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Advanced Sensors for the Detection of Heavy Metals

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A special issue of Sensors (ISSN 1424-8220). This special issue belongs to the section "Chemical Sensors".

Deadline for manuscript submissions: closed (30 September 2019) | Viewed by 42623

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Special Issue Editors

Prof. Dr. José Manuel Dı́az-Cruz

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Guest Editor

Department of Chemical Engineering and Analytical Chemistry, University of Barcelona, E08028 Barcelona, Spain
Interests: electrochemical sensors; screen-printed devices; chemometrics; heavy metal ions; food authentication
Special Issues, Collections and Topics in MDPI journals

Dr. Núria Serrano

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Guest Editor

Department of Chemical Engineering and Analytical Chemistry, University of Barcelona, Martí i Franquès 1-11, 08028 Barcelona, Spain
Interests: electrochemical sensors; screen-printed devices; chemometrics; persistent and emerging pollutants; electronic tongues; liquid chromatography; food authentication
Special Issues, Collections and Topics in MDPI journals

Dr. Xavier Cetó

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Guest Editor

Department of Chemical Engineering and Analytical Chemistry, University of Barcelona, Barcelona, Spain
Interests: electrochemical (bio)sensors, screen-printed devices, electronic tongues, chemometrics, heavy metal ions, food authentication
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Heavy metal ions coming from both natural and anthropogenic sources dramatically contribute to environmental pollution and constitute a serious threat for human health, especially considering its non-biodegradable character and the tendency to bioaccumulate and biomagnificate. This is why many international regulations stablish maximum concentrations for a series of metals and metalloids in water, food products and drugs, mostly based on toxicological studies. This requires the development of reliable analytical methods for the determination of such substances. For this purpose, inductively coupled plasma (ICP) techniques are very well suited, since they provide multi-element analysis with an excellent accuracy. However, ICP methods suffer from too high costs and lack of portability, which is a serious drawback in situations that require in situ measurements, fast and cheap screening of as much elements as possible or real-time monitoring in flow systems. In these cases, electrochemical, optical and hybrid sensors, alone or integrated into sensor arrays, can be a valuable alternative to ICP methods.

With these facts in mind, many efforts have been made in the last years to develop suitable sensors for the fast, low-cost, in situ, on-line detection of heavy metal ions. In this context, there is an increasing popularity of screen-printed devices, nanoparticles and nanomaterials and a growing interest on the combination of sensors into complex arrays and on the powerful chemometric methods required for processing the resulting multivariate data sets.

In this regards, this Special Issue aims to cover the advances in electrochemical, optical and hybrid sensing technologies for fast, reliable and affordable detection of heavy metal ions. Both research papers and review articles will be considered. We look forward to and welcome your participation in this Special Issue.

Potential topics may be the following:

Electrochemical sensors for heavy metal detection based on screen-printed devices
Electrochemical sensors for heavy metal detection based on nanoparticles and nanomaterials
Modification of electrodes using different strategies (drop casting, electroplating, electrografting, electropolymerization, etc.) in order to detect heavy metals.
Optical sensors for heavy metal detection
Biosensors for the detection of heavy metals
Heavy metal sensing in flow systems
Electronic tongues and other sensor arrays for detecting heavy metals
Chemometric methods for the analysis of data obtained with heavy metal sensors
Application of heavy metal sensing to environmental analysis
Heavy metal sensing in food science

Prof. Dr. José Manuel Dı́az-Cruz
Prof. Dr. Núria Serrano
Dr. Xavier Cetó
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Sensors is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

Heavy metal ions
Electrochemical sensors
Optical sensors
Hybrid sensors
Biosensors
Sensor arrays
Electronic tongues
Screen-printed devices
Complexing agents
Sensors modification
Flow-injection analysis (FIA)
Sequential-injection analysis (SIA)
Screening of heavy metals
Monitoring of heavy metals
Determination of heavy metals
Multivariate data analysis
Chemometrics
Food safety
Drug analysis
Environmental monitoring

Published Papers (10 papers)

