Electroanalytical detection of heavy metals using metallophthalocyanine and silica-coated iron oxide composites

The monitoring of heavy metal ions particularly in water is important in safeguarding the environment and humans from the toxic effects these metal ions pose. This work describes the synthesis, characterization and electrocatalytic properties of silica-coated iron oxide nanoparticles (Si-NP) in the presence of cobalt or iron phthalocyanines (MPc) for heavy metal (HM) detection. TEM, XRD, XPS and VSM confirmed the successful synthesis of Si-NP with an average diameter of 12.07 nm. The electrochemical sensing properties of MPc/Si-NP-modified glassy carbon electrodes (GCE) were assessed for HM detection. Differential pulse anodic stripping voltammetry (DPASV) studies indicated detection limits that compared positively with the literature. The FePc/Si-NP composite showed the lowest detection limits (S/N?=?3) of 3.66, 11.56, 2.28, 4.54 μg L^?1 for arsenic (As), cadmium (Cd), mercury (Hg) and lead (Pb), respectively. A linear working range of 10–100 μg L^?1 was obtained for As³⁺, Hg²⁺ and Pb²⁺ ions while it was between 20 and 100 μg L^?1 for Cd²⁺ ions. Both composites displayed reproducible signals for the simultaneous detection of the HMs for ten consecutive scans. These composites offer a cheap and simplistic sensing device for HM analysis.     

Novel potentiometric sensor for the trace-level determination of Zn2+ based on a new nanographene/ion imprinted polymer composite

In this research, a new strategy for construction of a development potentiometric carbon paste Zn²⁺-ion selective electrode based on a novel nano-sensing layer is suggested. The proposed nano-sensing layer was prepared with the addition of a synthesised Zn²⁺-ion imprinted polymer nanoparticles ‘as an efficient sensing agent’ into the carbon paste matrix consisting of graphite powder, nanographene-composite ‘graphene nanosheets decorated with silver nanoparticles’ and 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide ‘ an ionic liquid ’, as the conducting binder. Under the optimised experimental conditions, the suggested nanographene-composite potentiometric sensor presented a low detection limit of 1.93 × 10^?1 μg L^?1 and a linear analytical range from 2.62 × 10^?1 to 6.54 × 10⁵ μg L^?1 with an excellent Nernstian slope of 29.80 mV decade^?1. The proposed zinc selective sensor was successfully applied for the highly sensitive determination of trace amounts of Zn²⁺ in environmental and biological samples with satisfactory results.     

Square-Wave Anodic Stripping Voltammetry (SWASV) for the Determination of Ecotoxic Metals,Using a Bismuth-Film Electrode

This article reviews the use of square wave anodic stripping voltammetry for the simultaneous determination of ecotoxic metals (Pb, Cd, Cu, and Zn) on a bismuth-film (BiFE) electrode. The BiFE was prepared in situ on a glassy-carbon electrode (GCE) from the 0.1 mol L^?1 acetate buffer solution (pH 4.5) containing 200 µg L^?1 of bismuth (III). The addition of hydrogen peroxide to the electroanalytical cell proved beneficial for the interference-free determination of Cu (II) together with zinc, lead, and cadmium, using the BiFE. The experimental variables were investigated and optimized with the view to apply this type of voltammetric sensor to real samples containing traces of these metals. The performance characteristics, such as reproducibility, decision limit (CC_a), detection capability (CC_β), sensitivity, and accuracy indicated that the method holds promise for trace Cu²⁺, Pb²⁺, Cd²⁺, and Zn²⁺ levels by employment of Hg-free GCE with SWASV. CCa, and CCβ were calculated according to the Commission Decision of 12 August 2002 (2002/657/EC). Linearity was observed in the range 20–280 µg L^?1 for zinc, 10–100 µg L^?1 for lead, 10–80 µg L^?1 for copper, and 5–50 µg L^?1 for cadmium. Using the optimized conditions, the stripping performance of the BiFE was characterized by low limits of detection (LOD). Finally, the method was successfully applied in real as well as in certified reference water samples.     

