An anodic stripping voltammetric approach for total mercury determination in sea sponges from the Niger Delta region of Nigeria.

Mercury pollution from ongoing crude oil refining and waste disposal activities threatens aquatic ecosystems and human health in the Niger Delta. Mercury monitoring exercise in this region is challenging due to the high cost of traditional instruments and the complexity of marine samples. This research presents a novel analytical method using differential pulse anodic stripping voltammetry (DPASV) with a glassy carbon electrode (GCE) to determine mercury levels in sea sponges from the Niger Delta. Using a 2.36 M HCl + 2.4 M NaCl supporting electrolyte, -0.6 V deposition potential, and 300 s deposition time, average mercury levels were found to be 0.98 mg kg-1, 0.63 mg kg-1 and 0.42 mg kg-1 for Ibiotirem, Kaa and Samanga, respectively. The result showed that the Niger Delta is polluted, and remediation efforts are necessary. Furthermore, the DPASV method could be used for routine mercury monitoring as it is cost-effective, user-friendly, and highly sensitive.

Adsorptive Stripping Voltammetric Quercetin Determination in Pharmaceuticals and Urine Samples Using a Long Service-Life Array of Carbon Composite Microelectrodes.

This article presents for the first time a new working electrode with a long service life- the bismuth-plated array of carbon composite microelectrodes for the simple, fast and sensitive determination of quercetin by adsorptive stripping voltammetry. The main experimental conditions were selected. The calibration graph was linear from 1 × 10-9 to 2 × 10-8 mol L-1 with an accumulation time of 60 s. The detection limit was equal to 4.8 × 10-10 mol L-1. The relative standard deviation for 2 × 10-8 mol L-1 of quercetin was 4.4% (n = 7). Possible interference effects resulting from the presence of other organic and surface active compounds and interfering ions were studied. The developed procedure was successfully applied to determine quercetin in pharmaceutical preparations and the spiked urine samples.

Electrochemical sensor for the analysis of 5-hydroxymethylcytosine in the presence of cytosine using pencil graphite electrode.

In recent years, important efforts have been made to elucidate the mechanisms of epigenetic regulation, and one of the most studied epigenetic modifications was DNA methylation/demethylation. In this study, the voltammetric behaviour of 5-hydroxymethylcytosine was studied in the pH range of 2.00-11.00 using pencil graphite electrodes by differential pulse and square wave voltammetry. The effect of buffer solutions, scan rate, square wave voltammetry parameters, and stripping conditions on the voltammetric responses of 5-hydroxymethylcytosine were performed. The electrochemical oxidation process of 5-hydroxymethylcytosine on the pencil graphite electrode was realized under adsorption control. In human urine, by square wave stripping voltammetry, 5-hydroxymethylcytosine was quantified in a concentration range of 1.00 × 10-5 M-2.00 × 10-4 M. The proposed method was tested in the presence of cytosine in human urine. The recovery value of 5-hydroxymethylcytosine was found to be 99.57 %.

Surface-Initiated Reversible Addition-Fragmentation Chain Transfer Polymerization (SI-RAFT) to Produce Molecularly Imprinted Polymers on Graphene Oxide for Electrochemical Sensing of Methylparathion.

A nonenzymatic redox-responsive sensor was put forward for the detection of methylparathion (MP) by designing globular nanostructures of molecularly imprinted polymers on graphene oxide (GO@MIPs) via surface-initiated reversible addition-fragmentation chain transfer polymerization (SI-RAFT). Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), and small-angle X-ray scattering (SAXS) studies have confirmed the successful formation of receptor layers of MIPs on RAFT agent-functionalized GO sheets. The electrochemical signal with an amplified current response was attained because of the enhanced diffusion rate of ions at the interface provided by widening the pore size of the MIP film. The analytical response of GO@MIPs, validated by recording square-wave anodic stripping voltammetry (SWASV) at varying MP concentrations, followed the linear response between 0.2 and 200 ng/mL. Under optimized conditions, the sensor exhibited a limit of detection of 4.25 ng/mL with high selectivity over other interfering ions or molecules. The anti-interfering ability and good recovery (%) in food samples directed the use of the proposed sensor toward real-time monitoring and also toward future mimicking of surfaces.

