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Cyclic Voltammetry - Science method

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  • In electrochemical reduction of CO2 what is the purpose of the following method?
  • 1. Linear sweep voltammetry
  • 2. Cyclic voltammetry
  • 3. Chronoamperometry
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Nazifa,
After you do LSV/CV analysis you will know the potentials that the reaction starts. Hold the voltage more negative than that using bulk electrolysis for some set time (such as 30 min or 1 h) and then sample the headspace and solution and analyze for products. Check out papers similar to what you want to do to see what voltages and times, etc they used. The size of your working electrode will affect your current and the total coulombs passed.
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These are the voltammograms for the electrocatalyst in 0.6M NaCl solution. I have to find out whether the reactions happening are oxygen evolution or chlorine evolution reaction. How to analyze these graphs and come to a conclusion?
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Hello.
What are the conditions of your experiments: pH?, reference electrode? What are the experimental differences between the first and second voltammogram you have shown?
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If current intensity is an additive property in voltammograms, then is the current intensity that is recorded at a potential greater than that of water oxidation a result of the oxidation of all species that oxidize at that potential? That is, if we have that water oxidation starts at 1.23 V and a species A is oxidized at 1.30 V, then the current measured at 1.30 V contains a contribution from water and species A?
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Fourier transformed alternating current voltammetry might be helpful. See an example
Lee CY, Guo SX, Murphy AF, McCormac T, Zhang J, Bond AM, Zhu G, Hill CL, Geletii YV. Detailed electrochemical studies of the tetraruthenium polyoxometalate water oxidation catalyst in acidic media: identification of an extended oxidation series using Fourier transformed alternating current voltammetry. Inorg Chem. 2012 Nov 5;51(21):11521-32. doi: 10.1021/ic301370y. Epub 2012 Oct 23. PMID: 23092201.
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I am working on Cyclic voltammetry and what is the importance of distance between three-electrode (reference electrode of silver/silver chloride electrodes (Ag/AgCl, a counter electrode of platinum wire and a glassy carbon electrode) and their dimensions.
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Ideally, you would have the reference electrode as close as possible to the working electrode to reduce iR drop. Additionally, the surface area of the counter electrode should be much larger (at least twice as large, but more is better) than the working electrode, but can be placed anywhere as long as electrical contact is maintained.
Chapter 3 of Eliaz and Gileadi from Physical Electrochemistry is helpful
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Hi dear friends
I'm challenged with a problem. I investigated scan rate effects for an electrochemical sensor. I found that the behavior of current with scan rate and the square root of scan rate is linear for them simultaneously (R2 for both approximately 0.99). My first question is, can I report both processes? My second question is for kinetic investigation, which equation is proper for calculating alpha(electron transfer coefficient) and n(number of electrons)?
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I have measured the electrochemical behavior of the N719 dye+TiO2 and the carbon quantum dot (CQD)+N719+TiO2 dye loaded counter electrode using cyclic voltammetry test. I have observed the flat shape CV curve in cathodic sweep. The oxidation peak failed to be observed. So, what are the possible reasons behind this? The curve attached in the file.
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Dear Ramhari Paneru,
if you want to see, for the beginning, good CV responses of the CQD and Dye you indeed need to do the CV measurements in their solution, which of course should contain a supporting electrolyte. But first, for clarity, do these measurements separately per each substance to see their electrochemical behavior in your solution. Only after you can do their joint solution and do their joint CV characterization at different their concentrations. If their redox peaks positions will change as compared with their separate solution, this can testify to their specific interactions which, in turn can affect their orbital levels. Hopefully this can help.
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Like I am doing CV for porphyrins and even for TPP I get good two one electron reduction peaks in DCM at 0.5 V/s but at low scan rate it is difficult.What could be the possible reason behind it?
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Dear Nivedita,
The peak height is directly proportional to the square root of the scan rate. Hence higher the scan rate higher the peak. Hence you may not see a visible peak at 0.1V/s
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I ran cyclic voltammetry for Cd in PBS on aptamer-modified electrode vs SCE scanned from -0.6 V to 0.2 V at 100 mV/s.
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Thank you for your suggestion, Sir Javier. So, what potential window can you suggest?
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Hi everyone
I'm looking for Laviron's equation for adsorption controlled process, could anyone help me?
thanks
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This image contains Laviron's equation for adsorption-controlled process.
You can read the article titled: "Trace analysis of Ponceau 4R in soft drinks using differential pulse stripping voltammetry at SWCNTs composite electrodes based on PEDOT:PSS derivatives"
You can also follow the last question I asked.
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If we do the cyclic voltammetry for an electronic material, what applications of these materials are possible?
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You may look at the applications for molecular electronics, supercapacitors, batteries, and bio-sensing.
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What material is proper for current collector for KOH electrolyte three electrode test system? Al, Ni Or what?
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Dear Dr. Ebrahimi
Aluminium is not proper for alkaline media because it dissolves in it and forming alkaline aluminate.. Ni may be proper for that l, but it's better to use Or current collector electrode
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I have little experience in supercapacitor testing. I am using Ni-foam as working electrode, Pt metal as counter electrode, 6 M KOH as electrolyte, and SCE as reference electrode.
In literature, I commonly find -1V to 0V voltage window is used for 6 M KOH electrolyte (but mostly vs Hg/HgO).
When I am testing my material in this voltage window, there is oxidation peak at around -0.2V for bare Ni-foam that affects my material CV (Image attached). (Redox peaks are also there in positive voltage window for bare Ni-foam)
Is there any suitable voltage window for SCE for carbon material testing in alkaline solution?