A new potentiometric sensor based on a high-performance composite for nanomolar determination of mercury (II) in environmental samples

A new potentiometric sensor for the rapid determination of Hg²⁺ based on modified carbon paste electrode consisting of room temperature ionic liquid, 1-Butyl-3-methylimidazolium hexafluorophosphate (BMIM-PF₆), multi-walled carbon nanotubes (MWCNTs), alumina nanoparticles and a synthetic macrocyclic diamide ‘7,10,13-triaza-1-thia-4,16-dioxa-6,14-dioxo-2,3;17,18-dinaphtho-cyclooctadecane’ as an efficient ionophore was constructed. Prepared composite is an ideal paste because it has low drift of potential, high selectivity and fast response time (10 s), which leads to a more stable potential signal. The morphology and properties of electrodes surface were characterised by scanning electron microscopy (SEM) and electrochemical impedance spectroscopy. A linear dynamic range of 2.01–2.01 × 10⁷ µg L^?1 with detection limit of 1.40 µg L^?1 Hg²⁺ was obtained at pH range of 2.5 to 4.5. The prepared modified electrode shows several advantages such as simple preparation method, high stability of the composite paste, high sensitivity, long-term life time (at least 13 weeks) and remarkable potentiometric reproducibility. The modified electrode was successfully applied for the accurate determination of trace amounts of Hg ²⁺ in environmental samples.     

Electrochemical determination of bisphenol A based on PHD/MWCNTs modified glassy carbon electrode

A novel electrochemical sensor for the determination of bisphenol A (BPA) was fabricated by block polyelectrolyte composite films, which composed of diblock polyelectrolyte poly (2-hydroxyethyl methacrylate)-b-poly (2-(dimethylamino) ethyl methacrylate) (PHEMA-b-PDMAEMA, noted as PHD in the later content) and multi-walled carbon nanotubes (MWCNTs). The tertiary amino groups of PDMAEMA can be protonated at physiological pH. The protonated PDMAEMA can thus interact with the negatively charged BPA through electrostatic attraction to increase the BPA sorption capacity and enhance the ability for highly sensitive detection of BPA. The PHD/MWCNTs composite films combine the electrocatalytic property of MWCNTs and the electrostatic attraction of protonated PHD. Because of the above-mentioned excellent property of the composite films, the PHD/MWCNTs/glassy carbon electrode exhibited good electrocatalytic activity to electrooxidation of BPA. The wide linear response range of the BPA sensor was from 4.56 × 10^?5 g L^?1 to 2.28 × 10^?2 g L^?1 with a lower detection limit of 2.28 × 10^?6 g L^?1 (S/N = 3) and high sensitivity 2442.86 μA L g^?1 cm^?2. The current reached the steady-state current with a shorter response time less than 4 s. The proposed method was successfully applied to determine BPA in real samples (PVC food package, milk, tap water and pond water) and satisfactory results were obtained. These results indicated that the block polyelectrolyte composite have potential applicability of the BPA sensor.     

Enhanced electrochemiluminescence of luminol at the gold nanoparticle/carbon nanotube/electropolymerised molecular imprinting composite membrane interface for selective recognition of triazophos

This paper reports a surface molecular self-assembly strategy for imprinting triazophos in the electropolymerised poly(aminthiophenol) (PATP) membranes at the surface of gold nanoparticle (AuNP)/carbon nanotube (CNT) composites modified glassy (GC) electrode for electrochemiluminescent (ECL) detection of pesticide triazophos. The electrochemical and ECL behaviours of luminol at the imprinted PATP/AuNP/CNT/GC electrode were investigated before and after the rebinding of triazophos. It was also found that the ECL intensity was strikingly enhanced by the adsorbed triazophos molecules in the imprinted PATP/AuNP/CNT composite membranes, which was about 5.2-fold as compared with the blank ECL intensity. On this basis, the molecularly imprinted polymer (MIP)-ECL sensor is established for high sensitive and selective detection of triazophos residues in vegetable samples. The resulting MIP-ECL sensor shows wide linear ranges from 3.1 × 10^?8 to 3.1 × 10^?5 g L^?1 with lower detection limit of 3.1 × 10^?9 g L^?1 for triazophos. Moreover, the MIP-ECL sensor has the advantages of high sensitivity, speed, specificity, stability and can become a promising technique for organophosphate pesticide detection.     

