Hi everyone, first time posting here, and I am in desperate need of some help with some CVs I've been taking.

For context, I am an organic chemist that has recently started learning and taking CVs for a project I am working on. I am trying to learn but clearly do not understand enough.

I needed to retake some CVs I did last week but ran out of the solvent (DMAc) I was using. When I grabbed a completely new bottle and did a blank measurement, I began seeing a weird impurity in my CVs. I then tried another new bottle and saw the same thing, and every new bottle I've tried has this impurity. I am completely out of my old solvent bottle so I am a bit stuck on what to do. The bottles are from the same manufacturer and same purity so I do not know why this is happening.

I first I tried distilling some DMAc and the impurity is still there. I've tried other solvents, and NMP also shows this exact impurity but ACN doesn't. I tried using ACN but when measuring my actual substrate I started seeing extra peaks I wasn't seeing before, so I scratched that. I tried switching to another electrolyte - even opening a new bottle of TEA PF6 and it still is showing up. I've washed by electrodes, polished my glassy carbon many times, rinsed the glass holder, sparged for 10+ minutes with N2, remade the electrolyte solution and nothing has worked.

I need to run a test with DMF but while I am doing that thought maybe reddit knows what this is , how to fix it or suggestions on what to do.

The CV in the picture attached has the following:

- 5mL anhydrous DMAc from Sigma-Aldrich 99.8% purity

- 0.1M TBA PF6

- Glassy carbon working electrode

- Pt wire counter

- Ag/AgCl reference

Literally just that - no substrate, nothing

In red is my blank with the exact same set up just w my other solvent bottle I took like a week ago (I know I also had something in there around 0.8V and the potential going up around +1.5V is due to solvent oxidation) and blue is now with this new DMAc bottle

Thank you guys in advance!

edit: Just tried DMF. Regular 99.8% pure DMF showed the peak but HPLC grade (>99.999%) did not -

Hello all,

I have been trying to wrap my head around doing this properly, and I wanted to pop this question here in case I am missing some knowledge as I come from a mechanical background.

I have an electrochemical cell that is connected to a control circuit. The circuit is designed to be as minimalist as possible and to have the least possible electrical interference.

I intend to perform measurements on the cell; to do so, I have opted for a 4-terminal connection, as this allows me to measure the voltage across the cell directly (as opposed to the full control circuit).

From short-circuit measurements and open-circuit measurements, I see that the circuit still has a certain signature and has a phase shift over 1kHz. It seems however that these measurements are highly repetitive. So my question is: What is the best way to compensate for this in this specific configuration? I see a lot of guides that do this for 2-wire connections or Kelvin connections where both electrodes are connected, but not for this specific setup.

Thank you in advance!

I was wondering if anyone would be willing to offer some tutoring or help me interpret and understand my electrochemical results.
I have used cyclic voltammetry and chronoamperometry in my experiments. I have very basic knowledge of these techniques and only a few results that I would like help understanding.
I would really appreciate it :)

Please forgive me for asking this, we are genuinely new to electrochem testing. We are planning to do CV and GCD tests using single junction Ag/AgCl as reference electrode. Our study is for investigating the specific capacitance of various activated carbon and polyaniline samples. We have decided to use NaCl as our electrolyte for this application. Does that mean we have to change the filling (internal) electrolyte as well? Thank you!

Hello,

I have a question regarding reference electrodes and whether my understanding of their limitations are correct.

We are an organic synthesis laboratory and only need to perform cyclic voltammetry measurements in aqueous systems once in a blue moon.

As I understand it, commercial reference electrodes require appropriate storage and maintenance to remain reliable over extended periods. My concern is that, given how rarely we perform electrochemical measurements, a commercial electrode would likely end up sitting in a drawer for years, only to be used without anyone verifying whether its potential is still reliable. I am also not enthusiastic to negotiate with my PI for every time that I might have to buy one.

For this reason, I had the idea to prepare a simple Ag/AgCl reference electrode with a 3 M KCl agar-agar salt bridge whenever needed, and to verify its potential before use, including measurements against the ferri/ferrocyanide redox couple and open circuit potential.