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Research

10 pages, 5071 KiB

Open AccessArticle

Disposable Injection Molded Conductive Electrodes Modified with Antimony Film for the Electrochemical Determination of Trace Pb(II) and Cd(II)

by Savvina Christidi, Alexia Chrysostomou, Anastasios Economou, Christos Kokkinos, Peter R. Fielden, Sara J. Baldock and Nicholas J. Goddard

Sensors 2019, 19(21), 4809; https://doi.org/10.3390/s19214809 - 05 Nov 2019

Cited by 11 | Viewed by 2823

Abstract

This work describes a novel electrochemical sensor fabricated by an injection molding process. This device features a conductive polymer electrode encased in a plastic holder and electroplated in situ with a thin antimony film. The antimony film sensor was applied to the determination of Pb(II) and Cd(II) by anodic stripping voltammetry (ASV). The deposition of Sb on the sensor was studied by cyclic voltammetry (CV) and microscopy. The experimental variables (concentration of the antimony plating solution, deposition potential and time, stripping waveform) were investigated, and the potential interferences were studied and addressed. The limits of detection were 0.95 μg L⁻¹ for Pb(II) and 1.3 for Cd(II) (at 240 s of preconcentration) and the within-sensor percentage relative standard deviations were 4.2% and 4.9%, respectively, at the 25 μg L⁻¹ level (n = 8). Finally, the sensor was applied to the determination of Pb(II) and Cd(II) in a phosphorite sample and a lake water sample. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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14 pages, 2818 KiB

Open AccessArticle

Strategies for Surface Modification with Ag-Shaped Nanoparticles: Electrocatalytic Enhancement of Screen-Printed Electrodes for the Detection of Heavy Metals

by Karina Torres-Rivero, Lourdes Torralba-Cadena, Alexandra Espriu-Gascon, Ignasi Casas, Julio Bastos-Arrieta and Antonio Florido

Sensors 2019, 19(19), 4249; https://doi.org/10.3390/s19194249 - 30 Sep 2019

Cited by 31 | Viewed by 3735

Abstract

Screen-printed carbon nanofiber electrodes (SPCNFEs) represent an alternative with great acceptance due to their results, as well as their low impact on the environment. In order to improve their performance, in the present work they were modified with silver nanoparticles (Ag-NPs) and electrochemically characterized by using anodic stripping voltammetry. From the Ag-NP synthesis, silver seeds (Ag-NS) and silver nanoprisms (Ag-NPr) were obtained. The Ag-NP formation was confirmed by micrographs, where Ag-NPs with diameters of 12.20 ± 0.04 nm for Ag-NS and 20.40 ± 0.09 nm for Ag-NPr were observed. The electrodes were modified by using three different deposition methods—drop-casting, spin-coating, and in situ approaches—that offer different nanoparticle distribution and electrode modification times. It was observed that the last methodology showed a low amount of Ag-NS deposited on the electrode surface and deep alteration of this surface. Those facts suggest that the in situ synthesis methodology was not appropriate for the determination of heavy metals, and it was discarded. The incorporation of the nanoparticles by spin-coating and drop-casting strategies showed different spatial distribution on the electrode surface, as proved by scanning electron microscopy. The electrodes modified by these strategies were evaluated for the cadmium(II) and lead(II) detection using differential pulse anodic stripping voltammetry, obtaining detection limit values of 2.1 and 2.8 µg·L⁻¹, respectively. The overall results showed that the incorporation route does not directly change the electrocatalytic effect of the nanoparticles, but the shape of these nanoparticles (spherical for seeds and triangular for prisms) has preferential electrocatalytic enhancement over Cd(II) or Pb(II). Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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16 pages, 1128 KiB

Open AccessArticle

Use of Cyanobacterial Luminescent Bioreporters to Report on the Environmental Impact of Metallic Nanoparticles

by Jara Hurtado-Gallego, Francisco Leganés, Roberto Rosal and Francisca Fernández-Piñas