A novel electrochemical sensor based on gold nanorods and Nafion-modified GCE for the electrocatalytic oxidation of nitrite

The high-quality CTAB-stabilized gold nanorods (Au NRs) were prepared by the way of seed-mediated protocol. The microstructure and composition of the Au NRs were identified by transmission electron microscopy, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy and UV–visible spectroscopy. Further, a novel non-enzymatic electrochemical sensor of nitrite based on Au NRs–Nafion-modified glassy carbon electrode (GCE) was successfully developed. Under the optimum experimental conditions, the electrochemical behaviors of nitrite on the Au NRs–Nafion-modified GCE were systematically studied by electrochemical impedance spectroscopy, cyclic voltammetry and chronoamperometry. The electrochemical investigations indicated that the Au NRs–Nafion-modified GCE had a wide linear range of 3.0 × 10^?6–6.0 × 10^?3 mol L^?1, an acceptable sensitivity of 130.9 ± 0.05 μA mM^?1 cm^?2, a fast response time of 3 s and a low detection limit of 0.64 ± 0.02 μmol L^?1 at the signal-to-noise ratio of 3 (S/N = 3). Additionally, the electrochemical sensor also showed good stability and favorable anti-interference capability for the detection of nitrite.     

Determination of Active Ingredients of Origanum Vulgare L. and Its Medicinal Preparations by Capillary Electrophoresis with Electrochemical Detection

Abstract

A method based on capillary electrophoresis with electrochemical detection (CE‐ED) has been developed for the first time for the separation and determination of isovanillic acid, vanillic acid, quercetin, rosmarinic acid, caffeic acid, and protocatechuic acid in Origanum vulgare L. and its medicinal preparations. The effects of working electrode potential, pH level, concentration of running buffer, separation voltage, and injection time on CE‐ED were investigated. Under the optimum conditions, the analytes could be separated in a 50 mmol L^?1 borate buffer (pH 8.7) within 21 min. A 300‐µm diameter carbon disk electrode has a good response at +0.95 V (vs. SCE) for all analytes. The response was linear over three orders of magnitude with detection limits (S/N=3) ranging from 4×10^?8 g mL^?1 to 2×10^?7 g mL^?1 for the analytes. The method has been successfully applied to the analysis of real sample, with satisfactory results.     

Fabrication of a nanostructured TiO2/carbon nanotube composite electrode for voltammetric and impedimetric determination of NTO explosive in the water and soil samples

An electrochemical oxidation route was developed for sensitive and selective assay of nitrotriazolone (NTO) explosive in some environmental samples on a multi-walled carbon nanotube (MWCNTs)/TiO₂ nanocomposite paste electrode, for prevention of the analytical interference of conventional reducible energetic compounds. Detailed evaluations were made for the electrochemical behaviour of NTO on the modified electrode by adsorptive stripping voltammetry, electrochemical impedance spectroscopy (EIS) and chronoamperometry techniques in the pH range of 2.0–10.0. Parameters such as diffusion coefficient constant of NTO were calculated, and various experimental conditions were also optimised. Under optimal conditions the calibration curve had two linear dynamic ranges of 130.0–3251.5 μg L^?1 and 6.5–26.0 mg L^?1 with a detection limit of 26.0 μg L^?1 (0.2 μmol L^?1) and precision of <3%. This electrochemical sensor was further applied to determine NTO in real soil and water samples with satisfactory results.     

Optimized solid phase extraction based on diethyldithiocarbamate-coated Fe3O4 magnetic nanoparticles followed by ICP-OES for determination of Cd(II) and Ni(II) in rice and water samples

In the present study, application of Fe₃O₄ magnetic nanoparticles (MNPs) coated with diethyldithiocarbamate as a solid-phase sorbent for extraction of trace amounts of cadmium (Cd²⁺) and nickel (Ni²⁺) ions by the aid of ultrasound was investigated. The analytes were determined by inductively coupled plasma-optical emission spectroscopy. Fe₃O₄ MNPs were prepared by solvothermal method and characterized with dynamic light scattering, scanning electron microscope and X-ray diffraction. Response surface methodology was used for optimization of the extraction process and modeling the data. The optimal conditions obtained were as follows: chelating agent, 1.2 g L^?1; pH, 6.13; sonication time, 13 min and Fe₃O₄ MNPs, 10.3 mg. The calibration curves were linear over the concentration range of 1–1,000 μg L^?1 for Cd²⁺ and 2.5–1,000 for Ni²⁺ with the determination coefficients (R ²) of 0.9997 and 0.9995, respectively. The limits of detection were 0.27 μg L^?1 for Cd²⁺ and 0.76 μg L^?1 for Ni²⁺. The relative standard deviations (n = 7, C = 200 μg L^?1) for determination of Cd²⁺ and Ni²⁺ were 2.0 and 2.7 %, respectively. The relative recoveries of the analytes from tap, river and lagoon waters and rice samples at the spiking level of 10 μg L^?1 were obtained in the range of 95–105 %.     

