Recent Trends in Electrochemical Methods for Real-Time Detection of Heavy Metals in Water and Soil: A Review

Pythagore L Kyabutwa; Nadiah Alyamni; Jandro L Abot; Alexander G Zestos

doi:10.1016/j.coelec.2025.101749

. Author manuscript; available in PMC: 2026 Aug 26.

Published in final edited form as: Curr Opin Electrochem. 2025 Aug 26;54:101749. doi: 10.1016/j.coelec.2025.101749

Recent Trends in Electrochemical Methods for Real-Time Detection of Heavy Metals in Water and Soil: A Review

Pythagore L Kyabutwa ^1,³, Nadiah Alyamni ^2,³, Jandro L Abot ¹, Alexander G Zestos ^3*

PMCID: PMC12453067 NIHMSID: NIHMS2108099 PMID: 40989831

Abstract

Heavy trace elements (HTEs), including toxic metals such as Pb, Hg, Cd, and As, present a growing environmental and public health concern due to their persistence and bioaccumulation in water and soil systems. Driven by increased demand for strategic and rare earth metals in emerging technologies, anthropogenic activities such as mining, industrial discharge, and agriculture have intensified environmental contamination. Traditional detection methods such as atomic absorption spectroscopy (AAS), inductively coupled plasma-mass spectrometry (ICP-MS), and X-ray fluorescence (XRFS), although highly sensitive, are limited by their cost, complexity, and lack of suitability for continuous measurement (real-time) without taking samples to the laboratory for analysis (in situ and online) applications. This review highlights recent advances in standard electrochemical techniques, particularly voltammetric ones such as square wave voltammetry (SWV), differential pulse voltammetry (DPV), and anodic stripping voltammetry (ASV), in addition to non-voltammetric including electrochemical impedance spectroscopy (EIS) and chronopotentiometry methods enhanced by nanomaterials, including carbon nanomaterials: single-walled carbon nanotubes (SWCNTs) and multi-walled carbon nanotubes (MWCNTs); metal and metal oxide nanoparticles; polymer and hybrid nanocomposites; and metal organic frameworks. These materials improve sensor sensitivity, selectivity, stability, and portability of standard electrochemical methods, making them ideal for real-time and in situ and online for HTEs. In this review article, current innovations in standard electrochemical techniques with nanomaterials and hybrid nanocomposites improving sensor architecture, functionalization, sensitivity and selectivity are discussed alongside performance metrics and limitations.

Keywords: Electrochemistry, Heavy Metals, Detection, Nanomaterials, Carbon Nanotube

Introduction

Trace elements (TEs) such as lithium (Li), cobalt (Co), and rare earth elements (REEs) are essential for key industrial sectors including electronics, renewable energy, and manufacturing. As the global energy transition advances, strategic elements like Li, Co, thorium (Th), and uranium (U) have become indispensable in energy storage and nuclear power technologies [1, 2]. This shift has led to a dramatic increase in exploration and exploitation of mineral deposits. However, these activities have resulted in the widespread environmental release of heavy trace elements (HTEs) such as chromium (Cr), lead (Pb), and mercury (Hg), as well as radioactive contaminants. These toxic elements are non-degradable, bioaccumulative, and often carcinogenic, posing a significant threat to both ecosystems and public health [3, 4]. Contamination of groundwater, river systems, and agricultural soils is largely driven by anthropogenic activities, including mining, industrial emissions, intensive agriculture, and rapid urbanization [5].

The growing concern over HTE pollution has drawn attention from major international institutions like the World Health Organization (WHO), the Food and Agriculture Organization (FAO), the Centers for Disease Control and Prevention (CDC), and the International Agency for Research on Cancer (IARC). These organizations have emphasized the necessity of monitoring HTE concentrations in environmental media to ensure ecosystem and human health protection [3, 6–9]. Traditional analytical methods such as inductively coupled plasma (ICP), X-ray fluorescence spectroscopy (XRFS), and atomic absorption spectroscopy (AAS) provide high sensitivity and precision for detecting low concentrations of HTEs in environmental samples with different matrices [3,10–15]. However, their applications are typically limited to well-equipped laboratories due to their high cost, labor-intensive processes, large instrumentation, and the requirement for skilled personnel. These limitations hinder continuous measurement (real-time) without taking a sample to the laboratory for analysis (in situ and online), HTE detection in water and soil, and field-scale deployment.

To overcome these problems, the scientific community has turned to electrochemical sensing technologies as a promising alternative. These approaches are characterized by their simplicity, portability, cost-effectiveness, and suitability for in situ and online monitoring [11–14]. In particular, the use of nanomaterials such as single-walled carbon nanotubes (SWCNTs), multi-walled carbon nanotubes (MWCNTs), graphene and its derivatives, metal and metal oxide nanoparticles, polymer and hybrid nanocomposites, and metal-organic frameworks has significantly improved the sensitivity and selectivity of electrochemical sensors [11–20]. Despite these advances, the electrochemical techniques used for monitoring HTEs in water and soil matrixes are still showing multiple challenges. Electrochemical sensors can suffer from limited electrode surface area and robustness, fouling due to matrix complexity, variability in environmental conditions (pH, ionic strength), and the absence of standardized calibration and validation protocols [21–22]. These limitations can affect reproducibility and limit long-term application in diverse field conditions. This review aims to examine the recent developments in electrochemical detection of HTEs using nanomaterials, with a particular focus on real-time applications in water and soil environments. Unlike traditional technique-centered reviews, this study emphasizes the classification of nanomaterials, their functional performance, and the specific challenges associated with soil and water matrices. The goal of this review is to guide future developments in designing robust, field-deployable sensors for environmental monitoring.