Development of MOF-derived Co3O4 microspheres composed of fiber stacks for simultaneous electrochemical detection of Pb2+ and Cu2.

As an ideal transition metal oxide, Co3O4 is a P-type semiconductor with excellent electrical conductivity, non-toxicity and low cost. This work reports the successful construction of Co3O4 materials derived from metal-organic frameworks (MOFs) using a surfactant micelle template-solvothermal method. The modified electrodes are investigated for their ability to electrochemically detect Pb2+ and Cu2+ in aqueous environments. By adjusting the mass ratios of alkaline modifiers, the morphological microstructures of Co3O4-X exhibit a transition from distinctive microspheres composed of fiber stacks to rods. The results indicate that Co3O4-1(NH4F/CO(NH2)2 = 1:0) has a distinctive microsphere structure composed of stacked fibers, unlike the other two materials. Co3O4-1/GCE is used as the active material of the modified electrode, it shows the largest peak response currents to Pb2+ and Cu2+, and efficiently detects Pb2+ and Cu2+ in the aqueous environment individually and simultaneously. The linear response range of Co3O4-1/GCE for the simultaneous detection of Pb2+ and Cu2+ is 0.5-1.5 µM, with the limits of detection (LOD, S/N = 3) are 9.77 nM and 14.97 nM, respectively. The material exhibits a favorable electrochemical response, via a distinctive Co3O4-1 microsphere structure composed of stacked fibers. This structure enhances the number of active adsorption sites on the material, thereby facilitating the adsorption of heavy metal ions (HMIs). The presence of oxygen vacancies (OV) can also facilitate the adsorption of ions. The Co3O4-1/GCE electrode also exhibits excellent anti-interference ability, stability, and repeatability. This is of great practical significance for detecting Pb2+ and Cu2+ in real water samples and provides a new approach for developing high-performance metal oxide electrochemical sensors derived from MOFs.

Exploring the synchronized effect of MWCNT/X-manganate (X-Cu, Zn) nanocomposite for the sensitive and selective electrochemical detection of Hg(II) and Pb(II) in water.

The presence of heavy metal ions in the environment is a long-lasting problem that requires the simultaneous detection of Hg(II) and Pb(II) which is both vital and challenging. This present study examines a simplified and effective approach for synthesizing multi-walled carbon nanotube-copper manganese oxide (MWCNT-CuMn2O4) and multi-walled carbon nanotube-zinc manganese oxide (MWCNT-ZnMn2O4) nanocomposites for electrochemical detection of heavy metal ions. The nanocomposites MWCNT-CuMn2O4 and MWCNT-ZnMn2O4 exceptional electrochemical performance was evaluated using Square Wave Anodic Stripping Voltammetry (SWASV). The fabricated MWCNT-ZnMn2O4 demonstrated lower values of Electrochemical Impedance Spectroscopy (EIS) with charge transfer resistance (Rct) of approximately 34.13 Ω. Remarkably, the MWCNT-ZnMn2O4 electrochemical sensor exhibited the widest linear ranges of 0.5-10 µM with sensitive detection limits (0.011 µM for Hg(II) and 0.014 µM for Pb(II)). Interestingly, the MWCNT-ZnMn2O4 sensor showed excellent capability in detecting Hg(II) and Pb(II) in real water samples with a recovery percentage of 94.1% and 91.3%. Overall, the MWCNT-ZnMn2O4 modified GCE showcased superior selectivity, sensitivity, reproducibility, stability, and repeatability.

Modified Gold Screen-Printed Electrodes for the Determination of Heavy Metals.