A new nano-composite electrode as a copper (II) selective potentiometric sensor

A macrocyclic ligand “7,10,13-triaza-1-thia-4,16-dioxa-20,24-dimethyl-2,3;17,18-dibenzo-cyclooctadecane-6,14-dione” as an efficient ionophore was used into a new Cu²⁺ nano-composite potentiometric carbon paste sensor containing multi-walled carbon nanotubes (MWCNTs), nanosilica particles, and room temperature ionic liquid (1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide, [BMP]Tf₂N). This potentiometric sensor responds to copper ions in a wide linear dynamic range of 4.50 × 10^?8 to 1.00 × 10^?2 mol L^?1 with Nernstian slope of 29.64 ± 0.10 mV per decade. The detection limit of 2.34 × 10^?8 mol L^?1 was obtained at the pH range 3.5–6.0. It has a fast response with response time of about 10 s, and can be used for at least 16 weeks without any considerable divergence in the potentials. The suggested sensor thus allows sensitive, selective, simple, low cost, and stable electrochemical sensing of Cu²⁺ ions in the presence of a large number of alkali, alkaline earth, transition and heavy metal ions. This sensor was successfully applied in the determination of copper ions in water and waste water samples.     

Use of ionic liquid based chitosan as sorbent for preconcentration of fluoroquinolones in milk,egg, fish,bovine, and chicken meat samples by solid phase extraction prior to HPLC determination

The possibility of using ionic liquid based chitosan sorbent for the separation and preconcentration of fluoroquinolone antibiotics (marbofloxacin, enoxacin, ofloxacin, ciprofloxacin, and enrofloxacin) has been studied. For this reason, different ionic liquids were prepared and coated on the chitosan sorbent. The conditions of the preconcentration of fluoroquinolones on a microcolumn have been optimized and the extraction efficiencies of the prepared sorbents have been compared. The compounds were eluted with 5 mL of 20% NH₃ (v/v, MeOH) solution and determined by HPLC with diode array and fluorescence detector. The limits of detection were found as 4.23 µ g L^?1 for marbofloxacin, and 1.09 µg L^?1 for enoxacin; 3.23 × 10^?3 µg L^?1 for ofloxacin; 8.39 × 10^?3 µg L^?1 for ciprofloxacin; and 19.50 × 10^?3 µg L^?1 for enrofloxacin. The developed method was applied for the analysis of fluoroquinolone in milk, egg, fish, bovine, and chicken samples and the recoveries were obtained in the range 70–100%.     

Electrochemical Enzyme‐Linked Immunoassay for the Determination of Estriol Using Methyl Red as Substrate

Abstract

A new electrochemical substrate for horseradish peroxidase, methyl red, is reported. In this reaction system, horseradish peroxidase can catalyze the redox reaction of methyl red and H₂O₂. Methyl red exhibits a sensitive voltammetric peak at?0.51 V vs. Ag/AgCl reference electrode, the decrease of the peak current of methyl red is in proportion to the concentration of horseradish peroxidase (HRP). The linear range for determination of horseradish peroxidase is 5.0×10^?8～5.0×10^?7 g mL^?1 and the detection limit is 1.8×10^?8 g mL^?1. The relative standard deviation is 3.3% when 2.0×10^?7 g mL^?1 HRP was sequentially determined 11 times. A voltammetric enzyme‐linked immunoassay method for the determination of estriol was developed, based on this electrochemical system. The linear range for determination of estriol is 1.0～1000.0 ng mL^?1, and the detection limit is 0.33 ng mL^?1. The relative standard deviation for 11 parallel determinations with 200 ng mL^?1 estriol is 4.8%. Some pregnancy serum samples were analyzed with satisfactory results.     