1. Brief Overview of Electrochemical Methods for Detection of Heavy Trace Elements in Soil and Water Matrices

Heavy trace elements (HTEs) such as Pb²⁺, Cd²⁺, Hg²⁺, As³⁺, Cr³⁺, Cu²⁺, Co²⁺, and Zn²⁺ have become significant environmental pollutants due to industrial development, mining prospection, energy transition, and modern agricultural practices. These pollutants accumulate in water and soil systems, ultimately entering the human food chain and causing toxic effects such as kidney damage, respiratory failure, neurological disorders, and cancer. To mitigate these risks, environmental agencies and governments have imposed stringent regulations on permissible levels of HTEs in the environment [1–5, 21–26]. Traditionally, quantification of HTEs relied on analytical techniques such as AAS, XRFS, XRD, and ICP-MS [10–15, 27–30]. While these methods offer high precision, they are costly, complex, and unsuitable for in-field deployment, especially in remote or resource-limited settings. Additionally, soil matrices often require complex sample pretreatment such as acid digestion due to the presence of organic matter, variable pH, and ion strength [20–22, 31–43].

To address the limitations of conventional methods, electrochemical techniques have emerged as powerful alternatives for in situ and real-time detection of HTEs in water and soils. These methods offer rapid analysis, high sensitivity, low cost, and the potential for portable sensor integration. However, the analytical approach often differs between soil and water samples due to the complexity and nature of the matrices [20–22, 31]. In water, detection generally involves simple filtration and pH adjustment before analysis. However, soil matrices require digestion with acids such as nitric acid (HNO₃) or chelating agents like ethylenediaminetetraacetic acid (EDTA) to extract metal ions prior to electrochemical detection [31,44–45]. Recently, standard electrochemical detection techniques enhanced by functionalized nanomaterials, such as voltammetric techniques (square wave voltammetry (SWV), differential pulse voltammetry (DPV), and anodic stripping voltammetry (ASV)) and non-voltammetric methods (chronopotentiometry and electrochemical impedance spectroscopy (EIS)), have shown multiple advancements, making them suitable for real-time detection of HTEs [41,47–51].

These enhanced electrochemical techniques do not rely on chemical reactivity alone, enabling broader analyte coverage and multiplexed analysis in environmental samples [52–53]. Chromatographic techniques, such as gas chromatography (GC) and high-performance liquid chromatography (HPLC), combined with diverse detection systems (microwave-induced plasma atomic emission spectroscopy, MIP-AES), offer powerful separation and quantification capabilities, especially for complex metal species in environmental matrices [40–42]. However, these methods often rely on chemical derivatization or specific reactivity for target detection. In contrast, electrochemical techniques such as voltammetry and potentiometry exploit intrinsic physicochemical properties of analytes (redox behavior, ion activity), allowing for broader analyte coverage and the possibility of multiplexed analysis without extensive sample preparation [32–36]. Table 1 provides an overview of electrochemical methods developed in the past three years for detecting HTEs in water, highlighting their detection ranges, sensitivity, selectivity, and recovery.

Table 1.

Enhanced voltammetric electrochemical methods for detection of heavy traces elements in water.

HTEs	Materials	Methods	Linear range	Limit of Detection	Temporal resolution and Selectivity	Stability	References
Pb²⁺	Carbon nanotube (CNT)/H₂pyrabza (ligand)/Proton Induced Gamma Emission (PIGE)	Square Wave Anodic Stripping Voltammetry (SWASV)	3.3–66 nM	1.1 nM	Remarkable sensitivity for simultaneous detection of Pb²⁺ and Hg²⁺	21days	[19]
	Higher density-CNTs rods microelectrode	SWASV	0.48–144.6 nM	0.45 nM	Wide detection range of Cu²⁺, Cd²⁺, and Pb²⁺ ions	15 days	[23,26]
	EDTA_Polyaniline (PANI)/SWCNT/Stainless Steel (SS)	Differential pulse voltammetry (DPV)	2–37 ϻM	1.65 ϻM	Excellent electrochemical sensing and selectivity performance for Cu²⁺, Hg²⁺		[24,42]
	MWCNTs-Polymer of Carbon Fluoride (POCF)/(PIGE)	Differential Pulse Adsorptive Stripping Voltammetry (DPASV)	16.65–1,153 nM	4.73 nM	Used for simultaneous detection of Cd²⁺, and Pb²⁺. Excellent selectivity	15 days	[25]
	Iron oxide 3 (Fe₃O₄)/Functionalized multi walled carbon nanotube (F-MWCNTs)/Glassy Carbon Electrode (GCE)	SWASV	0.5–30.0 ϻM	0.08 nM	Synergetic interaction between Fe₃O₄ and F-MWCNTs	30 days	[42]
	MWCNT-Beta-Cyclodextrin (βCD)/Screen-Printed Electrode (SPE)	DPASV	14.96–498.52 nM	4.34nM	Selective detection of Pb²⁺		[14,26,33–36]
	Ion-Implanted Polymer (IIP)/(MWCNT)/Carbon Paste Electrode (CPE)	Square wave voltammetry (SWV)	0.01–80 nM	0.0038 nM	Sensor effective in determining Pb²⁺ levels		[14]
	Bismuth-Copper (BiCu)-Nanoparticles (ANPs)	(SWASV)	0.5–100 ppb	0.081 ppb	Used for real-time detection of Pb²⁺, Cd²⁺.		[27,38]
Hg²⁺	CNT/H2pyrabza (ligand)/PIGE	SWASV	3.3–66 nM	0.36 nM	This electrode is an alternative to hanging mercury drop electrodes (HMDEs). Providing higher sensitivity and selectivity to Hg2+	21 days	[19]
	EDTA_PANI/SWCNTs/Stainless Steel (SS)	Differential pulse voltammetry (DPV)	2 ϻM - 2 mM	0.68 ϻM	No significant interference observed in presence of Mn²⁺, Cu²⁺, Fe³⁺, and Fe²⁺		[23,42]
	Mercury 2 imprinted polymethyl thiobenzoate (Hg^2+-PMBT)/Gold Nanoparticles (AuNPs)/SWCNTs/GCE	DPASV	0.4–96.0 nM	0.08 nM	Excellent selectivity in presence of 100-fold molar excess of Pb²⁺, Zn²⁺, and Cu²⁺	30 days	[20,27]
	Fe₃O₄/F-MWCNTs)/GCE	SWASV	0.5–20.0 ϻM	0.05 nM	Simultaneous detection of Zn²⁺, Cd²⁺, and Pb²⁺ ions in real tap water samples	30 days	[24,42]
	Gold or Molybdenum disulfide (Au/MoS2)-MWCNT/GCE	DPV	0.1 nM-1ϻM	0.05 nM	Excellent sensitivity for Hg²⁺	30 days	[27,28]
	MWCNTs-Polymer of Carbon Fluoride (POCF)/PIGE	DPASV	32.41-736.77nM	9.47nM	Measurement of Cd²⁺ and Pb²⁺ions	15 days	[26,33–35]
	Fe₃O₄/F-MWCNTs/GCE	SWASV	0.5–30.0 ϻM	0.05 nM	Simultaneous detection of Zn²⁺, Cd²⁺, and Pb²⁺ ions	30 days	[42]
Cu²⁺	EDTA_PANI/SWCNTs/Stainless Steel (SS)	DPV	1.2 ϻM-2 mM	0.08 ϻM	No interference in presence of Mn²⁺ and other metals		[23,42]
	Fe₃O₄/F-MWCNTs/GCE	SWASV	0.5–30.0 ϻM	0.02 nM	Simultaneous detection of Zn²⁺, Cd²⁺, and Pb²⁺ ions	30 days	[30–32]
As³⁺	F-MMWCNTs	SWASV	3.3–6.6 nM	20.02nM	Detection of As³⁺ with a LOD of 20.nM		[52]