Screen-printed electrodes (SPEs) are reliable, portable, affordable, and versatile electrochemical platforms for the real-time analytical monitoring of emerging analytes in the environmental, clinical, and agricultural fields. The aim of this study was to evaluate the electrochemical behavior of gold screen-printed electrodes (SPGEs) modified with molecules containing amino (Tr-N) or α-aminophosphonate (Tr-P) groups for the selective and sensitive detection of the toxic metal ions Pb2+ and Hg2+ in aqueous samples. After optimizing the analytical parameters (conditioning potential and time, deposition potential and time, pH and concentration of the supporting electrolyte), anodic square wave stripping voltammetry (SWASV) was used to evaluate and compare the electrochemical performance of bare or modified electrodes for the detection of Hg2+ and Pb2+, either alone or in their mixtures in the concentration range between 1 nM and 10 nM. A significative improvement in the detection ability of Pb2+ ions was recorded for the amino-functionalized gold sensor SPGE-N, while the presence of a phosphonate moiety in SPGE-P led to greater sensitivity towards Hg2+ ions. The developed sensors allow the detection of Pb2+ and Hg2+ with a limit of detection (LOD) of 0.41 nM and 35 pM, respectively, below the legal limits for these heavy metal ions in drinking water or food, while the sensitivity was 5.84 µA nM-1cm-2 and 10 µA nM-1cm-2, respectively, for Pb2+ and Hg2+. The reported results are promising for the development of advanced devices for the in situ and cost-effective monitoring of heavy metals, even in trace amounts, in water resources.

Hydrogen-bond organic-framework-based electrochemical sensor for highly sensitive determination of trace cadmium ions in environmental and e-cigarette samples.

BACKGROUND: The heavy metal ion Cd2+ is acutely toxic, and excessive concentrations can have adverse effects on human production and life, and even lead to significant public health risks and environmental impacts. There are several mature non-electrochemical methods for heavy metal detection, but these methods are characterized by high cost, which makes it difficult to be applied to the field for timely detection. Therefore, it is necessary to prepare a new electrochemical sensor that is environmentally friendly and capable of detecting Cd2+ in the environment quickly, easily and sensitively. RESULTS: In this study, hydrogen-bonded organic frameworks (HOFs) were synthesized by a simple hydrothermal reaction. The prepared materials consisted of only C, N and O and had a thin lamellar structure. The HOFs were integrated into a novel electrochemical sensor to achieve accurate detection of Cd2+ ions in real aqueous environments by square wave anodic dissolution voltammetry. The sensor has a wide linear range and a detection limit as low as 0.13 µg/L. Several real water samples, such as tap water, lake water, and e-cigarette digest, were analyzed to simulate the working environment of the sensor, and the results showed that the recoveries of Cd2+ ranged from 95.75 % to 101.2 %. SIGNIFICANCE: We pioneered the detection of heavy metal ions Cd2+ in e-cigarette digestate samples with the innovative use of HOFs as the sensor material, which demonstrated the potential application in electrochemical sensing with extremely low background current value and high sensitivity, providing new ideas for environmental monitoring and public health control.

Highly sensitive determination of trace arsenic(III) onto carbon paste electrode modified with graphitic carbon nitride decorated Fe-MOF.

An effective electrochemical sensor was developed to detect and determine of the As(III) by modifying the carbon paste electrode (CPE) with graphitic carbon nitride decorated with iron-based metal-organic frameworks (Fe-MOF/g-C3N5). The differential pulse anodic stripping voltammetry (DPASV) method was used to analyze As(III) ions in a phosphate buffer solution (0.10 M, pH = 5). Fe-MOF/g-C3N5/CPE showed high sensitivity (4.24 µA µg-1 L), satisfactory linear range (0.50 µg L-1-5.00 µg L-1 and 5.00 µg L-1-30.00 µg L-1), and low detection limit (LOD, 0.013 µg L-1). The prepared sensor was showed an excellent repeatability and selectivity, and successfully used for determination of the As(III) ion in ambient waters and apple juice samples.

