12 research outputs found

    Techno-Economic Analysis of Electrocoagulation on Water Reclamation and Bacterial/Viral Indicator Reductions of a High-Strength Organic Wastewater—Anaerobic Digestion Effluent

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    This study investigated the use of iron and aluminum and their combinations as electrodes to determine the technically sound and economically feasible electrochemical approach for the treatment of anaerobic digestion effluent. The results indicated that the use of iron as anode and cathode is the most suitable solution among different electrode combinations. The reduction of turbidity, total chemical oxygen demand, total phosphorus, total coliforms, Escherichia coli, Enterococci, and phages in the reclaimed water were 99%, 91%, 100%, 1.5 log, 1.7 log, 1.0 log, and 2.0 log, respectively. The economic assessment further concluded that the average treatment cost is $3 per 1000 L for a small-scale operation handling 3000 L wastewater/day. This study demonstrated that the electrocoagulation (EC) is a promising technique for the recovery and reclamation of water from anaerobic digestion effluent. Even though its energy consumption is higher and the nitrogen removal is insufficient compared to some conventional wastewater treatment technologies, there are several advantages of the EC treatment, such as short retention time, small footprint, no mixing, and gradual addition of coagulants. These features make EC technology applicable to be used alone or combined with other technologies for a wide range of wastewater treatment application

    Next-Generation Diamond Electrodes for Neurochemical Sensing: Challenges and Opportunities

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    © 2021 by the authors. Licensee MDPI, Basel, Switzerland. Carbon-based electrodes combined with fast-scan cyclic voltammetry (FSCV) enable neurochemical sensing with high spatiotemporal resolution and sensitivity. While their attractive electrochemical and conductive properties have established a long history of use in the detection of neurotransmitters both in vitro and in vivo, carbon fiber microelectrodes (CFMEs) also have limitations in their fabrication, flexibility, and chronic stability. Diamond is a form of carbon with a more rigid bonding structure (sp3-hybridized) which can become conductive when boron-doped. Boron-doped diamond (BDD) is characterized by an extremely wide potential window, low background current, and good biocompatibility. Additionally, methods for processing and patterning diamond allow for high-throughput batch fabrication and customization of electrode arrays with unique architectures. While tradeoffs in sensitivity can undermine the advantages of BDD as a neurochemical sensor, there are numerous untapped opportunities to further improve performance, including anodic pretreatment, or optimization of the FSCV waveform, instrumentation, sp2 /sp3 character, doping, surface characteristics, and signal processing. Here, we review the state-of-the-art in diamond electrodes for neurochemical sensing and discuss potential opportunities for future advancements of the technology. We highlight our team’s progress with the development of an all-diamond fiber ultramicroelectrode as a novel approach to advance the performance and applications of diamond-based neurochemical sensors

    New Avenues in Electrochemical Systems and Analysis

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    Fabrication and characterization of boron doped diamond microelectrode arrays of varied geometry

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    Boron doped diamond (BDD) is a well-known electrode material that exhibits an excellent electrochemical potential window with very low background current. With this, microelectrodes and microelectrode arrays (MEAs) have been found to even further lower background currents without compromising sensitivity. As such, BDD MEAs are excellent electrode materials for a variety of electroanalytical applications, capable of multi-mode detection. We fabricated BDD MEAs adapting traditional semiconductor microfabrication processes; the resulting MEAs were patterned in different geometries to find an optimum electrochemical response, depending on the application. This is demonstrated using 4 different MEA geometries of different size and spacing using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS), where the charge transfer resistance (Rct) increases as the electrodes are farther spaced from one another. Excellent sigmoidal voltammogram shape in CV was obtained for each BDD MEA geometry. BDD MEAs spaced farther from one another were found to give better resolution from the background in fast scan cyclic voltammetric measurements of dopamine due to the decrease in the double layer capacitance (Cdl) as verified with EIS. This work furthers the understanding of BDD MEAs and their pertinence to sensitive electroanalytical techniques. Keywords: Boron doped diamond, Microelectrode arrays, Fabricatio

    Cloud Point Extraction for Electroanalysis: Anodic Stripping Voltammetry of Cadmium

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    Cloud point extraction (CPE) is a well-established technique for the preconcentration of hydrophobic species from water without the use of organic solvents. Subsequent analysis is then typically performed via atomic absorption spectroscopy (AAS), UV–vis spectroscopy, or high performance liquid chromatography (HPLC). However, the suitability of CPE for electroanalytical methods such as stripping voltammetry has not been reported. We demonstrate the use of CPE for electroanalysis using the determination of cadmium (Cd<sup>2+</sup>) by anodic stripping voltammetry (ASV). Rather than using the chelating agents which are commonly used in CPE to form a hydrophobic, extractable metal complex, we used iodide and sulfuric acid to neutralize the charge on Cd<sup>2+</sup> to form an extractable ion pair. This offers good selectivity for Cd<sup>2+</sup> as no interferences were observed from other heavy metal ions. Triton X-114 was chosen as the surfactant for the extraction because its cloud point temperature is near room temperature (22–25 °C). Bare glassy carbon (GC), bismuth-coated glassy carbon (Bi-GC), and mercury-coated glassy carbon (Hg-GC) electrodes were compared for the CPE-ASV. A detection limit for Cd<sup>2+</sup> of 1.7 nM (0.2 ppb) was obtained with the Hg-GC electrode. ASV with CPE gave a 20x decrease (4.0 ppb) in the detection limit compared to ASV without CPE. The suitability of this procedure for the analysis of tap and river water samples was demonstrated. This simple, versatile, environmentally friendly, and cost-effective extraction method is potentially applicable to a wide variety of transition metals and organic compounds that are amenable to detection by electroanalytical methods