Sensors 2019, 19(16), 3597; https://doi.org/10.3390/s19163597 - 19 Aug 2019

Cited by 5 | Viewed by 2605

Abstract

Due to their ecological relevance, low cost, and easy maintenance, cyanobacteria have been used for bioreporter development. In this study, a battery of cyanobacterial bioreporters has been used to assess the ecotoxicity of four highly used metallic nanoparticles (NPs). The toxicity of these NPs was tested using the bioreporter Nostoc CPB4337 (Anabaena CPB4337). As oxidative stress is a primary toxic mechanism of metallic NPs, cyanobacterial reactive oxygen species (ROS)-detecting bioreporters were used. Metallic NPs release metal ions, which contribute to their toxic effect and the formation of ROS, so a metal-detecting bioreporter was also used to detect the bioavailable metals. The results confirm that ROS production by NPs was due to the NPs per se and not by released free-ions, which in fact were almost undetectable. Although the metal-detecting bioreporter could not detect the dissolved metal ions, it was able to detect the metallic NPs themselves, indicating that this bioreporter may be useful to detect them in the environment. ROS production varied depending on the growth medium or environmental matrices conditions and on the NP type. This work demonstrated the different levels of ROS production by metallic NPs and the importance of nanotoxicology studies in real matrices. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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11 pages, 2058 KiB

Open AccessArticle

A Simple and Label-Free Detection of As³⁺ using 3-nitro-L-tyrosine as an As³⁺-chelating Ligand

by Jin-Ho Park, Gyuho Yeom, Donggu Hong, Eun-Jung Jo, Chin-Ju Park and Min-Gon Kim

Sensors 2019, 19(13), 2857; https://doi.org/10.3390/s19132857 - 27 Jun 2019

Cited by 7 | Viewed by 3178

Abstract

A simple and rapid As³⁺ detection method using 3-nitro-L-tyrosine (N-Tyr) is reported. We discovered the specific property of N-Tyr, which specifically chelates As³⁺. The reaction between As³⁺ and N-Tyr induces a prompt color change to vivid yellow, concomitantly increasing the absorbance at 430 nm. The selectivity for As³⁺ is confirmed by competitive binding experiments with various metal ions (Hg²⁺, Pb²⁺, Cd²⁺, Cr³⁺, Mg²⁺, Ni²⁺, Cu²⁺, Fe²⁺, Ca²⁺, Zn²⁺, and Mn²⁺). Also, the N-Tyr binding site, binding affinity, and As³⁺/N-Tyr reaction stoichiometry are investigated. The specific reaction is utilized to design a sensor that enables the quantitative detection of As³⁺ in the 0.1–100 μM range with good linearity (R² = 0.995). Furthermore, the method’s applicability for the analysis of real samples, e.g., tap and river water, is successfully confirmed, with good recoveries (94.32–109.15%) using As³⁺-spiked real water samples. We believe that our discovering and its application for As³⁺ analysis can be effectively utilized in environmental analyses such as those conducted in water management facilities, with simplicity, rapidity, and ease. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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12 pages, 3548 KiB

Open AccessArticle

Preparation of Selective and Reproducible SERS Sensors of Hg²⁺ Ions via a Sunlight-Induced Thiol–Yne Reaction on Gold Gratings

by Olga Guselnikova, Vaclav Svorcik, Oleksiy Lyutakov, Mohamed M. Chehimi and Pavel S. Postnikov

Sensors 2019, 19(9), 2110; https://doi.org/10.3390/s19092110 - 07 May 2019

Cited by 21 | Viewed by 3936

Abstract

In this contribution, we propose a novel functional surface-enhanced Raman spectroscopy (SERS) platform for the detection of one of the most hazardous heavy metal ions, Hg²⁺. The design of the proposed sensor is based on the combination of surface plasmon-polariton (SPP) supporting gold grating with the high homogeneity of the response and enhancement and mercaptosuccinic acid (MSA) based specific recognition layer. For the first time, diazonium grafted 4-ethynylphenyl groups have undergone the sunlight-induced thiol–yne reaction with MSA in the presence of Eosine Y. The developed SERS platform provides an extremely sensitive, selective, and convenient analytical procedure to detect mercury ions with limit of detection (LOD) as low as 10⁻¹⁰ M (0.027 µg/L) with excellent selectivity over other metals. The developed SERS sensor is compatible with a portable SERS spectrophotometer and does not require the expensive equipment for statistical methods of analysis. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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13 pages, 2314 KiB