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On the other hand, emerging technologies, including nanomaterial-based sensors and microfluidic platforms, further enhance sensitivity, selectivity, and field deployability for HTEs detection. These innovations enable rapid, on-site monitoring, facilitating timely assessments of environmental and health risks. Additionally, recent advances in chemometrics and machine learning have become instrumental in handling complex datasets, enabling more accurate calibration, pattern recognition, and multivariate analysis, thereby improving the overall reliability and precision of HTEs analyses [10–13]. Compared to the monitoring of pollution due to HTEs in soil matrices, applying the electrochemical technique for detection of HTEs in water environments is more straightforward due to the homogenous and dilute nature of the sample [45–49]. Modified and functionalized electrodes such as gold nanoparticles (AuNPs), reduced graphene oxide (rGO), or screen-printed carbon electrodes (SPCEs) have shown excellent results in detecting various HTEs like Fe³⁺, Hg²⁺, Cd²⁺, and Zn²⁺ with low detection limits and high recovery rates [20–26, 31–37, 40, 51]. Moreover, the heterogeneous nature and complexity of soil sample analysis require more rigorous preparation [21, 22, 31]. Recent studies have shown that modified electrodes using Bi-based nanomaterials, carbon nanomaterials, metal oxide nanomaterials, and polymer-metal hybrids have achieved high selectivity and sensitivity in detecting Pb²⁺, As³⁺, and Hg²⁺ in pretreated soil samples [28,38–41,43–46]. Table 2 compares electrochemical methods applied to water and soil, summarizing detectable elements, strengths, limitations, and references.

Table 2:

Comparison of between electrochemical methods used for detecting heavy traces elements in water and soils

Method	Detectable element in water	Detectable Element in soils	Advantages	Disadvantages	References
Square Wave Anodic Stripping Voltammetry (SWASV) and Cyclic voltammetry (CV)	Easily detects (Pb²⁺, Cd²⁺, Zn²⁺, Cu²⁺, Ni²⁺, As³⁺ and Hg²⁺) in water samples with a detection limit range of (0.01–80 nM)	Can detect (Pb²⁺, Cd²⁺, Zn²⁺, Cu²⁺, Ni²⁺ and As³⁺) and can shows interference with organics matrix	The technique shows high sensitivity and low limit of detection, very rapid temporal resolution, and a good signal to noise ratio with possible multiplexing in detection of HTEs in water and soils	Matrix effects from organics in soil requires sample pretreatment and electrode surface must be clean for each test (require too much time)	[21,24]
Differential Pulse voltammetry (DPV)	Easily detects (Pb²⁺, Cd²⁺, Zn²⁺, Cu²⁺, As³⁺, and Hg²⁺) in water sample with a detection limit range of (0.1 nM-1ϻM)	Aids in detection of (Pb²⁺, Cd²⁺, Zn²⁺, Cu²⁺ and As³⁺) in soils samples with a selectivity value of 0.08 ϻM	High-resolution time and it is very manageable and good for detecting (0.1 nM) trace concertation and speciation studies. It is also showing a higher selectivity (0.08 ϻM) which make it suitable and applicable in complex matrices	Use for soil samples requires more time consuming than SWV technique and it is very sensitive to electrode surface conditions	[22]
Anodic stripping voltammetry (ASV)	Aids in detection of (Pb²⁺, Cd²⁺, Zn²⁺, Cu²⁺, Hg²⁺, Tl³⁺, Bi³⁺ and Ni²⁺) with a detection limit of (0.1nM-0.01 mM)	Detection of (Pb²⁺, Cd²⁺, Cu²⁺, Zn²⁺, Ni²⁺ and Tl³⁺) is possible but, it shows higher interference in presence of different higher oxidants ions	More applicable and excellent for ultra-trace concentration test that make it suitable for multielement analysis. The preconcentration enhances sensitivity	Requires pretreatment and conditioning to limit electrode fouling possibility. High ionic strength samples may interfere with detection	[20,31]
Differential Pulse Adsorptive Stripping Voltammetry (DPASV) using biomolecules	HTEs like (Cu²⁺, Pb²⁺, Cr²⁺, Ni²⁺ and Fe³⁺) can be easily detected in water samples by using this technique, with a detection limit of (0.5–20.0 mM)	Can easily detect (Cu²⁺, Fe²⁺, Mn²⁺, Cr²⁺ and Pb²⁺)	Provides redox and mechanistic info, and it easy manageable for portable sensors (Fast screening tool and simple to implement)	Not suited for trace concentration detection due to low sensitivity compared to ASV or DPV	[21,29]
Chronopotentiometry	Aids in detect (Pb²⁺, Cd²⁺, Zn²⁺ and Cu²⁺) in water sample with a detection limit of (6.5–147.8 Mg/L)	After preconcentration of the sample, can help detect (Pb²⁺, Cd²⁺ and Zn²⁺)	Suitable for kinetic studies and can help to analyze ions in diffusion process	Lower sensitivity, not ideal for multielement detection Requiring precise control of conditions in both soils and water samples	[21,31–33]
Electrochemical impedance spectrometry (EIS)	After functionalization, can help to detect (Pb²⁺, Hg²⁺, Cd²⁺, Cu²⁺ and As³⁺) in water sample	Can be applied to detect (Pb²⁺, Cd²⁺, Cu²⁺, As³⁺) via sensor-based recognition	Excellent for biosensor integration with high surface sensitivity. This technique is very good for real-time monitoring	Requires functionalized electrodes and as an aid in complex data analysis and it is often used for indirect detection of HTEs in solution	[21–24]