Expert recommendations will be highly appreciated.
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Hi Muhammad, for an alkaline environment Hg/HgO is best. I have see people using Ag/AgCl and it works also, as long as the measurements are quick. Make sure the references are calibrated after the uses
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I conducted CV analysis on my electrodes to be used in a microbial electrosynthesis cell and cant find a simple comparison of different materials. The CV analysis was completed in a fixed potential range from -1 to 1 at a scan rate of 20 mV/s. Could anyone help me figure out what the difference in between the graphs indicates? thank you
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Carl Pichon read this paper, it may be useful to you.
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as I know the cyclic voltammetry was using three electrodes, but how do cv with coin cells?
what is the potential window?
what is the reference potential and electrode?
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you can try to measure 'typical' CV with Li-ion coin cells[1] (in a proper V-window[2]) provided the (critical) condition for a very low V-scan rate (0.1 mV/s, or even lower) value.
2. see Figure(s) 3, in: 'Fluorinated Electrolytes for Li-Ion Batteries...'
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We have used the thin film Cyclic Voltametery method but the film starts to peel off during the scanning. We also tried the UPS but results show a lot of noise. Please suggest any alternative......
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I am trying to detect the hexavalent chromium by using cyclic voltammetry, first I tried to see at varying concentrations at ppm level and then tried with ppb level. I was able to achieve a gradual increase in current at ppm level with no significant difference in peak potential. But at ppb level, the current generated is the same but with a gradual change in peak potential. So, what is the reason for this?
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Gautami Kj If you can show images of your voltammograms it would be easy to understand what can be happening. The potential peak at ppb is the same than using concentrations of Cr(VI) at ppm levels?
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In case of Randles sevick eqn used for diffusion coefficient of Li ions in Li-ion batteries, what will be the concentration? Will it be the concentration of Li ions in the electrolyte of at electrode? How can we calculate concetration?
In this paper concentration of Li ions is given 23 mol per dm3. How have they calculated?
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Dear all, the Randles-Sevcik equation is used to calculate the diffusion coefficient of a species to the electrode where it reacts. The concentration is the bulk concentration.
For more information please see my article on CV and the associated YouTube videos:
Also if you are interested in estimating the diffusion coefficient of inserted species in the insertion material, please find some guidelines here:
The best method is to use EIS with the proper equivalent circuit.
Let me know if you need more information or details.
Best regards,
Nicolas
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How Cyclic Voltammetry can be performed as in the amount of solutions or which reference electrode to be used and the procedure to be followed ?
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Nidhi Singh the general procedure is almost the same for all voltammetry methods:
1. Prepare the sample in the supporting electrolyte at concentrations that are appropriate for your analyte and in the appropriate type of supporting electrolyte.
2. Define the region of potentials (for example: 0 - 800 mv) in which you will record the voltammograms.
3. Define the speed of sweeps and the number of cycles.
4. Record the voltammograms of the supporting electrolyte without anlyte, this will allow you to create a baseline for residual current evaluation.
4. Record the voltammograms of the sample.
5. Determine the peak current as well as peak potential.
The calomel electrode is sufficient for almost all voltammetric experiments.
The sample amount (solution amount) is defined by the volume of the cell, In most experiments it is only necessary that the electrodes are covered by the solution.
Aspects as the iR drop are defined by the electrode arrangement (distance between them), the support electrolyte and its concentration.
Voltammetric methods usually present many variables that influence the voltammograms and parameters such as peak current, peak potential, average potential and others. Therefore, it is recommended that if you do not have experience, someone guides your experimental work.
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There are two samples for one is showing something but for other random graph is showing scan rate 20 to 100 mv/ sec in 0.1 kno3
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This is just showing an ohmic response. You can calculate the resistance from the graph and see if it is a plausible value for your electrolyte. If it is too high, you probably have poor connections at your electrode. This latter seems the most likely, since almost every metal electrode would ordinarily show water oxidation or oxide formation, or usually both, at potentials as positive as 1.5 V to Ag/AgCl. Also, the hysteresis is low relative to the current again consistent with a high resistance in series with the working electrode. What peaks are you expecting? Is there an electroactive species that you expect to be oxidised in this potential range?
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I have measured the CV of metal oxide based supercapacitor cathode materials, My CV curve is not a closed loop rather there is a small shift. what are the possible reasons of this?
is this all right or a closed curve is required?
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We are getting same issue we also try more cycle
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I did Cyclic voltammetry and the result is plotted as E vs Log ABS I. Can this graph be analyzed as CPDP or the method should be different? my field is not electrochemistry so I am so confused.
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Mandana Ghasemiansafaei the typical CPDP graphs are E vs. Log (current density). Current density is calculated as i/A, where i is the current and A is the area of the electrode. You can also plot a graph of E vs. Current Density if you do not want to use the log.
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I am trying to detect Calcium in PBS. I am use an Ag/AgCl reference electrode, glassy carbon working electrode and platinum wire counter electrode. I am using PBS pH 8.5 with 0.5 MgCl2 as the electrolyte solution.
I did a background scan of PBS, then added 1mM CaCl2 to the PBS. I was able to see a clear reduction peak (see attached picture) at -0.110V. Since The PBS + MgCl2 already contains Chlorine, I assumed that this peak was due to the calcium.