Open AccessArticle

Multiplexed Ultra-Sensitive Detection of Cr(III) and Cr(VI) Ion by FET Sensor Array in a Liquid Medium

by Suman Shahim, Revathi Sukesan, Indu Sarangadharan and Yu-Lin Wang

Sensors 2019, 19(9), 1969; https://doi.org/10.3390/s19091969 - 26 Apr 2019

Cited by 16 | Viewed by 5201

Abstract

Chromium, one of the top five toxic heavy metals ranked according to significance in public health by WHO, exists as Cr(III) which is naturally occurring or Cr(VI) which is anthropogenic in origin. The EPA specifies the maximum contaminant level in drinking water to be 10⁻⁶ M or 0.1 mg/L or 100 ppb for the total dissolved Cr. To ensure the water consumed by the population has these pollutants below the safe threshold, this report demonstrates a field effect transistor (FET) based sensor design incorporating a highly target specific ion-selective membrane combined with extended gate technology which manifests sensitivity exceeding the Nernst limit aided by the high field effect in the short gap region of extended gate technology. Characterization and repeated testing of the portable device revealed a commendable calibration sensitivity of 99 mV/log [Cr³⁺] and 71 mV/log [Cr⁶⁺] for Cr(III) and Cr(VI) respectively, well surpassing the Nernst limits of sensitivity and offering a detection limit lower than ion-selective electrodes (10⁻⁶ M), and comparable to the expensive benchtop laboratory instrument, ICP-MS. This report presents a robust, easy to fabricate, economic and efficient handheld biosensor to detect the chromium in a liquid sample whether it exists as Cr(III) or Cr(VI). Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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11 pages, 2199 KiB

Open AccessFeature PaperArticle

Trace Voltammetric Determination of Lead at a Recycled Battery Carbon Rod Electrode

by Kevin Honeychurch

Sensors 2019, 19(4), 770; https://doi.org/10.3390/s19040770 - 13 Feb 2019

Cited by 6 | Viewed by 4669

Abstract

Carbon rod electrodes (CREs) were obtained from recycled zinc–carbon batteries and were used without further modification for the measurement of trace concentrations of lead (Pb). The electrochemical behavior of Pb at these electrodes in a variety of supporting electrolytes was investigated by cyclic voltammetry. The anodic peaks obtained on the reverse scans were indicative of Pb being deposited as a thin layer on the electrode surface. The greatest signal–to–noise ratios were obtained in organic acids compared to mineral acids, and acetic acid was selected as the supporting electrolyte for further studies. Conditions were optimized, and it was possible to determine trace concentrations of Pb by differential pulse anodic stripping voltammetry. A supporting electrolyte of 4% v/v acetic acid, with a deposition potential of −1.5 V (vs. SCE) and a deposition time of 1100 s, was found to be optimum. A linear range of 2.8 µg/L to 110 µg/L was obtained, with an associated detection limit (3σ) of 2.8 µg/L. A mean recovery of 95.6% (CV=3.9%) was obtained for a tap water sample fortified with 21.3 µg/L. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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12 pages, 3833 KiB

Open AccessArticle

Nafion-Protected Sputtered-Bismuth Screen-Printed Electrode for On-site Voltammetric Measurements of Cd(II) and Pb(II) in Natural Water Samples