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In general, electrochemical techniques especially those enhanced by functional nanomaterials have significantly advanced the capabilities for detecting trace, heavy metals in complex matrices [53–56]. While water offers a less interfering background and faster analysis, soil detection remains more intricate but increasingly feasible with optimized sample preparation and advanced electrode materials [20–23,31,53–56]. This section bridges the understanding of how HTEs detection must be adapted to different environmental samples and highlighted the way for developing multi-environment electrochemical sensors. Likewise, to soils samples analysis, HTEs detection in water samples use various electrochemical techniques such as ASV, DPV, SWV, EIS, etc. [21,22,57–62]. These techniques applied to water sample are more straightforward due to lower matrix interference of water samples and they are easier for in situ applications [7–10,26–36,63–65].

1.1. Voltammetric Techniques Applied for Detection of Heavy Traces Elements in Soils and Solution

a. Differential Pulsed Voltammetry Techniques (DPV) and Square Wave Voltammetry (SWV)

Recently, SWV and DPV have been used to detect heavy metals like Pb²⁺, Cd²⁺, Hg²⁺, Fe²⁺, Fe³⁺, and As³⁺ in soil samples and waters [15,20–28]. The DPV methods apply current or potential pulses to measure resulting current variations. This technique is providing high sensitivity and selectivity for HTEs [22–30]. In the other hand, SWV is a variant of DPV [66]. The SWV methods applied to water and soils samples offering advantages such as background suppression and enhanced sensitivity, making it a powerful tool for electrochemical analysis [67–72]. For example, reduced graphene oxide (rGO), gold nanoparticles (AuNPs), or nanostar electrodes (Fig. 1) combine with modified glassy carbon electrode (GCE) are used with DPV technique for trace level detection of Fe³⁺ in water sample with high sensitivity and detection limit of 3.5nM [22–35,42–54]. Using DPV with glassy carbon electrode modified with tannic acid-coated or supported gold nanoparticles (AuNP@TA-GCE) is highly sensitive and selective for detection of Hg²⁺ in real tap water. However, using SWV method with AuNP@TA-GCE can selectively detect Hg²⁺ in the presence of competing ions such as Zn²⁺ and Al³⁺, with a measurable lower limit of 100 fM [20–26,44–51].

Figure 1: — Representative Nyquist plots obtained on AuNS- (A) and AuNP-modified (B) CPSPE in the presence of ionic complex of iron cyanate ([Fe(CN)₆]⁴⁻ / Fe(CN)₆]³⁻; 10 mM) with 100 mM KCl with relative NP masses of 0.33–3. Figures reproduced with permission from Ref. [77].

Also, a green and straightforward strategy for the fabrication of graphite screen-printed carbon electrodes (GSPEs) with tin nanoparticles (SnNPs) via electric spark discharge process was employed for the sensitive detection of Cd²⁺ and Zn²⁺ in tap and bottle water samples. SnNPs-GSPEs electrodes exhibited stable response to Cd²⁺ and Zn²⁺ for a period of two weeks and interference of Cu²⁺ on the detection of these ions was successfully alleviated by the addition of ferrocyanide and gallium ions, respectively. With the SWV method, the environmentally friendly sensor displayed high sensitivity for Cd²⁺ and Zn²⁺ with a detection limit of 0.5 and 0.3 μg/L, respectively [20–23,26,31–37].

b. Anodic Stripping Voltammetry (ASV)

According to Potes-Lesoinne et al., V. Skiba et al., Yang et al., and Zhao et al., the ASV technique is a widely used voltammetric method for detecting and monitoring HTEs concentrations in soil and water [46–50]. This electrochemical technique is often coupled with a portable potentiostat and offers high sensitivity, selectivity, accuracy, and effectiveness for real-time detection and quantification of trace concentration of Cu²⁺, Pb²⁺, Hg²⁺, Cd²⁺, Ce³⁺, Zn²⁺, and As³⁺ [65–70]. The trends in an electrochemistry approach applied for HTEs detection in water and soils shows the great significance in the development of electrochemical sensors based on novel functional Bi/Bi₂O₃ co-doped porous as carbon composite (Bi/Bi₂O₃@C) that was prepared by simple carbonization of bismuth-based metal-organic frameworks (Bi-MOFs) [27,38]. The application of ASV technique has been used with Bismuth-Copper-Nanoparticles (BiCu-ANPs) electrodes to detect traces concentration (0,5–100ppb) of Pb²⁺, Cd²⁺, and Zn²⁺ in soil samples extracted with HNO₃ or EDTA [28;71–73]. The ASV method using SWCNT, MWCNT electrodes or SPCEs electrodes have been applied to analyze traces concentration (0,01–80nM)) of As³⁺ and Hg³⁺ in agricultural soil samples [21,22;28]. Additionally, the sensitive electrochemical sensor for Pb²⁺ detection was constructed by modifying Bi/Bi₂O₃@C on the surface of the glassy carbon electrode (GCE) based on the square wave anodic stripping voltammetric (SWASV) [40]. The different factors affecting the analytical performance were optimized systematically, such as material modification and concentration, deposition time, deposition potential, and pH value [20,27,40]. Under optimized conditions, the proposed sensor exhibited a wide linear range from 37.5 nM to 2.0 μM with a low detection limit of 6.3 nM. Meanwhile, the proposed sensor showed good stability, acceptable reproducibility, and satisfactory [38]. Trifunctional nanocomposites have also been used for the recognition and elimination of heavy metal ions (Figure 2).