    Analysis of Ag(I) Biocide in Water Samples Using Anodic Stripping Voltammetry with a Boron-Doped Diamond Disk Electrode

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    The electroanalytical performance of a new commercial boron-doped diamond disk and a traditional nanocrystalline thin-film electrode were compared for the anodic stripping voltammetric determination of Ag­(I). The diamond disk electrode is more flexible than the planar film as the former is compatible with most electrochemical cell designs including those incorporating magnetic stirring. Additionally, mechanical polishing and surface cleaning are simpler to execute. Differential pulse anodic stripping voltammetry (DPASV) was used to detect Ag­(I) in standard solutions after optimization of the deposition potential, deposition time and scan rate. The optimized conditions were used to determine the concentration of Ag­(I) in a NASA simulated potable water sample and a NIST standard reference solution. The electrochemical results were validated by ICP-OES measurements of the same solutions. The detection figures of merit for the disk electrode were as good or superior to those for the thin-film electrode. Detection limits were ≤5 μg L<sup>–1</sup> (S/N = 3) for a 120 s deposition period, and response variabilities were <5% RSD. The polished disk electrode presented a more limited linear dynamic range presumably because of the reduced surface area available for metal phase formation. The concentrations of Ag­(I) in the two water samples, as determined by DPASV, were in good agreement with the concentrations determined by ICP-OES

    Isatin Detection Using a Boron-Doped Diamond 3‑in‑1 Sensing Platform

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    Boron-doped diamond (BDD) is a promising electrochemical tool that exhibits excellent chemical sensitivity and stability. These intrinsic advantages coupled with the material’s vast microfabrication flexibility make BDD an attractive sensing device. In this study, two different 3-in-1 BDD electrode sensors were fabricated, characterized, and investigated for their capability to detect isatin, an anxiogenic indole that possesses anticonvulsant activity. Each device was comprised of a working, reference, and auxiliary electrode, all made of BDD. Two different working electrode geometries were studied, a 2 mm diameter macroelectrode (MAC) and a microelectrode array (MEA). The BDD quasi-reference electrode was studied by measuring its potential against a traditional Ag/AgCl reference electrode. While the potential shifted as a function of solution pH, a miniscule potential drift was observed when holding the solution pH constant. Specifically, the BDD quasi-reference electrode had a potential of −0.2 V (vs Ag/AgCl) in a pH 7 solution, and this remained stable for a 30-h time period. For the detection of isatin, solutions were analyzed using both sensors in pH 7.4 phosphate buffered saline (PBS). Using the MEA sensor, the limit of detection (LOD, (3σ)/<i>m</i>) for isatin was found to be 0.04 μM; an increase to 0.22 μM was observed with the MAC sensor. These results were compared to those obtained from UV–vis spectrophotometry, where a 0.57 μM LOD was observed. The feasibility for use in a complex sample matrix was also examined by completing measurements in urine simulant. The results presented herein indicate that both 3-in-1 BDD sensors are applicable at low limits of detection with potential application as an electrochemical detector for chromatographic methods

    Bare and Polymer-Coated Indium Tin Oxide as Working Electrodes for Manganese Cathodic Stripping Voltammetry

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    Though an essential metal in the body, manganese (Mn) has a number of health implications when found in excess that are magnified by chronic exposure. These health complications include neurotoxicity, memory loss, infertility in males, and development of a neurologic psychiatric disorder, manganism. Thus, trace detection in environmental samples is increasingly important. Few electrode materials are able to reach the negative reductive potential of Mn required for anodic stripping voltammetry (ASV), so cathodic stripping voltammetry (CSV) has been shown to be a viable alternative. We demonstrate Mn CSV using an indium tin oxide (ITO) working electrode both bare and coated with a sulfonated charge selective polymer film, polystyrene-<i>block</i>-poly­(ethylene-<i>ran</i>-butylene)-<i>block</i>-polystyrene-sulfonate (SSEBS). ITO itself proved to be an excellent electrode material for Mn CSV, achieving a calculated detection limit of 5 nM (0.3 ppb) with a deposition time of 3 min. Coating the ITO with the SSEBS polymer was found to increase the sensitivity and lower the detection limit to 1 nM (0.06 ppb). This polymer modified electrode offers excellent selectivity for Mn as no interferences were observed from other metal ions tested (Zn<sup>2+</sup>, Cd<sup>2+</sup>, Pb<sup>2+</sup>, In<sup>3+</sup>, Sb<sup>3+</sup>, Al<sup>3+</sup>, Ba<sup>2+</sup>, Co<sup>2+</sup>, Cu<sup>2+</sup>, Ni<sup>3+</sup>, Bi<sup>3+</sup>, and Sn<sup>2+</sup>) except Fe<sup>2+</sup>, which was found to interfere with the analytical signal for Mn<sup>2+</sup> at a ratio 20:1 (Fe<sup>2+</sup>/Mn<sup>2+</sup>). The applicability of this procedure to the analysis of tap, river, and pond water samples was demonstrated. This simple, sensitive analytical method using ITO and SSEBS-ITO could be applied to a number of electroactive transition metals detectable by CSV
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