by Samuel Frutos-Puerto, Conrado Miró and Eduardo Pinilla-Gil

Sensors 2019, 19(2), 279; https://doi.org/10.3390/s19020279 - 11 Jan 2019

Cited by 20 | Viewed by 4496

Abstract

In this work, we explore the protection with Nafion of commercial sputtered-bismuth screen-printed electrodes (Bi_SPSPEs), to improve its ability for on-site determination of Cd(II) and Pb(II) ions in ambient water samples. The modified screen-printed platform was coupled with a miniaturized cell, in combination with a battery-operated stirring system and a portable potentiostat operated by a laptop for decentralized electrochemical measurements using Square-Wave Anodic Stripping Voltammetry (SWASV). We also describe a detailed electrode surface characterization by microscopy and surface analysis techniques, before and after the modification with Nafion, to get insight about modification effect on signal size and stability. Optimization of the chemical composition of the medium including the optimization of pH, and instrumental parameters, resulted in a method with detection limits in the low ng/mL range (3.62 and 3.83 ng·mL⁻¹ for Cd and Pb respectively). Our results show an improvement of the sensitivity and stability for Nafion-protected Bi_SPSPEs in pH = 4.4 medium, and similar or lower detection limits than comparable methods on commercial Bi_SPSPEs. The values obtained for Pb(II) and Cd(II) in natural water samples agreed well with those obtained by the much more costly Inductively Coupled Plasma Mass Spectrometry, ICP-MS, technique as a reference method (recoveries from 75% to 111%). Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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16 pages, 3847 KiB

Open AccessArticle

Reusability of SPE and Sb-modified SPE Sensors for Trace Pb(II) Determination

by Matjaž Finšgar, David Majer, Uroš Maver and Tina Maver

Sensors 2018, 18(11), 3976; https://doi.org/10.3390/s18113976 - 15 Nov 2018

Cited by 12 | Viewed by 4766

Abstract

In this work, unmodified screen-printed electrode (bare SPE) and Sb-film modified SPE (SbFSPE) sensors were employed for the analysis of trace amounts of Pb(II) in non-deaerated water solutions. The modified electrode was performed in situ in 0.5 mg/L Sb(III) and 0.01 M HCl. The methodology was validated for an accumulation potential of –1.1 V vs. Ag/AgCl and an accumulation time of 60 s. A comparative analysis of bare SPE and SbFSPE showed that the detection and quantification limits decrease for the bare SPE. The method with the bare SPE showed a linear response in the 69.8–368.4 µg/L concentration range, whereas linearity for the SbFSPE was in the 24.0–319.1 µg/L concentration range. This work also reports the reason why the multiple standard addition method instead of a linear calibration curve for Pb(II) analysis should be employed. Furthermore, the analytical method employing SbFSPE was found to be more accurate and precise compared to the use of bare SPE when sensors were employed for the first time, however this performance changed significantly when these sensors were reused in the same manner. Furthermore, electrochemical impedance spectroscopy was used for the first time to analyse the electrochemical response of sensors after being used for multiple successive analyses. Surface characterisation before and after multiple successive uses of bare SPE and SbFSPE sensors, with atomic force microscopy and field emission scanning electron microscopy, showed sensor degradation. The interference effect of Cd(II), Zn(II), As(III), Fe(II), Na(I), K(I), Ca(II), Mg(II), NO₃^–, Bi(III), Cu(II), Sn(II), and Hg(II) on the Pb(II) stripping signal was also studied. Finally, the application of SbFSPE was tested on a real water sample (from a local river), which showed high precision (RSD = 8.1%, n = 5) and accurate results. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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13 pages, 2586 KiB

Open AccessArticle

Functionalized Fiber End Superstructure Fiber Bragg Grating Refractive Index Sensor for Heavy Metal Ion Detection

by Rex Xiao Tan, Stephanie Hui Kit Yap, Yung Chuen Tan, Swee Chuan Tjin, Morten Ibsen, Ken Tye Yong and Wenn Jing Lai

Sensors 2018, 18(6), 1821; https://doi.org/10.3390/s18061821 - 05 Jun 2018

Cited by 21 | Viewed by 4773

Abstract

We present a novel superstructure fiber Bragg grating fiber end sensor capable of detecting variations in refractive index (RI) of liquids and potentially that of gases, and demonstrated an application in the detection of heavy metal ions in water. The sensor is capable of sensing RI variations in the range of 1.333 to 1.470 with good sensitivity of up to 230 dB/RIU achieved for the RI range of 1.370 to 1.390. The sensor is capable of simultaneously measuring variations in ambient temperature along with RI. A simple chemical coating was employed as a chelating agent for heavy metal ion detection at the fiber end to demonstrate an possible application of the sensor. The coated fiber sensor can conclusively detect the presence of heavy metal ions with concentrations upwards of 100 ppm. RI sensing capability of the sensor is neither affected by temperature nor strain and is both robust and easily reproducible. Full article

(This article belongs to the Special Issue Advanced Sensors for the Detection of Heavy Metals)

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