Rapid determination of uracil in biological fluids at mercury thin film electrode for early detection of potential 5-fluorouracil toxicity due to dihydropyrimidine dehydrogenase deficiency.

Determination of plasma uracil was reported as a method for evaluation of Dihydropyrimidine dehydrogenase (DPD) activity that is highly demanded to ensure the safe administration of 5-fluorouracil (5-FU)-based therapies to cancer patients. This work reports the development of a simple electroanalytical method based on adsorptive stripping square wave voltammetry (AdSWV) at mercury film-coated glassy carbon electrode (MF/GCE) for the highly sensitive determination of uracil in biological fluids that can be used for diagnosis of decreased DPD activity. Due to the formation of the HgII-Uracil complex at the electrode surface, the accuracy of the measurement was not affected by the complicated matrices in biological fluids including human serum, plasma, and urine. The high sensitivity of the developed method results in a low limit of detection (≈1.3 nM) in human plasma samples, falling below the practical cut-off level of 15 ng mL-1 (≈0.14 µM). This threshold concentration is crucial for predicting 5-FU toxicity, as reported in buffer, and ≤1.15% in biological samples), and accuracy (recovery percentage close to 100%).

Effect of Temperature on the Removal of Interferences in the Voltammetric Procedure for the Determination of Cr(VI).

The aim of this paper was to investigate the effect of temperature on the removal efficiency of surfactant-induced interferences. Surfactants were removed as a result of mixing with XAD-7 resin. The study was carried out using the example of Cr(VI) determination by adsorption stripping voltammetry (AdSV). Measurements were carried out using a solution containing Cr(VI), acetate buffer (pH = 6.2), DTPA, KNO3, and different surfactants. Ten mL of the solution was mixed with 0.5 g of XAD-7 resin at different temperatures for 5 min prior to voltammetric measurement. The effect of the mixing temperature of the sample with the resin on the voltammetric Cr(VI) signal in the presence of different surfactants was studied in the range from 20 to 60 °C. The proposed method of removing interference from surfactants by mixing the sample with the XAD-7 resin at 60 °C was used for the determination of trace amounts of Cr(VI) in river water containing non-ionic, anionic, cationic surfactants, and biosurfactants.

Voltammetric co-determination of lead and copper in gunshot residue based on iron oxide particle/spent coffee grounds-modified electrode.

A novel electrochemical sensor was developed for the detection of lead (Pb) and copper (Cu) ions using spent coffee grounds decorated with iron oxide particles (FeO/SCG). The FeO-decorated SCG was used to modify a glassy carbon electrode (GCE). FeO, SCG, and FeO/SCG were characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The electrochemical properties of the modified electrode were characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrode modifications increased the active surface area and electron transfer and enhanced the accumulation of the target analyte. In the optimal condition, the developed sensor showed linear ranges of 1.0 µg L-1-0.05 mg L-1 and 0.05 mg L-1-0.8 mg L-1 for Pb2+ and 5.0 µg L-1-0.1 mg L-1 and 0.1 mg L-1-0.8 mg L-1 for Cu2+. The limit of detection (LOD) was 1.0 µg L-1 for Pb2+ and 2.4 µg L-1 for Cu2+. The developed sensor was successfully applied to determine Pb2+ and Cu2+ in bullet holes. The results were in good agreement with those obtained by inductively coupled plasma optical emission spectrometry (ICP/OES).

Anodic stripping voltammetry of arsenic determination with edible mushroom-nafion-modified glassy carbon electrode.