Figure 2: — Schematic diagram of **(Aa)** hydrolysis and condensation of tetraethyl orthosilicate (TEOS) on Fe3O4 surface, (Ab) functionalization onto Fe3O4@SiO2. **(Ba)** Adsorption of heavy metal ions (HMIs) onto Fe₃O₄@SiO₂ and Fe₃O₄@SiO₂/TACTDD (Adsorbent dose = 1.0 g/L; Adsorbate dose = 200 mg/L; V = 50 mL; t = 12 h; Room temperature; No pH pre-adjustments; HMI = Cr³⁺, Mn²⁺, Fe³⁺, Co²⁺, Cu²⁺, Zn²⁺, Ag⁺, Cd²⁺, Hg²⁺ and Pb²+); **(Bb)** Effects of Fe³⁺ initial concentrations on adsorption; **(Bc)** Langmuir and **(Bd)** Freundlich linear fits of Fe³⁺ ion adsorbed onto Fe₃O₄@SiO₂/TACTDD. Figures reproduced with permission from Ref. [75].

c. Cyclic Voltammetry

Cyclic voltammetry (CV), as a classical electrochemical technique, is commonly used to analyze molecules including metals such as Pb²⁺, Hg²⁺, and Cu²⁺ [28]. When coupled with specific electrodes, it enhances sensitivity for detecting these metals in soil and water [51,56]. The technique involves sweeping the electrode potential and measuring the resulting current response, allowing control over the chemical reactions of heavy metals in water [53–58]. CV provides insights into the electrochemical dynamics of heavy metals and is relatively simple to use. Carbon fiber microelectrodes (CFMEs) have been utilized with fast-scan cyclic voltammetry (FSCV) for the measurement of several trace metals including copper, zinc, aluminum, magnesium, and calcium. A significant signal enhancement was reported following the deposition of a diethyl benzene linker onto the surface of the CFME for Cu²⁺ detection [55–57].

1.2. Non-Voltammetric Techniques for Heavy Metals Detection in Soils and Solution

a. Chronopotentiometry

This electrochemical technique allows the simultaneous detection of several elements HTEs in water or soil ecosystem and involves applying a constant current and measuring the potential over time. It is particularly effective for analyzing the electrodeposition of heavy metals and is valuable for precise quantification of heavy metals at low concentrations in solution (Figure 3A) [3,50]. This method is simple for use, does not use expensive chemical reagents, and it possesses high sensitivity exceeding known methods of potentiometric titration [50]. Applying the electrodeposition of the organic layer on the sensitive and stable electrodes modified with 4-aminothiophenol surface with chronopotentiometry technique to detect Pb²⁺ by differential pulse voltammetry with a linear range of 2.5–400 μg/L and the detection limit of 1.2 μg/L and Cd²⁺ with the calibration line in the range of 2.5–400 μg/L and a detection limit of 1.5 μg/L. Low interferences were observed and the electrodes were used for analysis of water samples [3,48].

Figure 3: — (A) Schematic of the chronopotentiometry technique for in situ heavy metal (HM) detection via electrodeposition(Aa), showing the two main steps of SWASV: deposition and stripping(Ab), and enhanced Cd²⁺ sensing using GSH, functionalized cysteamine, and a graphene-like 2D structure (Ac). (B) General setup for electrochemical HMI detection. Figure reproduced with permission from Ref. [49,60].

b. Electrochemical Impedance Spectroscopy

Electrochemical Impedance Spectroscopy (EIS) is an electrochemical technique increasingly used for detecting heavy metals like Zn²⁺, Cd²⁺, and Cu²⁺ due to its ability to provide insights into detection mechanisms [17,54]. EIS measures the system’s response to alternating current, allowing analysis of solution conductivity and measurement of metal concentrations, as well as the study of electrode and solution properties [57]. Recent research shows that applying EIS using functionalized carbon nanotube (FCNT) electrodes helps detecting Cr⁵⁺ in mining and industrial contaminated soils after sample extraction. For example, the electrochemical oxidation of pyrene was studied using a glassy carbon electrode (GCE) modified with a nanocomposite of copper oxide nanoparticles (CuONPs) and functionalized multi-walled carbon nanotubes (FMWCNTs) [26,29,30–37,39]. The CuONPs were synthesized via chemical co-precipitation and combined with FMWCNTs to enhance conductivity and catalytic activity [41]. Electrochemical studies using both EIS and CV with the modified electrode GCE/FMWCNTs/CuONPs showed highest current response and lowest charge transfer resistance. The sensor exhibited high sensitivity with a detection limit of 1.30 μM for pyrene. The use of EIS technique is also showed good potential for detecting toxic HTEs such as Pb²⁺, Cd²⁺, Hg²⁺, and As³⁺. The synergistic effect between CuONPs and FMWCNTs enhanced electron transfer. This nanocomposite sensor is suitable for environmental monitoring [26,29,30–37,41]. Figure 3B shows the HTEs response and general detection process.

2. Nanomaterials Combine with Electrochemical Techniques Detection of Heavy Trace Elements in water and soils matrices

Electrode materials are at the heart of electrochemical sensing [2–10]. Their physicochemical properties, such as conductivity, surface area, and binding affinity, play a crucial role in determining the sensor’s selectivity, sensitivity, detection limit, and reproducibility [6, 8, 17–23]. Recent research conducted in this field demonstrates that the modification and functionalization of electrodes with nanostructured materials (carbon nanomaterials, metals and metal oxide nanomaterials, polymer and hybrid nanomaterials, and metal-organic frameworks) has dramatically improved the analytical performance of electrochemical sensors for HTE detection in both aqueous and solid matrices [6, 18, 31–38].

Standards electrochemical techniques introduced in the previous section used for HTEs detection in water and soil environments shows different response performance (portability, temporal resolution, sensitivity, speed, detection limit, sensitivity, stability, etc.) for in situ HTEs analysis [20–23, 31]. The matrix complexity in soil can introduce interferences and affect the selectivity performance of the sensors. In addition, in comparison to the detection of HTEs in water that is generally more direct after basic filtration and pH adjustment, analyzing HTEs in soil samples usually requires acid digestion before any electrochemical analysis [11–18, 20–23, 31]. This section categorizes recent advances in electrode materials by nanomaterial type and highlights how each contributes to enhanced electrochemical behavior.