Then I tried to see the difference between different additions of CaCl2 to PBS (333uM, 666uM and 1mM) using CV. Sometimes I saw a reduction peak at the expected potential (-0.110V) and other times I did not - independedent of the addition of CaCl2 to the solution. For instance, in one experiment, I did a CV with 1mM CaCl2 added, and did not see the peak, I cleaned the electrode, repeated the measurement, and afterwards I did see it.
I have cleaned the electrode with alumina between each measurement, made sure there are no bubbles attached to either the working or counter electrode.
Can anyone suggest how I can troubleshoot this experiment so that I can get reproducible measurements?
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Nico Crudele record voltammograms out of PBS, and you maybe will know if your problem is related with the PBS medium.
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How can one find the CMC of the binary system using the diffusion coefficient from cyclic voltammetry? And also, explain the term "Probe Diffusion Coefficient" and how to calculate it?
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Hello Ravi
Please go through the following attached papers. one is very old may be you will find them beneficial and get your answer out of it. These papers are well explaining the critical micelle concentration determination along with probe diffusion coefficient calculations.
Hope so they will work for you.
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How to calculate the Ragone Plot (energy density&power density) with cyclic voltammetry and galvanostatic discharge-charge. the algorithm is the same with Double Layer Capacitors (EDLCs), supercapacitors the symmetric cell represents.
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Thank you very much, Dr. Debika Gogoi
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Can I determine the presence and concentration of iron nanoparticles in an aqueous solution using techniques such as cyclic voltammetry or square wave voltammetry?
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@ Daniel, I don't think the concentration of iron nanoparticles you can measure by using cyclic voltammetry technique because cyclic voltammetry can only be used to measure a number of electrochemical properties (viz. reversibility of a reaction, reduction potential, electron transfer kinetics etc.) about a material, not concentration.
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whie working on CV on iron we get peaks in which two peaks (one oxidizing-anodic and one reducing-cathodic ) peak which continues to grow on while we increase the number of scanning. why is it so? whats the reason behind this? i am referring to peak 3 and 4 in attached picture.
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in order to help you with this problem, i like to know in what form are the iron ?
because, if is a powder, this behavior can be explain like a constant oxidation reduction of this powder which accumulates in its oxidized state and each cycle increases the amount.
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Hello everybody,
I would like to ask you about my cyclic voltammogram. It looks weird because of special 'triangle shaped peaks". Have you seen this graph before or you have some suggestion where the problem is? Cathode - Nasicon +PVDF +NMP +C on copper foil, cathode - sodium foil or sodium metatitanate foil on copper foil, separator and typical electrolyte for sodium ion batter. Assembling battery and setting of software were checked by my older colleague who has good results.
Thank you!
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This is due to some parameters like poor diffusion of Na-ion, the thickness of electrodes, scan rate, porosity, and thickness of the separator.
I would recommend you measure the electrochemical impedance spectroscopy. for better understanding.
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Hello everyone, 
I am trying to do a 4 point measurement to calculate the sheet resistance of a graphene layer by the van der Pauw method. I am trying to set it up with 1 or 2 potentiostats. I need to induce either a constant current or voltage in 2 points and read the resulting resistance between  2 other points. I am doing this with the Ivium software. Any suggestions on how to do this preferably on a single potentiostat?  (Note: I could do this type of measurements with 2 multimeters but the readings wouldn't be very accurate)
All suggestions will be very appretiated. 
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Provide/pass a small constant current (among 2 points) e.g. in Galvanostatic mode (not in Potentiostatic mode), and read the resulting Voltage (resistance, R1VdP) between the 2 other points.
Repeat 'the same', as the above measurement(s), by (inter)changing the (4-)contacts, according to the specs found in the Van der Pauw method[1].
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Hello
I'm doing CV measurements for a standard JARI CELL and I am trying to obtain some CV's but I'm not getting good curves. There is lot of noise in the curve.
I then tried using the dummy cell but the results are the same. Has anybody else experienced this?
I'd really appreciate your suggestions.
Thanks
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Okay. Thank you Dennis . I really appreciate this.
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I have calculated the portion of diffusion-controlled and capacitive-controlled current using power-law relationship from Cylic Voltammetry data of battery electrode material using five different scan rates. However, I am looking to plot the area of capacitive contribution inside my CV curve area, or in other word, combine both CV curve and its capacitive contribution. Thank you.
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Did you find the answer of this question Dedy Setiawan ?
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Hello, I'm studying about planar supercapacitor that patterned like comb.
I have a question how I can calculate the areal capacitance (Ca) from Cyclic voltammetry in two and three electrode system, respectively.
I read many paper and some says ;
Ca = (absolute area of enclosed CV curve)/ 2 * (scan rate)*(potential window)*(electrode area) (1)
and the other says
Ca = (absolute area of enclosed CV curve)/ (scan rate)*(potential window)*(electrode area) (2)
what is different between them?
I've just seen that, in two electrode system,
Ccell = Cworking electrode/2
is it related the factor 2 in denominator of equation 1?
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Hello Hyeonwoo Kim ,
Here is a paper (you can also read the references of the paper)
Hope it helps.
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Greetings!
I have prepared a several UME exemplars for the project I am working on. These were prepared from an etched Au wire (d = 0.25 mm) placed inside a PTFE tubing, with wire protruding from the tubing cca 3 mm on etched side. This setup was then sealed in a polyethylene coating in a way that only the very apex of the etched Au tip is exposed.