An edible Mushroom-Nafion modified glassy carbon electrode (M2N5-GCE) was prepared using a homogeneous mixture varying the concentrations of these, in addition to the origin of the mushroom (Shiitake, Lentinula edodes, M1 and Abrantes, Agariscus bisporus, M2) and applied to the As(III) determination by anodic stripping voltammetry. After choosing the optimal conditions in the preparation of the electrode, the second stage was to study the effects of various parameters such as supporting electrolyte, pH, accumulation potential, and time (Eacc, tacc). The optimum experimental conditions chosen were Britton Robinson buffer 0.01 mol L-1 pH:4.6; Eacc: -1.0 and tacc: 60 s obtaining a signal of oxidation of As(0) to As(III) about 0.08 V. Peak current was proportional to arsenic concentration over the 19.6-117.6 µg L-1 range, with a 3σ detection limit of 13.4 µg L-1. The method was validated using As(III) spiked tap water from the laboratory with satisfactory results (RE:3.0 %). Finally, the method was applied to the determination of As(III) in water samples from the Loa River (Northern Chile) in the presence of As(V) in a concentration >20 times higher (RE: 2.3 %).

Bismuth Film along with dsDNA-Modified Electrode Surfaces as Promising (bio)Sensors in the Analysis of Heavy Metals in Soils.

Heavy metals constitute pollutants that are particularly common in air, water, and soil. They are present in both urban and rural environments, on land, and in marine ecosystems, where they cause serious environmental problems since they do not degrade easily, remain almost unchanged for long periods, and bioaccumulate. The detection and especially the quantification of metals require a systematic process. Regular monitoring is necessary because of seasonal variations in metal levels. Consequently, there is a significant need for rapid and low-cost metal determination methods. In this study, we compare and analytically validate absorption spectrometry with a sensitive voltammetric method, which uses a bismuth film-plated electrode surface and applies stripping voltammetry. Atomic absorption spectroscopy (AAS) represents a well-established analytical technique, while the applicability of anodic stripping voltammetry (ASV) in complicated sample matrices such as soil samples is currently unknown. This sample-handling challenge is investigated in the present study. The results show that the AAS and ASV methods were satisfactorily correlated and showed that the metal concentration in soils was lower than the limit values but with an increasing trend. Therefore, continuous monitoring of metal levels in the urban complex of a city is necessary and a matter of great importance. The limits of detection of cadmium (Cd) were lower when using the stripping voltammetry (SWASV) graphite furnace technique compared with those obtained with AAS when using the graphite furnace. However, when using flame atomic absorption spectroscopy (flame-AAS), the measurements tended to overestimate the concentration of Cd compared with the values found using SWASV. This highlights the differences in sensitivity and accuracy between these analytical methods for detecting Cd. The SWASV method has the advantage of being cheaper and faster, enabling the simultaneous determination of heavy elements across the range of concentrations that these elements can occur in Mediterranean soils. Additionally, a dsDNA biosensor is suggested for the discrimination of Cu(I) along with Cu(II) based on the oxidation peak of guanine, and adenine residues can be applied in the redox speciation analysis of copper in soil, which represents an issue of great importance.

Development and Characterization of a Sol-Gel-Functionalized Glass Carbon Electrode Probe for Sensing Ultra-Trace Amounts of NH3 and NH4+ in Water.

This study centers on the development and characterization of an innovative electrochemical sensing probe composed of a sensing mesoporous functional sol-gel coating integrated onto a glassy carbon electrode (sol-gel/GCE) for the detection of NH3 and/or NH4+ in water. The main interest for integrating a functional sol-gel coating onto a GCE is to increase the selective and sensing properties of the GCE probe towards NH3 and/or NH4+ ions. The structure and surface morphology of the newly developed sol-gel/GCE probe were characterized employing scanning electron microscopy (SEM), atomic force microscopy (AFM), dynamic light scattering (DLS), and Fourier-transform infrared (FTIR), while the electrochemical sensing properties were evaluated by Berthelot's reaction, cyclic voltammetry (CV), and adsorptive square wave-anodic striping voltammetry (Ads SW-ASV). It is shown that the newly developed sol-gel coating is homogeneously deposited on the GCE with a sub-micron and uniform thickness close to 630 nm and a surface roughness of 25 nm. The sensing testing of the sol-gel/GCE probe showed limits of detection and limits of quantitation of 1.7 and 5.56 nM of NH4+, respectively, as well as a probe sensitivity of 5.74 × 10-1 µA/µM cm-2. The developed probe was fruitfully validated for the selective detection of NH3/NH4+ in fresh and sea water samples. Computed Student texp (0.45-1.25) and Fexp (1.69-1.78) (n = 5) tests were less than the theoretical ttab (2.78) and Ftab (6.39) at 95% probability.