2.1. Electrochemical Methods Based on Carbon nanomaterials for Detection of Heavy Trace Elements in water and soil

Carbon nanomaterials, especially carbon nanotubes (CNTs), graphene and graphene derivatives, have become the most widely studied materials for electrochemical sensor platforms. Their exceptional electrical conductivity, high surface-to-volume ratio, and chemical stability make them ideal candidates for HTEs detection in various environments [17–23,27–30,35–37]. The SWCNTs, and MWCNTs are often functionalized with chelating agents such as EDTA or polymers to increase their selectivity and attraction capacity for specific metal ions like Pb²⁺, Cd²⁺, and Hg²⁺ [19–23,31]. Applying CV technique coupled with specific electrodes based on carbon nanomaterials, become more sensitive to analyze molecules including metals such as Pb²⁺, Hg²⁺, and Cu²⁺ in soil and water [28,53,57–59]. Conducting fast-scan cyclic voltammetry (FSCV) test, carbon fiber microelectrodes (CFMEs) have been utilized to quantify several heavy trace metals including Cu²⁺, Zn²⁺, Al³⁺, Mn²⁺, and Ca²⁺ [56–58].

For instance, a sensor platform using EDTA-functionalized MWCNTs demonstrated improved detection of Cr³⁺ ions via anodic stripping voltammetry [22, 64–70]. Graphene oxide (GO) and reduced graphene oxide (rGO) combining with SWCNT or MWCNT are also commonly used to simultaneously several HTEs in water and soil matrices. Their functional groups (-OH, -COOH, -O-) allow strong interactions with metal ions [28–30,71–74]. Additionally, recent researches (table 1) using DPV or SWV coupled with functionalized nanocomposite electrodes combining graphene oxide (GO) or reduced graphene oxide (rGO) with metals nanoparticles such as gold nanoparticle (AuNPs), silver nanoparticles (AgNPs), or bismuth nanoparticles (BiNPs) have shown increased electron transfer kinetics and higher detection sensitivity with very low detection limit [28–30,35–41]. Simultaneous detection of Pb²⁺, Cd²⁺, and Hg²⁺, using carbon nanomaterials commonly integrated with SWASV and DPASV, offers high sensitivity and low detection limits, often in the nanomolar to sub-nanomolar range [14].

Functionalization strategies such as incorporating iron oxide nanoparticles (Fe₃O₄) and polymers like polyfluorocarbon (POCF) enhance synergistic interactions, significantly improving the electrochemical response and selectivity for simultaneous detection of multiple elements such as Pb²⁺, Cd²⁺, As³⁺, Zn²⁺, Cu²⁺, and Hg²⁺ with long-term stability up to 30 days [24,25,42]. For example, Fe₃O₄/F-MWCNT-modified glassy carbon electrodes demonstrated ultra-low detection limits (0.05 nM) for Hg²⁺ and Pb²⁺ and excellent selectivity in real water samples [42]. Ligand-modified CNT electrodes also exhibit remarkable performance for dual detection of Pb²⁺ and Hg²⁺ ions, serving as a superior alternative to traditional mercury-based electrodes by offering higher sensitivity and reducing environmental hazards [19].

Additionally, composites with bismuth-copper nanoparticles and ion-imprinted polymers provide real-time detection capabilities across a broad linear range with minimal interference, enhancing sensor applicability in complex environmental matrices [27,38]. The widespread adoption of carbon nanomaterial-based electrochemical sensors is driven by their outstanding temporal stability (15–30 days) and ability to detect multiple heavy metals simultaneously with minimal cross-interference [23,26,33]. Collectively, these trends reflect a strong shift toward multifunctional, rapid, and cost-effective electrochemical sensing platforms poised to improve heavy metal monitoring in water and soil environments.

2.2. Electrochemical Methods Based on Metal and Metal Oxide Nanoparticles for Detection of Heavy Trace Elements in water and soil

Based on to their specific physical and chemical characteristics, metals and metals oxide nanoparticles have been used to detect, quantify and remove toxic heavy metal ions from polluted water and soils matrices. Recent researches in electrochemistry have been conducted to synthesize magnetic nano adsorbents due to low cost-effectiveness, being environment-friendly, easy application as a technique, high availability, biodegradability, and strong affinity for metal capping and quantification in diverse metrices [75] (Figure 2). Metal and metals oxides nanoparticles such as CuO, ZnO, TiO2, MnO2, Fe₃O₄, gold (AuNPs), silver (AgNPs), bismuth (BiNPs), palladium (PdNPs), platinum (PtNPs) and copper (CuNPs) nanoparticles respectively, are commonly incorporated into electrode surfaces to enhance redox reactions and lower the detection limits of sensors [20–23,28,73].

It was demonstrated that the poisoning reduction of toxic heavy metals in water and soils environments, post-discharge removal of metals using nanoparticles is one of the remediation technologies being explored nowadays [76–77] (Figure 1). For example, cyclic voltammetry technique combined with magnetic iron oxide nanoparticles (Fe₃O₄-NPs), has proven to be an effective method for detecting and removing toxic heavy metals such as Cd, Cr, Cu, Fe, Ni, Pb, and Zn from both water and soil samples. In water, the nanoparticles performed best at a pH of 4.5, where removal efficiency ranged between 63.5% and 98.3%. For soil, testing was conducted at a more acidic pH of 0.7, and the removal efficiency ranged from 69.6% to 99.6%. Interestingly, in both water and soil, the optimal removal occurred in under 20 minutes. However, if the process continues too long in highly acidic conditions, the nanoparticles may begin to break down or release the metals they’ve captured, reducing overall effectiveness [75].

In addition, metal oxide nanoparticles such as ZnO, TiO₂, and Fe₃O₄ provide catalytic activity and contribute to the adsorption of trace metals. Their use in hybrid nanocomposites can significantly enhance selectivity and electron transfer, especially when integrated with carbon nanostructures [17,18,29]. Mesoporous silica nanoparticles (SiO₂ NPs) have attracted significant attention in adsorption and catalysis applications due to their high surface area, tunable surface chemistry, and large pore volume. Recent studies have demonstrated the successful synthesis of SiO₂ nanoparticles employed as adsorbents for the removal of Pb²⁺ and Cu²⁺ ions from wastewater, achieving adsorption capacities of 140.06 mg/g and 149.25 mg/g[72–76].

