Oxygen reduction reaction measurements on platinum. Pdf an experimental study of mass transfer to an amalgamated copper rotating disc electrode has been employed to determine an empirical correlation. We present a thorough electrochemical study of the mechanism of borohydride oxidation on gold and platinum surfaces via cyclic voltammetry and rotating disk and ringdisk electrode voltammetry. Determining the behavior of the rotating disk electrode system 3 state, each uorine atom will accept one electron e whenever these are available and each ouride molecule will undergo the following reaction. The rde system is a valuable experimental tool because it allows us to study the effects that convection the transport of the reactants in. In order to avoid or reduce these problems, gloaguen et al.
Please read sections 1643 through 1655 for background information on. This electrode is amenable to rigorous theoretical. Determining the behavior of the rotating disk electrode system 5 is not too small in comparison to the size of the container. It consists of a central disc electrode and a concentric ring electrode. The autolab rrde is a lownoise rotating ring disk electrode that can be used to perform electrochemical measurements under controlled hydrodynamic conditions. Previous work performed on rotating disk electrode niu and cheng, 2008 demonstrated that, in the absence of sands, an accelerated fluid flow could enhance diffusion of oxygen towards the electrode surface, resulting in the al alloy oxidation. This movement of rotation leads to a very well defined solution flow pattern. Theoretical concepts and application of a rotating disk. The rotating ringdisc electrode allows the testing of end products and intermediates of electrochemical reactions.
Rotating diskelectrode aqueous electrolyte accelerated stress tests for pgm electrocatalystsupport durability evaluation doe durability working group 1042011. Many elements emit light in the visible region of the spectrum. Pdf analytical procedure for accurate comparison of. Rotating disk electroderotating ringdisk electrode.
The bas rde2 rotator is a miniature rotator system for use in constantrpm and hydrodynamic modulation rotating disk electrochemistry. A rotating disk electrode rde is a hydrodynamic working electrode used in a three electrode. Rotating disk electrode rotational speed gamry instruments. Characterization of highsurfacearea electrocatalysts using. Rotating disk electrode rde voltammetry has been touted as a simple means for benchmarking the oxygen reduction reaction orr activity of platinumbased electrocatalysts in proton exchange. The gamry instruments mobile app is a convenient way to find technical support articles, application notes, electronic versions of our instruments user manuals as well as news and events happening in the electrochemical research arena. The structure is rotated about an axis perpendicular to the surface of the disc electrode.
Rotating diskelectrode aqueous electrolyte accelerated stress tests for pgm. Rotating disk rde pine research instrumentation store. Rotating disk experiments are performed where defined mass transport to the sample electrode is desired. Testing oxygen reduction reaction activity with the. Overview of rotating disc electrode rde optical emission spectroscopy for inservice oil analysis 4 an important consideration when designing a spectrometer is the region of the spectrum where the wavelengths of interest occur.
Rotating disk electrode method request pdf researchgate. Oxygen reduction reaction measurements on platinum electrocatalysts utilizing rotating disk electrode technique i. An example of this type of experiment would be catalyst evaluation. Influence of the composition and preparation of the. Fundamentals of rotating disc and ringdisc electrode. While the bulk solution far away from the electrode remains wellstirred by the convection induced by rotation, the portion of the solution nearer to the electrode surface tends to rotate with the electrode. Rotating ring disk electrode rrde the autolab rrde is a lownoise rotating ring disk electrode that can be used to perform electrochemical measurements under controlled hydrodynamic conditions. However, in the presence of sands, the sand impingementresulting damage to the electrode dominates. Rotating disk electrode electrochemistry resources. The rotating disk electrode rde allows the user to control the velocity of the fluid. As the potential at the disk is swept from high to low values, the onset of orr gives rise to a negative cathodic signal that is observable at approximately 0. The rotating disc electrode rde is the classical hydrodynamic electroanalytical technique used to limit the diffusion layer thickness. The theory for the hydrodynamics at the rde 4042 assumes that the electrode is uniformly accessible and affords a precise and reproducible control of the convection and diffusion of reactant to the electrode. Rotating disk electrode rde voltammetry at glassy carbon electrodes in 300 to 500 l volumes has been shown in the literature by this laboratory and others.
Theoretical concepts and applications of a rotating disk electrode. The system allows a good controlling of the convection and diffusion. The laminar flow at a rotating disk electrode conveys a steady stream of material from the bulk solution to the electrode surface. Oxygen reduction reaction with the rotating ring disk. Oxygen reduction reaction with the rotating ring disk electrode page 2 of 3. The end of a cylinder, comprised of an electrode embedded in an inert material is placed in solution and rotated about the axis r 0 as shown in fig. A rotating ringdisc electrode rrde is a double working electrode used in hydrodynamic voltammetry, very similar to a rotating disk electrode rde. Figure 5 also shows the kouteckylevich analysis for, and the essentially identical slope demonstrates the 4electron reduction to water on, which agrees with previously reported rotating ringdisk electrode rrde measurements on.