However, as my background is in organic synthesis and I have very limited practical experience with electrochemistry, I wanted to ask here if you would consider CV measurements obtained using such a setup suitable for publication in organic chemistry journals, provided that the electrode construction and verification procedures are properly documented.

I plan to first record a blank voltammogram of the electrolyte solution, then add the analyte and record its voltammogram, and finally add potassium ferrocyanide to the same solution and record another voltammogram. This would provide an internal reference measured under identical conditions.

The aim would primarily be to determine midpoint potentials for reversible redox processes, including their dependence on pH.

Would you consider this a sufficiently reliable approach for publishable electrochemical data? And if not, do you have any suggestions to improve it besides the obvious "Buy a commercial reference electrode".

Good Day again everybody! We are now going to test our 17 electrodes (Activated Carbon + PANI casted onto nickel foam) for CV and GCD. Should we use the same electrode for both CV and GCD or should we prepare two identical electrodes (mass loading is noted of course) for each test? Thank you!

Hi all!

I'm trying to measure organic compounds in DMF and TBAPF6 at appropriate concentrations. As far as I know, using sat. Ag/AgCl reference electrode is not recommended for non-aqueous samples, yet the paper I'm trying to compare my results to used it without apparent troubles? I'm seeing water traces in my background and also features in my actual samples that aren't in the paper. I dry my solvent over 3A sieves and degass with nitrogen, so I suspect the only source of water is the Ag/AgCl electrode is leaking into my cell (graph attached).

Do you all think its possible to use my Ag/AgCl electrode as a quasi-reference electrode so I don't introduce any water in the first place? If so, how should I prepare it?

Thanks !!

Hello guys! Does anyone have any experience recoating their Ag/AgCl electrodes? How do you do it? We have a three-electrode setup and an EDAQ potentiostat.

Hi. I'm a new student working on corrosion. I am struggling with understanding EIS. Just reading theory and papers is not working for me. I don't know what kind or data should I be looking for in echem analyst nor the kind of parameters I should set while running a test. What is the purpose for running OCP in the beginning. I'm sorry if it's a stupid question.

Where is a good place to start?

I want to ingredients for making an electroplate bath with a fine silver anode , I’ve heard curse is one chemical , please help me thanks

1.immersion fluids channel

2.insulation fluids " "

3.gas channel

For batteries, data centers, compute irrespective of size .

Is these solutions are at notch already?

These are are for high lifecycles and high duration of heat production either should be recovered or disclose autonomy.

Would love to hear technology on these , companies doing it and where does this manufacturing capacity at and most importantly what % of this can be done with bio technology or bio liquids.

Is this a tech that needs attention and R&D .

From india

I have an exam coming up on the 12th, and I’m a graduate student taking Electrochemical Methods of Analysis. I’m honestly struggling badly with this class right now. I feel like I’m understanding almost nothing that’s being taught, and the professor’s notes are pretty scattered, so I’m having a really hard time putting the concepts together.

The textbook we’re using is Electrochemical Methods: Fundamentals and Applications by Allen J. Bard and Larry R. Faulkner. I know it’s considered a great book, but I’m finding it extremely difficult to learn from it without some kind of guidance.

At this point, I’m genuinely getting scared about the exam. If anyone knows of good online resources, YouTube channels, lecture notes, websites, or anything else that actually explains electrochemistry from the basics and makes the concepts easier to understand, I would really appreciate it.

Also, if you’ve taken a similar graduate-level electrochemistry course, any advice on how to prepare for an exam like this would be extremely helpful.

Hi, I'm currently doing my Master thesis in chemistry (based in Germany). It's in the field of bubble dynamics at structured electrodes and previously I have experience with Sea water electrolysis and various Electrochemical characterization, high speed imaging, optical characterization etc. I really like the work I do, I find it extremely fascinating but it has been very hard to find jobs. A lot of Semiconductor/battery industry seemed closely related but I never seem to even get interviews. Just a lot of rejections and honestly puts me down a lot.

A PhD is an option, but I've wanted a small break from studying and wanted to explore industry options. Any advice is appreciated , maybe you've been in similar situations or have known someone.

The following text is the output from Gemini after I asked it to create something using the electrode I had and then prepare it for posting on Reddit.