After visual checking the UMEs under the optical microscope, I wanted to evaluate them with cyclic voltammmetry. My plan was to check the CV response in a solution of 1 mM K4[Fe(CN)6] in 0.1 M Na2SO4 aqueous electrolyte. I prepared the solution and assembled the cell. Used the Ag/AgCl as my reference electrode and Au wire (d = 0.5mm) as the counter electrode. Counter electrode was rinsed with acetone and distilled water, flame annealed and then let cool in an argon atmosphere. Solution was sparged with argon gas for cca 30 mins before performing the CV.
Test run with Au macroelectrode at 25 mV/s looked fine in my opinion (see Fig. 1), so I proceeded with my UME exemplars. None of them showed the expected steady-state voltammetric response, but rather a highly distorted one with one or more crossovers during the cycle. Black lines on Figs 2-4 show the initial voltammetric responses of selected three different UMEs at 10 mV/s. Voltammograms of other exemplars at the same scan rate more or less resemble one of the three shapes presented in Figs 2-4. Additional electrochemical cleaning, performed by CV polarization of the UME/electrolyte interface with the cathodic limit set to -1 V vs. Ag/AgCl at 10 mV/s, had no improving effect on the voltammogram shape. Red lines in Figs 2-4 show the voltammetric response of presented UME exemplars after cleaning.
Any idea why those voltammograms look so terrible and far away from expected steady-state shape? Could be an effect of electrolyte leakage caused by imperfect seal between Au wire and polyethylene insulation, or due to some microcracks development? Or is it the effect of capacitive contribution to measured current? Or perhaps my UME design is flawed?
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The signal you're measuring for the UMEs looks like it has a very periodic oscillation, to me that suggests external electrical noise. There are a few things I can think of that may help. If you haven't already done so I would suggest reducing the current range you are working at on moving from the macro electrode to the UME. For the macro electrode you will be ok working with something like 10-100 uA/V whereas for your UME you will probably want something more like 1-100 nA/V to get the best signal. You may also need to change the bandwidth option you are using, what works fine for a macro electrode is not always ok for a UME. Finally if you can't remove the oscillation with these sorts of filters, you may need to use a Faraday cage when working with the UME.
This article and the links within might help: https://www.biologic.net/topics/how-to-get-quality-measurements/
I hope this helps!
Samantha
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Please suggest me to how to perform cyclic voltammetry, when the composition of electrolyte is unknown how can we use reference electrode in that type of fuel cell setup.
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You can get details in paper
Harnisch, F., & Freguia, S. (2012). A basic tutorial on cyclic voltammetry for the investigation of electroactive microbial biofilms. Chemistry–An Asian Journal, 7(3), 466-475.
Even I can help you out for CV measurement & analysis -MFC
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Hello. I am running cyclic voltammetry with bare gold electrode. The voltammograms are very different from that in literature. Please see attached file for the image. What could be done? Thank you.
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re-check the solution you made and plug the three electrodes.as I see in the image, you have a problem with the electrical connection.
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i want to know what is the process going on in the electrolyte during the cyclic voltammetry of Nickel cobalt alloy electrode due to which these oxidation and reduction peaks of Nickel and Cobalt were seen?
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Dear Abhinav Maurya,
Can you tell us more about the elecrolyte you use and the oxidation/reduction potentials ?
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Hello everyone!
I'm working on the electrosynthesis of polymer film based on metallo-porphyrin (in fig 1). For the polymer synthesis, I'm performing cyclic voltammetry using a solution prepared in ACN with TBAP as supporting electrolyte.
The resulting voltammogram is shown in figure 2.
From this, it seems that the polymer is conductive with an increase in the current cycle by cycle.
I'm trying to characterize the polymer in a solution of a redox probe (e.g. [Fe(CN)6] 3-/4- prepared in water with KCl as supporting electrolyte ), by cyclic voltammetry. The comparison between the bare electrode and the functionalized electrode with polymer shows a dramatical decrease in current after the electropolymerizationpolymerization.
How is it possible to describe this different "behaviour" of the film?
Any useful papers?
Thank you!
Tiziano
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Dear Nicolas Murer, thank you very much for your reply.
I'm showing you the Nyquist plot for the bare electrode and the data fitting with a Randles circuit. It seems that there is a Warburg component in the impedance spectrum. Is it an useful information?
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Hello
My question is about initial charging and formation On small and laboratory scale,
With two cells and H2SO4 electrolyte.
How many stages are required for initial charging?
It was mentioned in an article that :"The formation process is based on three successive charging steps: charging at a rate of 0.1 C for 3 h, at a rate of 0.14 C for 24 h and again at a rate of 0.1 C for another 3h"
But when we tested this formation, our electrochemical tests like cyclic voltammetry had a problem.
We have a power supply. For applying formation, we inflate the voltage to infinite and then change the current.
It is told that each 15 grams positive active material in a lead acid battery requires 1Ah capacity.
So at the first time we weigh positive active material and then calculate capacity. It is called "C".
According to the article that I mentioned, we start formation: first stage 0.1 C for 3h, 0.14 C for 24 h and again 0.1 C rate for 3h.
Actually I don't know where our problem is.
Articles often low  mentioned about initial charging and formation of lead acid batteries do not explain well
Thank you
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Also as you know maybe your starting material is tribasic lead sulfate or lead sulfate according to that not. All current is used for making lead dioxide there is also oxygen evolution reaction (0.1C*3+0.14C*24+0.1C*3)~4time the Capac
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In cyclic voltammetry application (as per circuit design given in image), the voltage difference between reference electrode (RE) and working electrode (WE) will be constant.