Analysis of Aromatic Amines in Surface Waters Receiving Wastewater from a Textile Industry by Liquid Chromatographic with Electrochemical Detection

Abstract

A high performance liquid chromatography (HPLC) method with electrochemical detection (ED) was developed for the determination of benzidine, 3,3‐dimethylbenzidine, o‐toluidine and 3,3‐dichlorobenzidine in the wastewater of the textile industry. The aromatic amines were eluted on a reversed phase column Shimadzu Shimpack C₁₈ using acetonitrile+ammonium acetate (1×10^?4 mol L^?1) at a ratio 46:54 v/v as mobile phase, pumped at a flow rate of 1.0 mL min^?1. The electrochemical oxidation of the aromatic amines exhibits well‐defined peaks at a potential range of +0.45 to +0.78 V on a glassy carbon electrode. Optimum working potentials for amperometric detection were from 0.70 V to +1.0 V vs. Ag/AgCl. Analytical curves for all the aromatic amines studied using the best experimental conditions present linear relationship from 1×10^?8 mol L^?1 to 1.5×10^?5 mol L^?1, r=0.99965, n=15. Detection limits of 4.5 nM (benzidine), 1.94 nM (o‐toluidine), 7.69 nM (3,3‐dimethylbenzidine), and 5.15 nM (3,3‐dichlorobenzidine) were achieved, respectively. The detection limits were around 10 times lower than that verified for HPLC with ultra violet detection. The applicability of the method was demonstrated by the determination of benzidine in wastewater from the textile industry dealing with an azo dye processing plant.     

Stripping voltammetric determination of mercury(II) and lead(II) using screen-printed electrodes modified with gold films, and metal ion preconcentration with thiol-modified magnetic particles

A novel approach to the electrochemical determination of heavy metals in tap water using anodic stripping voltammetry was developed using screen-printed electrodes modified with gold films. After optimisation of the experimental conditions, the screen-printed electrodes modified with gold films displayed excellent linear behaviour in the examined concentration range from 2 to 16 µg L^-1 mercury and lead in 50 mM HCl with a detection limit of 1.5 µg L^-1 and 0.5 µg L^-1 for mercury and lead, respectively. In order to decrease the working range down to less than 1 µg L^-1, a preconcentration step based on the use of magnetic particles modified with thiols was introduced into the protocol. Applying optimum binding conditions, the assay using screen-printed electrodes modified with gold films displayed excellent linear behaviour in the concentration range 0.1 to 0.8 µg L^-1 in 50 mM HCl. The detection limit after a 120 s deposition time for mercury and lead were 0.08 µg L^-1 and 0.02 µg L^-1, respectively. The method has been applied to the determination of mercury and lead traces in tap water     

Simple and fast voltammetric procedure of U(VI) determination in the presence of high concentrations of surface active substances

In this work, a simple and fast procedure for elimination of interfering surface active substances and for U(VI) adsorptive stripping voltammetric determination was developed. The adsorption in the form of U(VI)-cupferron complexes was performed, because as it was proved before, U(VI) forms with cupferron stable complexes, which were employed in voltammetric procedures. The procedure is based on two steps: the first is an adsorption of surface active substances onto an Amberlite XAD-16 or XAD-7 resin and the second is a voltammetric determination of U(VI) with a pulsed potential of accumulation alternate –0.65–0.3 V with the frequency of 0.5 Hz and then the differential pulse voltammogram was recorded, whereas the potential was scanned from –0.65 to –1.2 V. The detection limit estimated from three times the standard deviation for a low U(VI) concentrations was equal to 1.7 × 10^?10 mol L^?1 (7.2 × 10^?8 g L^?1). The linear range of U(VI) was observed over the concentration range from 5.0 × 10^?10 mol L^?1 (2.1 × 10^?7 g L^?1) to 2.0 × 10^?8 mol L^?1 (8.5 × 10^?6 g L^?1) for an accumulation time of 60 s. The influence of different kinds of surfactants, such as non-ionic, cationic and anionic on the uranium voltammetric signal was studied. The results confirm the possibility of U(VI) determination in water samples containing high concentrations of surface active substances even up to 50 mg L^?1.     