Hi everyone,

I’m working on a low-cost, benchtop setup to selectively reduce the C=C double bond in cinnamaldehyde to produce hydrocinnamaldehyde via Electrocatalytic Hydrogenation (ECH).

Because I want to avoid high overpotentials that trigger aggressive Hydrogen Evolution (HER) or over-reduction into hydrocinnamyl alcohol, I am trying to keep the cathode potential modest (aiming for a cell voltage around 2.2V–2.5V). I don't have a potentiostat, so I am trying to adapt basic household electronics to self-regulate.

Here is the proposed blueprint. I would appreciate any criticism or optimization tips on the circuit design, electrolyte balance, and cell geometry.

The Proposed Setup

1. Power Supply & Electronics

* Power Source: Standard 5V USB phone charger brick. * Current Limiter: A 47 Ω, 2-Watt ceramic power resistor wired in series on the positive (5V) line. * Target Metrics: Based on estimated cell resistance, this should cap the maximum current to roughly 50mA–70mA, dropping the voltage across the beaker electrodes down to a gentle 2.2V – 2.5V.

2. Electrodes & Geometry

* Cathode (-): A large 150 mm x 50 mm Platinum-coated Titanium (Pt/Ti) mesh. * Anode (+): A high-purity graphite rod harvested from a zinc-carbon lantern battery (significantly smaller in surface area than the cathode mesh). * Electrode Spacing: Fixed exactly 2 cm apart to maintain consistent cell resistance.

3. Electrolyte & Solvent System

* Solvent: A 70% Isopropyl Alcohol (or Ethanol) / 30% Water blend. This is intended to fully dissolve the cinnamaldehyde while maintaining decent ionic conductivity. * Supporting Electrolyte: 1.5g to 2g of Sodium Sulfate (Na₂SO₄) or Ammonium Chloride (NH₄Cl) per 100 mL. Note: Avoiding NaCl to prevent chlorine gas evolution at the anode.

4. Mass Transport & Anode Protection

* The "Hamster Wheel" Problem: To prevent the newly reduced hydrocinnamaldehyde from drifting to the graphite anode and re-oxidizing, I plan to tightly wrap the graphite anode in 4–5 layers of thoroughly rinsed, non-woven fabric (boiled baby wipes) secured with zip-ties. This creates a macro-porous diffusion barrier. * Agitation: The cell will be placed on a magnetic stirrer at a high, vigorous setting to force cinnamaldehyde onto the Pt/Ti cathode surface and out of the stagnant anode wrapper.

Questions for the Community

1. Electrode Asymmetry: My cathode mesh (150x50mm) has a much larger surface area than the carbon rod anode. This gives me a beautifully low current density at the cathode (which I hope minimizes radical dimerization/fouling), but will the smaller anode bottleneck the cell resistance too much under a 5V supply?
2. Mass Transport vs. Destruction: Will the rinsed fabric wrapper be sufficient to prevent significant anodic re-oxidation over a multi-hour run, or should I abandon the single-compartment setup entirely for a short, wide paper-towel salt bridge across two separate beakers?
3. Solvent System: Does a 70/30 alcohol-water mix provide enough proton availability for smooth Volmer-step adsorption on the platinum without spiking the solution resistance too high for a 5V source?

Let me know what flaws you see or what you would change! Thanks.

We still optimizing the system. But strange peak keeps showing up and literature doesn't fully explain what this might be. Maybe any of you had any encounter with it?

We are using Au surface modified with thiols solution as WE, Pt as CE and Ag/AgCl as RE.

With this system we try to reduce and oxidize Q10 in phospholipid membrane model. It has cholesterol and phosphatidyl MLV with Q10 inside. The solution we used was phosphate buffer with pH around 7.5.

The scan speed here 0.05 V/s.

Any insights or experiences would be helpful!

Thanks in advance!