Moreover, silica-based zinc oxide nanocomposites have been developed as effective adsorbents for the removal of Ni²⁺, Cd²⁺, and Cu²⁺ ions from aqueous solutions, with corresponding adsorption capacities of 32.53 mg/g, 32.10 mg/g, and 30.98 mg/g. Moreover, big progress in the last two years, have been demonstrated by the using of bismuth-based electrodes combine with SWASV, DPV and ASV techniques. The bismuth nanomaterials in particular, have gained attention as non-toxic alternatives to mercury electrodes. BiNPs are often used in combination with carbon-based substrates to improve mechanical stability and surface area [28]. Electrochemical sensors using BiNP-modified electrodes have been successfully used for the detection of Pb²⁺ and Cd²⁺ in both water and soil samples with high accuracy and recovery rates [28,32–34].

2.3. Electrochemical Methods Based on Polymer and Hybrid Nanocomposites for Detection of Heavy Traces Elements

Conducting polymers such as polyaniline (PANI), polypyrene (PPy), and polythiophene (PTh) are often employed to functionalize electrodes due to their redox-active behavior and film-forming properties [20–22]. When combined with nanostructured materials like CNTs or metal nanoparticles, they offer a synergistic effect, improving both sensitivity and selectivity [18,31,35]. Hybrid nanomaterials like CNT/PANI, rGO/AuNPs, and BiNPs/graphene combine give the advantages of individual components, allowing for multi-functional sensing platforms [29–31]. These composites have demonstrated excellent performance in simultaneous detection of multiple HTEs, especially when applied with stripping voltammetry techniques [21–23,36]. Recently, square wave voltammetry (SWV) and differential pulsed voltammetry (DPV) have been used to detect heavy metals like Pb²⁺, Cd²⁺, Hg²⁺, Fe²⁺, Fe³⁺, and As³⁺ in soil samples and waters [15,20–28].

The use of polymer and hybrids nanomaterials with DPV and SWV methods is providing high sensitivity and selectivity for HTEs [22–30, 66]. The SWV methods applied to water and soils samples offering advantages such as background suppression and enhanced sensitivity, making it a powerful tool for electrochemical analysis [67–72]. For example, reduced graphene oxide (rGO) or gold nanoparticles (AuNPs) combine with modified glassy carbon electrode (GCE) are used with DPV technique for trace level detection of Fe³⁺ in water sample with high sensitivity and detection limit of 3.5nM [22–35,42–54]. Using DPV with glassy carbon electrode modified with tannic acid-coated or supported gold nanoparticles (AuNP@TA-GCE) is highly sensitive and selective for detection of Hg²⁺ in real tap water. However, using SWV method with AuNP@TA-GCE can selectively detect Hg²⁺ in the presence of competing ions such as Zn²⁺ and Al³⁺, with a measurable lower limit of 100 fM [20–26,45–53].

Additionally, a green and straightforward strategy for the fabrication of graphite screen-printed carbon electrodes (GSPEs) with tin nanoparticles (SnNPs) via electric spark discharge process was employed for the sensitive detection of Cd²⁺ and Zn²⁺ in tap and bottle water samples. The SnNPs-GSPEs electrodes exhibited stable response to Cd²⁺ and Zn²⁺ for a period of two weeks and interference of Cu²⁺ on the detection of these ions was successfully alleviated by the addition of ferrocyanide and gallium ions, respectively. Using SWV method, the environmentally friendly sensor displayed high sensitivity for Cd²⁺ and Zn²⁺ with a detection limit of 0.5 and 0.3 μg/L, respectively [20–23,26,31–37].

The HTEs detection in water and soils using electrochemical sensors based on novel functional Bi/Bi₂O₃ co-doped porous as carbon composite (Bi/Bi₂O₃@C) that was prepared by simple carbonization of bismuth-based metal-organic frameworks (Bi-MOFs) shows higher sensitivity and selectivity to metals like Pb²⁺, Cd²⁺, Hg²⁺, Cu²⁺, Fe³⁺, and As³⁺ in a multiplex system without interference [27,38]. The application of ASV technique has been used with Bismuth-Copper-Nanoparticles (BiCu-NPs) electrodes to detect trace concentrations (0,5–100ppb) of Pb²⁺, Cd²⁺, and Zn²⁺ in soil samples extracted with HNO₃ or EDTA [28,73–75].

The ASV technique based on SWCNT, MWCNT electrodes or SPCEs electrodes have been applied to analyze trace concentrations (0.01–80 nM) of As³⁺ and Hg²⁺ in soil samples [21,22,28]. Moreover, the sensitive electrochemical sensor for Pb²⁺ detection was constructed by modifying Bi/Bi₂O₃@C on the surface of the glassy carbon electrode (GCE) based on the square wave anodic stripping voltammetric (SWASV) [40]. Recent research shows that applying EIS using hybrid functionalized carbon nanotube (FCNT) electrodes helps detecting Cr⁵⁺ in mining and industrial contaminated soils after sample extraction [58]. For example, the electrochemical oxidation of pyrene was studied using a glassy carbon electrode (GCE) modified with a nanocomposite of copper oxide nanoparticles (CuONPs) combined with the functionalized multi-walled carbon nanotubes (FMWCNTs) [26,29,30–37,39]. The CuONPs were synthesized via chemical co-precipitation and combined with FMWCNTs to enhance conductivity and catalytic activity [41]. The use of the modified electrode GCE/FMWCNTs coupled with SWASV showed highest current response and lowest charge transfer resistance. The current electrode exhibited high sensitivity with a detection limit of 1.50 μM for detecting toxic HTEs such as Pb²⁺, Cd²⁺, Hg²⁺, and As³⁺ which make it suitable for environmental monitoring [26,29,30, 37,41].