Synthesis and application of bismuth nanoparticle-loaded longan porous carbon for simultaneous electrochemical determination of Pb(II) and cd(II) in seafoods.

The discarded longan shell-derived porous carbon material (LPC) served as a scaffold for synthesizing bismuth nanoparticle-loaded longan porous carbon nanocomposite (BiNPs@LPC) via a hydrothermal method. Then BiNPs@LPC was utilized to modify screen-printed carbon electrodes (SPCE) for simultaneous detection of Pb(II) and Cd(II) by square wave anodic stripping voltammetry (SWASV). The material was thoroughly characterized by scanning electron microscopy, X-ray diffraction, Raman spectra, Brunauer-Emmett-Teller analysis, electrochemical impedance spectroscopy and cyclic voltammetry. BiNPs@LPC exhibited abundant porous structures, high surface area, and numerous active sites, which could improve significantly response sensitivity. Under optimal conditions, the peak currents of Pb(II) and Cd(II) exhibited favorable linear relationships with the concentration within a range of 0.1-150 µg L-1, with detection limits (S/N = 3) of 0.02 µg L-1 and 0.03 µg L-1, respectively. BiNPs@LPC/SPCE demonstrated remarkable selectivity, stability and repeatability. The proposed method was successfully applied for the detection of Pb(II) and Cd(II) in seafoods achieving satisfying recovery of 97.8%-108.3% and 96.7%-106.4%. These excellent test properties were coupled with convenience for batch preparation of the modified electrodes, highlighting its potential for practical applications in heavy metal detection of real samples.

Microelectrode Voltammetric Analysis of Low Concentrations of Se(IV) Ions in Environmental Waters.

The current research is an attempt to analyze on-site selenium(IV) ions in environmental water samples using an eco-friendly miniaturized sensor developed by deposition of a very thin amount of metallic bismuth in a solid Bi electrode tightly closed in miniaturized housing. Numerous experimental variables are optimized, including the composition of the supporting electrolyte and its pH, as well as activation and accumulation conditions. Under optimized measurement conditions, the method shows high sensitivity, permitting a very low limit of detection equal to 7 × 10-10 mol L-1 to be achieved in a short accumulation time of 50 s. The performance of this microsensor was investigated against numerous interference factors and its good anti-interference capability was demonstrated. A series of voltammetric experiments by differential pulse cathodic stripping voltammetry (DPCSV) were carried out and they proved that the miniaturized sensor is characterized by very good accuracy and precision as well as long-term stability. The solid bismuth microelectrode displays a good voltammetric response in the analysis of diverse samples with a complex matrix and demonstrates a good recovery rate.

Electrochemical Detection of Cd2+, Pb2+, Cu2+ and Hg2+ with Sensors Based on Carbonaceous Nanomaterials and Fe3O4 Nanoparticles.

