Microwave activation of electrochemical processes: enhanced PbO2 electrodeposition, stripping and electrocatalysis

Marken, Frank; Tsai, Yu Chen; Saterlay, Andrew J.; Coles, Barry A.; Tibbetts, Daniel F.; Holt, Katherine B.; Goeting, Christiaan H.; Foord, John S.; Compton, Richard G.

doi:10.1007/s100080000162

Cited by 31 publications

(21 citation statements)

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“…1) consisted of a three-electrode arrangement with a Pt-mesh counter electrode (2), a saturated Calomel electrode (SCE, Radiometer) as reference (1), and a special microwave working electrode (3) made of 250 mm diameter platinum wire (Micro Glass Instruments, Greensborough, Victoria 3088, Australia or Scienglass, 46 Witney Road, Long Hanborough, Oxfordshire OX8 8BJ, UK). The working electrode was modi®ed [17] with a 150 mm diameter tungsten rod coated with a borondoped diamond ®lm (doping level approximately 10 19 ± 10 20 cm 73 ) connected to the platinum wire with conducting silver loaded epoxy adhesive and mounted with Torr Seal [17]. For microwave activation experiments a modi®ed multimode microwave oven (Panasonic NN-3456, 2.45 GHz) with modi®ed power supply, a water energy sink, and a special port [18] for the electrochemical cell were used.…”

Section: Instrumentationmentioning

confidence: 99%

“…The combination of microwave enhancement and boron-doped diamond electrode material has been introduced and explored for analytical procedures recently [17]. It was discovered that both the deposition of Pb metal at negative potential followed by anodic stripping, and the deposition of PbO 2 at positive potential followed by cathodic stripping are enhanced in the presence of microwave activation.…”

Section: Introductionmentioning

confidence: 99%

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Microwave-Enhanced Anodic Stripping Detection of Lead in a River Sediment Sample. A Mercury-Free Procedure Employing a Boron-Doped Diamond Electrode

et al. 2001

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Microwave activation of electrochemical processes has recently been introduced as a novel technique for the enhancement and control of processes at the electrode‐solution interface and is employed here to improve the analytical detection of Pb2+. Instead of the conventional mercury‐based accumulation and stripping procedure, mercury‐free boron‐doped diamond electrodes are employed. The deposition and anodic stripping detection by square‐wave voltammetry of Pb2+ in a 0.1 M HNO3 solution is shown to be strongly enhanced by microwave activation at boron‐doped diamond electrode. The temperature at the electrode‐solution interface is calibrated with reversible redox couple Fe3+/Fe2+ (4 mM Fe3+, 4 mM Fe2+) in 0.1 M HNO3 and a standard addition procedure is developed for the sensitive detection of Pb2+ concentrations from 1 µM to 5 µM. The limit of detection by square‐wave voltammetry after 20 s deposition time was found to be 0.1 µM and 1.0 µM with microwave activation and without microwave activation, respectively. Then, the Pb content in a water sediment sample detected by anodic stripping voltammetry at boron‐doped diamond electrodes is shown to be in good agreement with two other independent analytical procedures based on ICP mass spectroscopy and on sono‐cathodic stripping voltammetry.

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Section: Instrumentationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Microwave-Enhanced Anodic Stripping Detection of Lead in a River Sediment Sample. A Mercury-Free Procedure Employing a Boron-Doped Diamond Electrode

et al. 2001

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“…Most studies to date explored the microwave effects at platinum electrodes. In one preliminary report, the microwave activation of electrochemical processes for the case of PbO 2 deposition and stripping at carbon and boron-doped diamond electrode has been reported [11].…”

Section: Introductionmentioning

confidence: 99%

Microwave Activation of Electrochemical Processes at Glassy Carbon and Boron‐Doped Diamond Electrodes

et al. 2005

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Voltammetric experiments under intense microwave field conditions have been carried out at a carbon microfiber electrode, an array of carbon microfiber electrodes, and at a boron-doped diamond electrode. For the reversible one electron redox systems Fe(CN) 3À=4À 6 and Ru(NH 3 ) 3þ=2þ 6 in aqueous KCl solution increased currents (up to 16 fold at a 33 mm diameter carbon microelectrode) and superheating (up to ca. 400 K at all types of electrodes) are observed. Electrodes with smaller diameter allow better signal enhancements to be achieved. From the missing effect of the supporting electrolyte concentration on the microwave enhanced currents, it can be concluded that effects observed at carbon electrodes (microwave absorbers) are due to the interaction of microwaves with the electrode material whereas for metal electrodes (microwave conductors) effects are dominated by the interaction of the microwaves with the aqueous dielectric. Short heat pulses can be applied by pulsing the microwave field and relatively fast temperature transients are observed for small electrodes. For the irreversible two electron oxidation of l-dopa in aqueous phosphate buffer, different types of effects are observed at glassy carbon and at boron-doped diamond. Arrays of carbon microfibers give the most reproducible and analytically useful current signal enhancements in the presence of microwaves.

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“…The technique has been further developed and effects explored for a wider range of electrochemical processes such as electro-analytical stripping [2,3], interfacial adsorption and deposition ]4], metal deposition [5,6], electron transfer and ECE-type electrochemical reactions [7], the oxidation of glucose [8], and has recently been employed for electrochemical processes in micellar solutions with highly insoluble redox systems [9 10]. Upon application of microwave radiation to the electrochemical system, the working electrode is acting as an "antenna" and self-focusing the microwave radiation occurs into a region within the diffusion layer at the electrode surface j solution interface.…”

Section: Introductionmentioning

confidence: 99%

Microwave Activation of Processes in Mesopores: The Thiourea Electrooxidation at Mesoporous Platinum

et al. 2006

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In situ microwave activation is applied to the electrochemical oxidation of thiourea at low surface area (polished polycrystalline) and at high surface area (electrodeposited mesoporous platinum coated) platinum microelectrodes. The one electron oxidation of thiourea to formamidine disulfide is monitored as a function of the different activation parameters. In the absence of microwaves (ambient temperature, low mass transport) increasing the surface area (roughness) increases the thiourea oxidation response predominantly due to adsorption effects. In the presence of high microwave intensities, high mass transport and thermal effects further increase the oxidation current at mesoporous platinum. The most effective thickness of the mesoporous platinum film for the thiourea oxidation process is estimated as 3 mm independent of electrode diameter, temperature, or mass transport effects.

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Microwave activation of electrochemical processes: enhanced PbO2 electrodeposition, stripping and electrocatalysis

Cited by 31 publications

References 0 publications

Microwave-Enhanced Anodic Stripping Detection of Lead in a River Sediment Sample. A Mercury-Free Procedure Employing a Boron-Doped Diamond Electrode

Microwave-Enhanced Anodic Stripping Detection of Lead in a River Sediment Sample. A Mercury-Free Procedure Employing a Boron-Doped Diamond Electrode

Microwave Activation of Electrochemical Processes at Glassy Carbon and Boron‐Doped Diamond Electrodes

Microwave Activation of Processes in Mesopores: The Thiourea Electrooxidation at Mesoporous Platinum

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