Permanent disk electrodes disk electrode 5 mm diameter permanently sealed in teflon, 12 mm outside diameter shroud. Pdf mass transfer to amalgamated copper rotating disk electrode. View the article pdf and any associated supplements and figures for a period of 48 hours. The autolab rrde uses 2 identical frictionless mercury contacts for low noise measurements and can be used. This requires about 2 or 3 ml of sample depending on the exact cap being used. The rotating ring disk electrode figure 5, which the ring electrode is arranged concentrically with respect to the disk electrode, the product of the electrode reaction occurring at the disk electrode interface is transported to the periphery by the centrifugal force of rotation 14. A 7 mm diameter electrode with short stainless steel shaft provides for a miniature and concentric circle electrode system that is capable for highly accurate rotation and modulation even at radial modulation rates or wave forms. B solution flow pattern near the disk electrode surface x is the coordinate direction perpendicular to the disk electrode surface, r is the coordinate direction parallel to the disk surface, and. These working electrodes are used in electrochemical studies when investigating reaction mechanisms related to redox chemistry, among other chemical phenomena. Part mf9006 instruction manual rotating disk electrode. Theoretical concepts and application of a rotating disk electrode rde and rotating ring disk electrode concentrated summer course in electrochemistry, september, 2014 barilan university. Impact of impurities, measurement protocols and applied corrections kazuma shinozaki,a,b,c. The ring and disk electrode assembly provides the means to detect reaction intermediates in situ through collection experiments.
Levich koutecky levich electrochemistry application. The rotating disk electrode rde technique is the most commonly used halfcell technique to screen the orr activity of novel pemfc catalysts synthesized on the mgscale as well as to study the orr kinetics on bulk catalyst surfaces and nanoparticle catalysts. Rotating disc electrode an overview sciencedirect topics. Astm d6595 17 standard test method for determination of. This paper verifies the theoretical concepts and shows one application of a rotating disk electrode rde. Request pdf rotating disk electroderotating ringdisk electrode generally, electrochemical techniques involve the application of potential current to an electrode and the measurement of the. This system used in electrochemical studies when investigating reaction mechanisms related to redox chemistry and other chemical phenomena. It is used to capture the product at a constant potential. The ring and disc electrode assembly provides the means to detect reaction intermediates in situ through collection experiments. Theoretical concepts and applications of a rotating disk. Performing the procedure with power on could result in serious or lethal electrical shock.
The electrode is rotated about its vertical axis figure 11. The disk s rotation is usually described in terms of angular velocity. Rotating disk electrode voltammetry applied to the. Rrde3a is a constant rotation system for use in hydrodynamic modulation rotating ring disk electrochemistry. Background pemfc mea thinfilm rde trends of activity and durability in rotating disc electrode rde studies can be used to predict trends in proton exchange membrane fuel cells pemfcs. The renewal of the solution at a disk electrode occurs thanks to an ascending movement of the solution perpendicularly to the electrode. Request pdf rotating disk electrode method in this chapter, to give readers the knowledge how to appropriately use rotating disk electrode rde in their. The rotating disk electrode rde was first examined theoretically by veniamin levich in the early 1950s. Students use the redox couple fecn63fecn64 to check the model and theoretical concepts that describe the rde behavior. The objective of this laboratory exercise is to demonstrate the application of rotating disk voltammetry for the determination of diffusion coefficients and heterogeneous electron transfer rate constants.
The rotating ringdisk electrochemistry of the copperii. Influence of the composition and preparation of the rotating disk electrode on the performance of mesoporous electrocatalysts in the alkaline oxygen reduction reaction. Voltammetry at the rotating diskelectrode rde is a widely used method for the study of electrode processes at solid electrodes. The steadystate mass transport conditions of the species involved in the redox reactions are then known 1,2. Rotating electrode system the systems approach to rotating electrodes the princeton applied research model 616 electrode rotator is a high precision, low mass. A rotating disk electrode rde is a hydrodynamic working electrode used in a three electrode system. Oxygen reduction reaction activity measurement for fuel. Electrochemistry rotating disk electrode rde author. Rde2 june 2000 part mf9006 instruction manual rotating disk electrode bioanalytical systems, inc.
The sample is placed in a sample cap, the disc is partially immersed in the oil sample and the disc rotates as the burn proceeds figure 3. This is a powerful instrument employed in electrochemistry, capable of controlling the transport regime of electroactive species toward the electrode. We have paid particularly close attention to the number of electrons transferred from a theoretical maximum of 8e. Please complete the following form and we will email a link to your. Rotating disk electrode voltammetric measurements of. With all parameters held constant in this equation, rdev can be. Both electrodes lie within one plane on the abutting face of a cylinder and are connected mechanically by a thin, electric isolating coat. The electrode rotates during experiments inducing a flux of analyte to the electrode. Rotating disk electrode voltammetry is a very commonly used experimental method. Rotating diskelectrode aqueous electrolyte accelerated. The rotating disk electrode rde is designed to enhance the mass transport to the electrode through convection, thus decreasing the effect of diffusion. Overview of rotating disc electrode rde optical emission spectroscopy for inservice oil analysis 4 to be mounted in a vacuum chamber or otherwise filled with gas transparent to fuv light, so the emitted light can reach the grating, be diffracted, and then be detected at the focal curve. Probing fuel cell electrocatalyst properties with rotating.
386 964 128 795 979 990 632 246 1467 642 698 77 1315 254 1470 412 1186 186 611 941 906 478 1349 732 1213 917 118 694 1080 196 1226 1142