2.4. Electrochemical Methods Based on Metal-Organic Frameworks (MOFs) for Detection of Heavy Trace Elements

Metal organic frameworks (MOFs) are porous crystalline materials that offer tunable chemical functionality, extremely high surface area, and metal-binding affinity. They are increasingly being investigated for sensor applications due to their excellent ion exchange properties [18, 29]. Recent research has explored MOF composites with graphene, CNTs, or polymer layers, enhancing both electron transfer and structural stability [18, 29, 35]. These emerging materials show promise for next-generation electrochemical sensors, particularly in challenging matrices like wastewater or contaminated soils. Additionally, flexible and 3D-printed electrodes using nanocomposites are gaining traction. These architectures support the development of portable, wearable, or in situ devices for continuous environmental monitoring [19–22, 36].

Calcium-based MOFs, particularly the calcium dimethylacetamide [Ca(H₄L) (DMA)₂] 2DMA (Ca-MOF), have shown rapid and nearly complete ion exchange with Cu²⁺ in aqueous media. Ca-MOF demonstrates high sorption capacities for heavy metals, notably Pb²⁺ (~522 mg/g) and Cd²⁺ (~220 mg/g), among the highest reported for MOFs. It also effectively captures Ni²⁺ and Zn²⁺, even in the presence of competing ions. A column packed with Ca-MOF in silica sand efficiently removed trace Pb²⁺ (~100 ppb) from wastewater simulants. Additionally, Ca-MOF was used to fabricate an electrochemical sensor capable of detecting Pb²⁺, Cd²⁺, Cu²⁺, and Zn²⁺ at low concentrations via anodic stripping voltammetry. This dual functionality as both sorbent and sensor positions Ca-MOF as a promising material for integrated heavy metal remediation and monitoring in water systems [42].

Additionally, a nanocomposite based on poly(amidoamine) dendrimers and nickel-based metal–organic frameworks (Ni-MOFs) has been developed as an electrochemical sensing platform for the simultaneous detection of Pb²⁺ and Cu²⁺ in water [32–42]. The modified glassy carbon electrode, operated via square wave anodic stripping voltammetry (SWASV), demonstrated a linear detection range of 1–100 μg/L and achieved detection limits of 1.21 μg/L for Pb²⁺ and 0.77 μg/L for Cu²⁺ well below the World Health Organization’s guidelines for drinking water. The sensor exhibited high selectivity (ΔI < 17% in the presence of tenfold interferents), strong repeatability (RSD < 3.56% across five electrodes), and operational stability (over 95% signal retention after 30 days) [39–42]. Notably, the system enabled rapid, on-site detection within seven minutes, highlighting its practicality for field deployment. Its compact design, low cost, and ease of use make it a promising alternative to traditional analytical methods for environmental monitoring and industrial wastewater analysis [42].

3. Conclusions and Outlook

The contamination of water and soil by HTEs poses a significant threat to ecosystems and public health. These metals are non-biodegradable and constitute a big risk. Traditional analytical methods such as Atomic Absorption Spectroscopy (AAS), Inductively Coupled Plasma Mass Spectrometry (ICP-MS), and X-ray Fluorescence Spectroscopy (XRFS) have long been used for the detection and quantification of HTEs due to their high sensitivity and accuracy. However, these methods are expensive, time-consuming, require well-equipped laboratories, and are not suitable for in situ or real-time monitoring limiting their use in field applications and decentralized settings. In the need of developing sensors for HTEs monitoring in situ, electrochemical detection methods have gained growing attention as alternatives for real-time, cost-effective, and portable monitoring of HTEs in both water and soil matrices. Standard techniques such as square wave voltammetry (SWV), differential pulse voltammetry (DPV), anodic stripping voltammetry (ASV), and electrochemical impedance spectroscopy (EIS), offer rapid response times and enhanced sensitivity and selectivity but they are still showing multiple challenges that differ from water or soil matrices (Table 1).

To further enhance the performance of electrochemical techniques, numerous nanomaterials such as carbon-based nanomaterials including single-walled carbon nanotubes (SWCNTs), multi-walled carbon nanotubes (MWCNTs), and reduced graphene oxide (rGO) which offer high surface area, excellent conductivity, and mechanical stability have been employed recently. Furthermore, functionalization of these nanomaterials introduces active sites for selective binding of metal ions, significantly improving sensitivity and selectivity. Additionally, metal nanoparticles like AuNPs, BiCu-AuNP; functional group such as OH-, -COOH; polymer and hybrid nanomaterials including AuNP@TA-GCE, Ca-MOF, Ni-MOF, Bi-MOF, Cu-MOF etc. coupled with CNTs (SWCNT and MWCNT) improve the selectivity and sensitivity of electrochemical sensors in detection at trace level of HTEs in soil and water.

However, their application still faces important challenges. In particular, soil sample analysis presents more complex matrix compared to water samples, with varying pH, ionic strength, and organic matter content, which can interfere with sensor response and limit accuracy. Additional issues include electrode fouling, sensor degradation over time, and lack of standardized protocols for calibration and inter-laboratory validation (Table 2). Also, materials like CNTs which constitute the base show higher degradability rate which make the materials non suitable for water and various environment monitoring. To significantly improve efficiency of the electrochemistry techniques and significantly reduce the environmental risk due to HTEs pollution, future research should focus on the development of multielement sensors for simultaneous detection multiple heavy metal ions in water and soils and strategies to minimize matrix effects, especially in complex soil environments.

In conclusion, considerable progress has been made to improve detection accuracy of electrochemical techniques for HTEs analysis. Key challenges remain such as multiplexed detection, integration with machine learning, and field-deployable robust sensors. A comprehensive approach that combines the design of robust nanomaterials and advanced electrochemical sensing techniques will be key to enabling next-generation technologies for accurate, real-time monitoring of heavy metal pollution in both water and soil systems. Such development will not only address environmental and health risks but also will enable future sustainable development and responsible resource management.

Footnotes

Declaration of interests

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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PERMALINK

Recent Trends in Electrochemical Methods for Real-Time Detection of Heavy Metals in Water and Soil: A Review

Pythagore L Kyabutwa

Nadiah Alyamni

Jandro L Abot

Alexander G Zestos

Abstract

Introduction