ material was successfully dispersed in distilled water in contrast to natural talc. Then, it was used to modify a glassy carbon electrode (GCE) by drop coating. The characterization of the resulting modified electrode by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) revealed its charge selectivity ability. In addition, EIS results showed low charge transfer resistance (0.32 Ω) during the electro-oxidation of [Fe(CN)₆]³⁻. Kinetics studies were also performed by EIS, which revealed that the standard heterogeneous electron transfer rate constant was (0.019 ± 0.001) cm.s⁻¹, indicating a fast direct electron transfer rate of [Fe(CN)₆]³⁻ to the electrode. Using anodic adsorptive stripping differential pulse voltammetry (DPV), fast and highly sensitive determination of Pb(II) ions was achieved. The peak current of Pb²⁺ ions on TalcNH₂/GCE was about three-fold more important than that obtained on bare GCE. The calculated detection and quantification limits were respectively 7.45 × 10⁻⁸ M (S/N = 3) and 24.84 × 10⁻⁸ M (S/N 10), for the determination of Pb²⁺ under optimized conditions. The method was successfully used to tap water with satisfactory results. The results highlight the efficient chelation of Pb²⁺ ions by the grafted NH₂ groups and the potential of talc-like amino-functionalized magnesium phyllosilicate for application in electrochemical sensors. Full article