A sensitive amperometric sensor for hydrazine based on Pt nanoparticles-reduced graphene oxide–multi-walled carbon nanotubes composite

The platinum nanoparticles-reduced graphene oxide-multi-walled carbon nanotubes composite (PtNPs-rGO-MWCNTs) has been synthesised by one-step chemical co-reduction strategy in ethylene glycol (EG) system using sodium citrate as reducing agent. The X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), as well as the electrochemical methods have been used for the characterisation of this composite. Benefiting from the large effective surface and good carrier function of rGO-MWCNTs, PtNPs in this nanocomposite have some excellent characteristics such as small particle size, good dispersion, as well as high electrocatalytic activity. Based on this, a new electrochemical sensor for hydrazine has been fabricated using dropping method. Under the optimum conditions, the linear range for the determination of hydrazine by amperometry at 0.20 V (vs. SCE) in phosphate buffer (pH 7.0) is from 2.0 × 10^?7 mol L^?1 to 2.3 × 10^?3 mol L^?1. The detection limit and sensitivity is 4.5 × 10^?8 mol L^?1 (S/N = 3) and 219.7 μA mM^?1, respectively. This sensor has some attractive analytical features such as low detection limit, wide linear range, high sensitivity, as well as good stability.     

Simultaneous determination of dopamine and serotonin by use of covalent modification of 5-hydroxytryptophan on glassy carbon electrode

An electrochemical biosensor was fabricated by covalent modification of 5-hydroxytryptophan (5-HTP) on the surface of glassy carbon electrode (GCE). The electrode, denoted as 5-HTP/GCE, was characterized by X-ray photoelectron spectroscopy, cyclic voltammetry and differential pulse voltammetry. For comparison, tryptophan modified GCE (TRP/GCE) and serotonin modified GCE (5-HT/GCE) were prepared by the same method. It was found that electrocatalytic ability of these electrodes was in the order of 5-HTP/GCE?>?TRP/GCE?>?5-HT/GCE for the oxidation of dopamine (DA) and 5-HT. The sensor was effective to simultaneously determine DA and 5-HT in a mixture. It can resolve the overlapping anodic peaks into two well-defined voltammetric peaks at 0.24 and 0.39 V (versus SCE). The linear response is in the range of 5.0?×?10^?7–3.5?×?10^?5 mol L^?1 with a detection limit of 3.1?×?10^?7 mol L^?1 for DA, and in the range of 5.0?×?10^?6–3.5?×?10^?5 mol L^?1 with a detection limit of 1.7?×?10^?6 mol L^?1 for 5-HT (s/n?=?3), respectively.     

A new calix[4]arene Schiff base sensor for Hg<Superscript>2+</Superscript> and Au<Superscript>3+</Superscript>

This article reports the selective sensing ability of a newly synthesized calix[4]arene Schiff base (C4TSB) derivative. C4TSB exhibited strong turn-off fluorescence affinity for Hg²⁺ and Au³⁺. The selective sensing ability of receptor was investigated in the presence of different co-existing competing ions. The limit of detection for Hg²⁺ and Au³⁺ was determined as 1.9 × 10^?5 and 1.0 × 10^?6 M, respectively. Receptor forms 1:1 stoichiometric complex with both metals and their binding constants were calculated as 7.9 × 10³ M^?1 for Hg²⁺ and 5.7 × 10³ M^?1 for Au³⁺. Complexes were also characterized through FT-IR spectroscopy.     

Ion Chromatography with Post-column Reaction and Serial Conductivity and Spectrophotometric Detection Method Development for Quantification of Transition Metal Dissolution in Lithium Ion Battery Electrolytes

We present a method for the separation and determination of transition metals in electrolytes based on ion chromatography (IC) with post-column reaction (PCR) and serial conductivity and spectrophotometric detection. Three IC columns [Metrosep C4—250/4.0 (column A), Metrosep C6—250/4.0 (column B), and Nucleosil 100-5SA—250/4.6 (column C)] with different capacities, and stationary phases were used and compared with each other for method development. All spectrophotometric measurements were carried out with 4-(2-pyridylazo)resorcinol (PAR) as PCR reagent at a wavelength of 500 nm. To characterize the precision of the separation, the selectivity for the analysis of transition metals (nickel, cobalt, copper, and manganese) in the presence of large amounts of lithium and the resolution of the peaks were determined and compared with one another. Furthermore, the limits of detection (LOD) and quantification (LOQ) were determined for the transition metals. The LODs and LOQs determined by column C were as follows: cobalt (LOD/LOQ): 9.4 µg L^?1/31.3 µg L^?1, manganese (LOD/LOQ): 7.0 µg L^?1/23.5 µg L^?1, and nickel (LOD/LOQ): 6.3 µg L^?1/21.1 µg L^?1. Finally, the concentration of transition metal dissolution of the cathode material Li₁Ni_1/3Co_1/3Mn_1/3O₂ (NCM) was investigated for different charge cut-off voltages by the developed IC method.