As per REDOX process (Reduction & Oxidation), the current will flow between counter and working electrode.
To maintain the constant voltage between RE & WE, the circuit must be close loop.
We have used I to V convertor, to convert the working electrode's current into voltage.
I have prepared attached circuit but not getting proper output.
What can be the issue in circuit. Please suggest.
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I recommend using Micro-Cap (http://www.spectrum-soft.com/download/download.shtm). All EE's at Emerson used Micro-cap, even though it cost $4,000 each. There are no other electronic SPICE modeling programs even close to Micro-Cap capability.
Micro-Cap is now free. Andy Thompson, owner of Spectrum Software, has retired.
Micro-Cap does worst case analysis --- changing the tolerances of components --- changing the temperature --- etc. And it is easy to use.
I have used Micro-Cap for all of my electronic designs since 2001. When I tested prototypes, they worked exactly as the model predicted.
The website --- https://NDAcademy.FoxPing.com/ --- 2.8 Electronic Cascade RC Filters --- and --- 7.2 Electronic SPICE Models --- provide examples.
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I use 1M LiTFSI, 0.01M Li-BP in DOL DME solution to observe redox peak of LiBP.
But it shows only anodic peak and not cathodic peak, how can I solve it??
In this CV, I used WE-Sus foil. CE- Li foil, and two electrode system and scan rate is 50 mV /s.
Many papers say its cathodic peak is located around 0.7 V in similar conditions.
I attached the graph.
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I think scan rate is very high. In general, for Li-ion battery case they go very very slow scan rate (like 1mV/s or less) as Li-ion diffusion is very slow.
Regards,
Bapi
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I am using Pt wire as a quasi reference and counter electrode (separate), and glassy carbon as a working electrode. I am getting this unusual reversible peak at between -1.5 and -1 V see attached the CV.
There were no electroactive species introduced in the electrolyte. I tried several times with various reference (Ag wire, Pt wire) and working (Au, GC, Pt), still, the peak remains there with a slight change in potential.
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Dipak Shinde You haven't removed oxygen from the cell enough. Oxygen reduction is quasi-reversible on CV
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In the case of exploring activated carbon based coin cell for supercapacitor, through my readings, it will be based on two-electrode system and the assembly is similar like li-ion battery.
However, how does the equipment setup to test the electrochemical performance (ie CV, GCD)? Will it still be the same as other battery testing? Also, what are the electrolytes suitable? (should it be organic / aqueous) ?
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You can use aqueous electrolyte ( eg: 3M KOH solution in DI) or solid state electrolyte (eg: PVA/KOH). In case of connection Wei Yan explained clearly.
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I don't mean low scan rate and high scan rate capacitance value being low or high. I want to ask these types of questions? How are the reactions affected by the scanning rate for 1000 cycles in cyclic voltammetry? Why is only 50 mV/s speed used for 1000 cycles? but for 5 cycles, for example, 2, 5, 10,30, and 50 mV/s speeds are used?
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When running a CV of one of my ligands, I see a return peak, however, there's a crossing in the curve. I was wondering what this could mean for my compound? Can this still be considered as something reversible, or is there a change happening to the compound? CVs are run in acetonitrile with NBu4PF6 as electrolyte, Pt work- and counter electrode, silver reference.
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Hello Sadaf Shakeel ,
If there is any adsorbed species in your electrode during forward scan, it may show peak(s) in reverse scan specially in slow scan rate. Compared with fast scan rate, if scan rate is slow, the adsorbed species get more time to be oxidized or reduced depending on its redox potential. Sometimes fast scan rate does not give enough time to occur this reaction in reverse scan.
You also may notice that, in multistep reaction, if scan rate is slow, sometimes we get two or three peaks. But if scan rate is too fast, number of peaks reduces.
Thank you.
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I have updated my manuscript but its the third time the reviewer send me this comment again.
What are the probable redox reaction during cyclic voltammetry?
Could anyone guide me on this, please
Thanks, A lot in advance for your precious time.
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Dear all, please have a look at the following link and the attached file. My Regards
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I want to perform CV for some sensitive complexes in inert conditions also at low temp. Can anyone suggest to me how to perform this or shall I need some sophisticated instrument facility?
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Aniruddha Sarkar You should work in a glove box. If not, you should prepare the sample in argon, pour the solution into the argon cell, and take the CV in a stream of argon.
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I've attached the image .
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First, increase the window potential based on the solvent used, then run a blank to check that your electrode configuration is okay with the electrolyte used. Just post this first so that we can check and then if it is okay, one can add polyoxometalate and check if it is redox-active in that potential window?
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I am trying to run cyclic voltammetry experiments on a modified electrode. The literature shows distinct peaks for the analytes (pesticides, phenols) using glassy carbon electrode(GCE) as working electrode. I am able to get the peak signal on GCE but not on the modified electrode. What could be the possible reasons?
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with great pleasure my dear
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When measuring the CV of a metal complex, I see an irreversible oxidation peak. We are interested in the amount of electrons that are involved in this oxidation event. How can one determine if the irreversible peak is the result of a one or a two electron reaction?
I added an image of the CV. I believe that using Laviron's equation is not suitable here because we are not investigating an adsorption reaction, everything in our system is homogeneous.
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Dear Francis Bru ,
if you plot the peak current as a function the square root of the scan rate, you could get the number of electrons involved in the reaction knowing the diffusion coefficient of the electroactive species, the initial concentration and the symmetry factor.