What is the best thing to cut gap wafer? I was thinking diamond pen but I also want small long rectangles and need precision

I'm currently (I want to give up) doing electroanalytical research with boron doped diamond as a working electrode in a 3 electrode system. This WE is getting me in trouble because its surface is heterogeneous (not all the surface have boron in it and the diamond structure might differ from point to point) and the reproductivity of the method is not good because the results will be different from batch to batch. In a day I can make an analytical curve for some analyte analysis (effortlessly) but next day it wouldn't work even following the same steps I've had made before.
I tried to change the analytes and got nothing still. In the beginning I thought that this WE would be good for my research because in the articles they say it's good, that has a wide potential window, good sensibility (better than GCE) and all but in truth it's otherwise. I tried to modify it with carbon paste modifiers (sort of kind) and nothing.
I think that's why there are more articles with other WE (GCE, GQD) in comparison with BDD. I regret not giving up on it before.

Hi everyone,

I developed a free web application for processing raw electrochemical data, particularly for supercapacitor and electrode research. It supports txt, bin, CSV and XL files

For GCD data, the application can:

Extract complete charge–discharge cycles
Calculate specific capacitance
Compare rate capability at different current densities
Calculate coulombic efficiency and capacitance retention
Generate graphs and identify potential data issues

For CV data, it can perform Dunn-model analysis using files collected at multiple scan rates, including:

Calculation of b-values
Determination of k₁ and k₂
Separation of capacitive and diffusion-controlled contributions
Calculation of contribution percentages at each scan rate
Generation of fitted curves, R² values, and summary graphs

The processed results can also be downloaded as a prepared Excel workbook for further plotting in Origin.

Web application:
https://st-rahman.com/electrochemical-analysis/

I would appreciate feedback from researchers who regularly analyze CV or GCD data, especially regarding calculation accuracy, usability, and features that could be added in future versions.

I have 3 unused 5V/100mA battery cyclers that would probably be a good fit for coin-cell cycling and other low-current electrochemistry work.

They have 4 current ranges and ±0.02% F.S. accuracy.

I'd much rather see them go to a lab or company that will actually use them than have them sit around. If you're in the U.S. and think one could be useful for your work, feel free to send me a DM. Cost is not really the main concern here.

Question for people experienced with materials characterization: how long did it take you to get genuinely comfortable interpreting results across multiple techniques (XRD + SEM + XPS etc.) together, rather than just running each one separately?

I ask because a couple of people told me it's mostly about expertise/experience rather than a tooling problem — which makes me wonder how that expertise is actually built. Was it mentorship, trial and error, a specific resource, something else? Curious what that learning curve actually looked like for you.

I am running EIS on a BZCY proton conductor in dry vs wet air and I have a result I cannot pin down. Nyquist plot attached, blue is dry, red is wet. Same sample, same setpoint temperature (500 degC), same electrodes, wet gas is air bubbled through water at room temperature.

What makes sense: the arcs collapse by about 4x in wet, and total resistance drops roughly 40%. That is what I expected from hydration putting protons in.

What confuses me: the high-frequency real-axis intercept moves the wrong way. It goes from about 90 ohm in dry to about 140 ohm in wet. If that intercept is bulk resistance, humidifying should have lowered it, not raised it by 50%.

Two explanations I can think of, and I cannot separate them from this data alone:

1. Artifact. Both spectra have an inductive tail at the high-frequency end. A series inductance drags -Zim down and pushes the apparent zero-crossing to the right of the true series resistance, and it pushes a small fast arc (wet) further than a big slow one (dry). So some or all of my 50 ohm might be nothing.
2. Real. In dry oxidizing air the oxygen vacancies get oxidized rather than hydrated, giving p-type hole conduction, and holes are much more mobile than protons. Humidifying consumes those vacancies to make protons and suppresses the holes, so bulk resistance goes up while grain boundary and electrode resistance go down. That would match the pattern exactly.

Questions:

1. Has anyone seen the HF intercept move up on humidification in a BZCY and confirmed it was real rather than instrumental? A reference would help, I could not find this specific signature.
2. How much inductive distortion before an eyeballed intercept is meaningless? Is a short-circuit blank with the same cell and leads enough, or do you always fit L explicitly?
3. Best discriminator for the hole hypothesis: pO2 dependence at fixed humidity, or just compare activation energies between the two atmospheres?
4. How long do you dwell after switching to wet gas before you trust the spectrum? I want to be sure I am not looking at a transient.