Two electrochemical sensors were developed in this study, with their preparations using two nanomaterials with remarkable properties, namely, carbon nanofibers (CNF) modified with Fe3O4 nanoparticles and multilayer carbon nanotubes (MWCNT) modified with Fe3O4 nanoparticles. The modified screen-printed electrodes (SPE) were thus named SPE/Fe3O4-CNF and SPE/Fe3O4-MWCNT and were used for the simultaneous detection of heavy metals (Cd2+, Pb2+, Cu2+ and Hg2+). The sensors have been spectrometrically and electrochemically characterized. The limits of detection of the SPE/Fe3O4-CNF sensor were 0.0615 µM, 0.0154 µM, 0.0320 µM and 0.0148 µM for Cd2+, Pb2+, Cu2+ and Hg2+, respectively, and 0.2719 µM, 0.3187 µM, 1.0436 µM and 0.9076 µM in the case of the SPE/ Fe3O4-MWCNT sensor (following optimization of the working parameters). Due to the modifying material, the results showed superior performance for the SPE/Fe3O4-CNF sensor, with extended linearity ranges and detection limits in the nanomolar range, compared to those of the SPE/Fe3O4-MWCNT sensor. For the quantification of heavy metal ions Cd2+, Pb2+, Cu2+ and Hg2+ with the SPE/Fe3O4-CNF sensor from real samples, the standard addition method was used because the values obtained for the recovery tests were good. The analysis of surface water samples from the Danube River has shown that the obtained values are significantly lower than the maximum limits allowed according to the quality standards specified by the United States Environmental Protection Agency (USEPA) and those of the World Health Organization (WHO). This research provides a complementary method based on electrochemical sensors for in situ monitoring of surface water quality, representing a useful tool in environmental studies.

How to overcome the difficulty in assaying Ni in biodiesel samples? Extraction induced by microemulsion breaking and square wave adsorptive stripping voltammetry could be the answer.

Herein, a simple, green, and relatively inexpensive approach to determine nickel (Ni) in biodiesel samples by square wave adsorptive cathodic stripping voltammetry (SWAdCSV) is presented. A method based on the accumulation of Ni as Ni(II)-dimethylglyoxime (Ni(II)(HDMG)2) on the glassy carbon electrode was carried out in a solution containing the aqueous phase extract (APhEx) obtained from an extraction induced by microemulsion breaking (EIMB), which was achieved by adding a few microliters of ultrapure water to a microemulsion composed of biodiesel, n-propanol and a diluted HNO3 solution. The LOD and LOQ were 0.2 µg L-1 and 0.8 µg L-1, respectively, and the accuracy was evaluated by recovery assays of spiked samples and by analyzing a standard reference material. Results obtained from a comparative method (HR-CS GF AAS) were also used for this evaluation. The method was applied to biodiesel samples produced from different feedstocks. To the best of the authors knowledge, it is the first time that: 1) Ni in biodiesel is determined by a voltammetric method; 2) EIMB is applied to extract Ni from this matrix and 3) this type of sample preparation method is used with adsorptive stripping voltammetry.

Rapid, simple, and simultaneous electrochemical determination of cadmium, copper, and lead in Baijiu using a novel covalent organic framework based nanocomposite.

It is of great significance to develop a simple and rapid electrochemical sensor for simultaneous determination of heavy metal ions (HMIs) in Baijiu by using new nanomaterials. Here, graphene (GR) was utilized to combine with covalent organic frameworks (COFs) that was synthesized via the aldehyde-amine condensation between 2, 5-dimethoxyterephthalaldehyde (DMTP) and 1, 3, 5-tris(4-aminophenyl) benzene (TAPB) to prepare a new GR/COFDPTB/GCE sensor for electrochemical sensing multiple HMIs. Compared with the glass carbon electrode (GCE), GR/GCE and COFDPTB/GCE, the developed sensor exhibited excellent electrochemical analysis ability for the simultaneous detection of Cd2+, Pb2+, and Cu2+ owing to the synergistically increased the specific surface area, the periodic porous network and plenty of effective binding sites, as well as the enhanced conductivity. Under the optimized experimental parameters, the proposed sensor showed good linearity range of 0.1-25 µM for Cd2+, and both 0.1-11 µM for Pb2+ and Cu2+ with the detection limits of Cd2+, Pb2+, and Cu2+ being 0.011 µM, 8.747 nM, and 6.373 nM, respectively. Besides, the designed sensor was successfully applied to the simultaneous detection of the three HMIs in Baijiu samples, suggesting its good practical application performance and a new method for the rapid detection of HMIs being expended.