You can find more details in p. 4 of the following application note:
The note uses the cyclic voltammetry simulation tool of EC-Lab. A demo version can be found here:
Let me know if this helps,
Best regards,
Nicolas
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it is a while that I am working on printing carbon electrodes for the detection of a variety of metabolites in blood. I have a problem with the inconsistency of electrode signals while doing chronoamperometry or cyclic voltammetry in 5 mM potassium ferricyanide/ 1 M KCl. there is around 16% to 36% coefficient of variation in cathodic peak signals of cyclic voltammetry and Area under the curve of the chronoamperometric diagram, I have a range of possibilities some of them are as follows: 1- cleanness of the area: which I did not print in a clean area. 2-electrode printing quality or 3-printing unevenness across printed sheets.
From what you know, which of these factors contribute more to the electrode signal variation?
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Cualquier factor que modifique la superficie del electrodo afecta la señal medida (repetibilidad y reproducibilidad). Usted debe estandarizar eficientemente las condiciones de impresión de forma tal que obtenga una superficie perfectamente pulida y homogénea.
Luego debe seleccionar adecuadamente por voltamperometría la ventana de potencial de trabajo así como el electrolito de transporte y su concentración óptima (probar con nitrato de potasio 0.1M), generalmente bajas concentraciones del electrolito ofrecen mejores resultados en los electrodos impresos. Luego debe seleccionar por cronoamperometría el intervalo de tiempo de medición de la señal en la cual la corriente medida tenga su mayor valor estable durante un tiempo más largo. Medición de corrientes pequeñas conducen a una disminución de la sensibilidad y corrientes de medición alta pero inestable conducen a una disminución de la repetibilidad.
En resumen la calidad de las señal obtenida dependen de las características de la superficie de impresión del electrodo y de las condiciones de trabajo ( pH, temperatura, ventana de electroactividad, potencial de media onda, electrolito de transporte, agitación y tiempo de medición de la corriente).
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Hi, we would like to measure the reduction potential of an enzyme. Can this be done via potentiometric titration? Our lab does not have cyclic voltammetry.
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Did you think to use ORP electrode for this purpose. it is a cheap and easy way that we use commonly in microbiology and food research to determine the oxidoreduction potential of the medium.
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It is happening with me and peak has shifted from 0.2 to 0.9v.
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hello,
this phenomenon is due to nucleation and growth deposition mechanism
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Good morning,
the research group I work for bought an Electrasyn. We have carried out some first experiments in cyclic voltammetry, however, we get bad results and for this, I am looking for advice. The reference electrode was filled with a 3M solution of KCl, and we use a concentration of the supporting electrolyte approximately 100 times higher than the substrate. As working electrode we use the GC (coated with a plastic polymer except for the tip) provided in the CV package and as counter we use the Pt electrode always present in the kit. With a swipe of 100 mV / s then we proceed with the experiment. the curve we get however turns out to be horrible and knurled. do you have any suggestions?
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Can we see a phase change in the cyclic voltammetry plot of a faradaic reaction for Supercapacitor, If yes please tell me how?
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Actually in battery and capacitors normally, redox (Ox/Red) reaction occur without change of its crystal structure. Therefore, i suggest you to look change of oxidation state rather phase change through CV analysis. The phase change could be checked via different numerous characterization tools.........
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Hello everyone, I ran a CV and EIS technique for a 0.1 M Vanadium sulphate dissolve in 2 M H2SO4 as analyte using a three-electrode setup consisting of Glassy carbon (3 mm dia) as WE, Ag/Agcl as RE and Pt mesh (2 cm * 2 cm) as CE. OCV corresponds to 0.66 V
When I ran the CV at a scan rate of 20, 50 and 100 mV/s, there exists a huge potential difference (1 - 0.6 V) between the two peaks, as well both peaks looks highly unsymmetrical. When the number of cycles is increased the potential differences get reduced up to 0.6 V but the unsymmetric nature of peaks doesn't show much difference. Please find the attachments
Also, when I ran EIS (potential at OCV, Amplitude of 10 mV, Frequency from 100 kHz to 10 mHz), I obtained charge transfer resistance of 65000 ohm (Literature value show resistance of less than 100 ohms). Please find the attachments.
For VOSO4 the oxidation has a huge peak while reduction peaks are very small, when I ran with V2O5, the reduction has a huge peak while oxidation peaks are very small. When I ran with half of VOSO4 and V2O5 both the peak look symmetrical. In all three cases, the potential difference is in the range of (1 - 0.6 V)
In a three-electrode setup, electrolyte and working electrodes are the performance influencing thing. I have bought vanadium sulphate from Alfa Aesar which ruled out any fault in the electrolyte, which makes me to think about the working electrode. It's a newly bought electrode from Admiral instruments. I polished my Working electrode between the runs and also I have done ohmic drop compensation. Nothing works!
What could have gone wrong? I am having a very hard time figuring out these things. Any help regarding the proper diagnosis of the fault and how to rectify those will be much helpful.
Thank you.
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The concentration 0.1 M VOSO4 is too high for CV, use around 1 mM
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I have synthesized NiCo2S4 using the exact same procedure in papers, with molarity in the ratio 1:2:4. The CV is ok, but I'm not getting the GCD graph. The discharging is very fast, like in milliseconds. If I try with a much lower current density it will never reach the upper cutoff voltage. I tried making different nanocomposites but I could never get GCD. I attach the CV graph for NCS at 20mV/S in 1M KOH solution.
I'm stuck with this problem for a very long time and don't know what to do. I will be grateful if someone could guide me through this.
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Hi Nithin,
Your CV behavior resembles a resistor rather than a capacitor. Even at 20 mVps scan rate, the current is too low (microAmps).
Moreover, the area occupied by CV loop is too small which indicates your material isn't reacting with electrolyte ions much.
You can use different ways to make it better but it's difficult to say since I don't know how how you prepared the electrode? Can you send the reference which you mentioned earlier for making the material.
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CV is the rapid technique and spectrophotometer method we are going to use different radicals like DPPH, ABTS, Fe3+ etc., which one is the most sensitive method to determine the antioxidant activity of biological extracts like fungal metabolites, Pigments etc.,
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Hello everyone! I have a problem while doing cyclic voltammetry.
I use ITO glass as the working electrode (my sample coated on it), Pt wire as counter electrode, and Ag/AgCl reference electrode.
Electrolyte solution was 0.1 M tetrabutylammonium hexafluorophosphate in dry acetonitrile.
I provided a blank test in the beginning using a washed clear ITO glass, sweeping potential was set from -2 V to 2 V, and I set the three loops for the test. However, ITO glass color changed gradually from yellow to brown (only soaked region), this color change was irreversible.
So I made the test again with another clear ITO glass, for this time I set the sweeping potential from -1.5 V to 1.5 V, and color change did not occur. Later I set the potential back to -2 V ~ 2 V, the color change appeared again!
I have tried some other ITO glass from different suppliers, this problem, however, still occur.
Can anybody give me some advice about this?
Best regards,
Yuhan
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this is general problem an you should need to read basic book . and u need to optimize concentration , scan range, scan rate , nd technical current volt cv relation ship with concentrations .
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In the review 'Energy transfer catalysis mediated by visible light: principles, applications, directions' (doi.org/10.1039/c8cs00054a) they talk about identifying the difference between electron transfer and energy transfer in different ways, the last of which: 'experimental or theoretical redox potential determination can also be used to exclude electron transfer processes and thus provide indirect evidence of a sensitization mechanism'.
How can one use the redox potentials obtained from a cyclic voltammogram to determine whether a photocatalyst undergoes an energy transfer mechanism and not a photoredox mechanism?
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This is a very fundamental question in photochemistry. As you probably know :
- Dexter mechanism, involved for exemple in triplet-triplet annihilation, is one type of energy transfer. And at closer look and generally represented, this mechanism involves reciprocal electronic transfer !
- The electron when added or removed to or from a molecule changes the energy of the molecule: can we talk about energy transfer also when transferring electron because of these modifications?!
I cannot directly answer your question but could decipher what the authors wanted to say: the sentence might seem to say that, if the redox potentials of your molecule, compared to your photoredox catalyst doesn't match, but, the given reaction occurs anyway, energy transfer might be involved.
This is well discussed in this publication of Yoon for example:
And also in those very interesting publications, where, it might be, even when redox potentials not matching... A discussion on redox-mediated reactions.
The question is still opened and I could also suggest you to have a look on this publication:
Hope this could help you!
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I knew that cyclic voltammetry was conducted with beakers using three electrodes, but when I read the battery-related paper, I saw that cv was performed with coin cells. How do coin cells apply reference electrodes? Like how do they set Li+/Li as a reference?
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yes, sometimes[1-4], It might be (critical and) decisive ('okay'[4]) to approach a time consuming measurement of the (quasi-potentials via) open-circuit potential, Voc, after acceptable (commonly, very long) relaxation time->oo, Voc(time->oo), in GITT[3] analysis of 'fresh' cells, whenever (long relaxation) time is not an issue.
1. GITT Analysis of Lithium Insertion Cathodes for Determining the Lithium Diffusion Coefficient at Low Temperature: Challenges and Pitfalls https://iopscience.iop.org/article/10.1149/1945-7111/ab9404/meta
2. Galvanostatic Intermittent Titration and Performance Based Analysis of LiNi0.5Co0.2Mn0.3O2 Cathode https://www.nrel.gov/docs/fy18osti/70071.pdf
3. Galvanostatic Intermittent Titration Technique (GITT) https://www.metrohm.com/en/applications/AN-BAT-003
4. for cells with a two-electrodes' configuration.
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Hi All,
I have been running CV on a single fuel cell using two different flow rates: 0.2 H_2/0.5 N_2 and 0.4 H_2 / 0.001 N_2 - A/C @ 20 mVs-1 scan rate. However, I am encountering a noise issue in the second flow rate which is supposed to give me a better CV curve with resolved Pt peaks. Can any one suggest how to get a proper CV?
Thank you
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Annacia Jeffers Thank you for the suggestion. The CV is run on a single cell which has already been conditioned. I will try to scan at a lower rate. Other observation was higher hydrogen evolution current or higher hydrogen desorption in the anode side of CV curve because of that there is a shift in CV curve.
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How to calculate oxidation current density from cyclic voltammetry?, and how to calculate photocurrent density from transient short-circuits photocurrent data?
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you are welcome
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I am wondering about the recommended scan rate to generate linear sweep voltammetry and cyclic voltammetry curves for a photoelectrochemical hydrogen cell because I read some papers using different scan rates for the same application.
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For cyclic voltammetry (CV) I would recommend to test 20 mV/s, 50 mV/s and 100 mV/s for LSV 5-50 mV/s.
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Dear all,
I'm running a cyclic voltammetry and I selected a voltage range to sweep in. There is, however, a problem.
I want to detect a current when my sweeping voltage is between -0.4v and 0.2 v. The voltages need to sweep in 4 steps, therefore I sweep voltages 0v.....0.2v......0v.....-0.4v in four steps. But I could only see anodic peak. I decided to sweep voltages this time as: 0v.....-0.4v......0v.....0.2v. In that case, I only could see the cathodic peak. I don't know how to sweep the voltage in a way that I can see both cathodic and anodic peak together? Does that mean that my sweep voltages should somehow change?
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I started using 3 electrode setup now and with MB, here are the results. My CE and RE electrodes are both Cu BE gold covered electrodes. As the experiment is running for more than 10 minutes with the same probe, I noticed that there is a very thin black color on my electrodes.
Can it be the copper that oxidises in the reaction? (However, after cleaning the surface with IPA, the black layer is disappeared.)
In the graphs I still can see the current shift after running few cycles. This can happen, as you mentioned, as a result of change in concentration profile of the oxidation, then. Michal Hanko
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We generally measure the capacitance by the three electrochemical techniques
1. Cyclic Voltammetry
2. Galvanostatic Charge/Discharge
3. Electrochemical Impedance spectroscopy
I want to just know that which one is best for calculating the capacitance for Supercapacitor? and why? What is the advantages and disadvantages over each other?
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All these electrochemical techniques have their own importance.
Cyclic voltammetry: is an electrochemical technique that takes place at the electrode-electrolyte interface for qualitative information of electrochemical reactions. Cyclic voltammetry is used to understand the mechanism of redox reaction and electron transfer kinetics of an electroactive species in electrolytes.
CV is an electrochemical technique for measuring the current response that develops in the electrochemical cell during a linearly cycled potential sweep between the chosen potential window. This process is repeated multiple times during the scan and changes in the current value are measured by the device. This scan generates a duck-shaped plot that is called cyclic voltammogram.
Galvanostatic charge-discharge technique: is also known as chronopotentiometry. It is used for testing of supercapacitor performance parameters like specific capacitance, cyclic stability, and resistance. Thereafter energy density, power density and columbic efficiency are calculated. In GCD current is controlled and voltage is measured. The voltage (V) is generated by the current applied during the charging process.
Electrochemical impedance spectroscopy: In the frequency domain, impedance spectroscopy is a powerful method to evaluate the specific capacitance. The supercapacitor is fabricated by two identical electrodes separated by solid/liquid/gel electrolyte. The IS gives the relation between idealized equivale@nt circuit and real system which comprises the electrical component (inductor, capacitor, resistor) in the parallel and series combinations. Electrochemical impedance spectroscopy is an AC technique in which an applied potential E(t) is modulated over time with a small amplitude (|E0| ∼ 5−10 mV) at a controlled frequency (ω).
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I'm trying to set up a CV experiment using an Arbin battery cycler, however when I try to save I get an error message saying that the Schedule must contain at least one step (presumably referring to the 'Step/ Limit' tab). I have tried adding a short 'rest' (OCV) step for 10 seconds to the 'Step/ Limit' tab, however when I run the schedule it finishes immediately after the rest step and does not transition to CV.
I've also tried dismissing the error message that says the Schedule must contain at least one step and trying to save anyway, but the Schedule fails to save when I do this.
I've followed the manual and made sure that CV is enabled in the Advanced Options of the configuration file, and I'm able to edit steps under the CV tab. I also followed the example in the manual for setting up a CV schedule, but this resulted in the above error.
Is there an additional setting that I need to change, or have I missed a key step?
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Thanks so much for your detailed answer.
I think I have managed to include the first part of your answer by adding a 'log' step to record the voltage each second (i.e. 'DV_Time').
However, my cell voltage (OCV) is ~2.3 V, and I set my CV limits as 1.5 V and 2.8 V, so hopefully this shouldn't cause a problem regarding the second part of your answer.
I think the problem might be in the 'Step/ limit' tab - when I set the 'PV Channel Time' step limit and set the schedule to progress to 'Next step', is it possible to direct the schedule to go to the CV schedule (i.e. that defined in the CV tab) as the next step (There is no next step defined within the 'Step/ limit' tab)? Currently I can't find a way to link the schedule defined in the 'Step/ limit' tab to steps defined in the 'CV schedule tab', however I'm not able to save and use the schedule with the 'Step/ limit' tab blank.
Thanks again for your help - it's really appreciated.
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I have been doing cyclic voltammetry of a ruthenium complex having counterion chloride. Changing it to PF6 gives rise to different spectra in the CV and one oxidation peak seems to be missing from the precursor?
Is it what generally happens? Can anyone give me any literature supporting this? Or something I am missing in the CV?
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Dear Arabinda Muley thank you for this very interesting technical question. Although we work in inorganic and organometallic chemistry, I'm absolutely not a proven expert in cyclic voltammetry. Thus please regard my suggestion as a non-expert answer. Apparently such an influence of the counter ions of metal complexes is not uncommon. To my knowledge it relates to the different adsorption behavior of the complexes to the electrodes. In this context, please have a look at the following potentially useful article:
Cyclic Voltammetry Examination for Effect of Counter Anion on Adsorptive Voltammetry of 11-Ferrocenytrimethylundecyl- ammonium at Carbon Paste Electrode
In this context please also have a look at the following relevant reference which is available as public full text:
Ruthenium Tetrazole-Based Electroluminescent Device: The Key Role of Counter-Ions for the Light Emission Properties
(see attached pdf file)
Good luck with your work and best wishes!