r/electrochemistry • • 20h ago

Question regarding homemade reference electrodes for CV measurements

4 Upvotes

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".


r/electrochemistry • • 1d ago

Destroyed SPCE

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3 Upvotes

I have modified a SPCE with GOx+BSA after drying added GA 2.5 % let dry in fridge for 3h
My SPCE is completely destroyed
I have tried to google de cracking issue but I can’t rinse anything about it

Has anyone experience the same thing?
I have also tried to adjust the concentration of GA to 0.5% and 0.25% but nothing works

There is nothing about it in literature. I have only found papers about cracking during manufacturing of the SPCE


r/electrochemistry • • 1d ago

Oparic: From raw electrochemical data to editable Origin® projects

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3 Upvotes

r/electrochemistry • • 2d ago

CV then GCD, change the electrode?

1 Upvotes

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!


r/electrochemistry • • 2d ago

Non-aqueous DMF for CV. Need advice.

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3 Upvotes

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 !!


r/electrochemistry • • 2d ago

Recoating Ag/AgCl Electrode

3 Upvotes

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.


r/electrochemistry • • 5d ago

Need help with EIS

3 Upvotes

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?


r/electrochemistry • • 7d ago

I need help knowing what goes into electroplating silver bath

0 Upvotes

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


r/electrochemistry • • 11d ago

Rilevatore antifumo a ionizzazione

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0 Upvotes

r/electrochemistry • • 11d ago

Electrochemistry & Semiconductor internships?

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2 Upvotes

r/electrochemistry • • 11d ago

Thermal management for heat in electronics

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0 Upvotes

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


r/electrochemistry • • 12d ago

I seriously need help with electrochemistry.

1 Upvotes

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.


r/electrochemistry • • 16d ago

Opportunities~

3 Upvotes

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.


r/electrochemistry • • 18d ago

Is Gemini good at this?

0 Upvotes

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.


r/electrochemistry • • 21d ago

Strange peak during reverse scan in cyclic voltammetry

3 Upvotes

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!


r/electrochemistry • • 23d ago

UD series on Electrochemical Engineering - Bamdad Bahar - The Electrochemical Century

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3 Upvotes

r/electrochemistry • • 25d ago

What to use to cut GaP Wafer

1 Upvotes

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


r/electrochemistry • • 27d ago

I think my method won't work. Have you worked with this WE before?

2 Upvotes

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.


r/electrochemistry • • Sep 14 '26

I built an app for electrochemical data sorting

7 Upvotes

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.


r/electrochemistry • • Sep 14 '26

Any U.S. labs doing coin-cell work need a low-current battery cycler?

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2 Upvotes

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.


r/electrochemistry • • Sep 12 '26

How long did it take you to get good at reading multiple characterization techniques together?

0 Upvotes

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.


r/electrochemistry • • Sep 10 '26

wet atmosphere shrinks the arcs but pushes the high-frequency intercept to higher resistance. Artifact or real?

2 Upvotes

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.
Nyquist plot

r/electrochemistry • • Sep 10 '26

How to resolve the issue of no plateau and an immediate current rise in the LSV measurement of HER

2 Upvotes

r/electrochemistry • • Sep 10 '26

RDE/RRDE expeiments with Pine MSR and CHI 660e

1 Upvotes

I'm currently working on setting up a *Pine Research Modulated Speed Rotator (MSR)* integrated with a *CHI 660 potentiostat* for oxygen reduction reaction (ORR) measurements in alkaline media. As part of validating the system, I've been testing a commercial 20 wt% Pt/C catalyst in 0.1 M KOH. However, I've been facing several challenges, including: • Very low current response • Excessive noise in CV and LSV measurements • Poor reproducibility between scans • Results that differ significantly from expected literature behaviour

After consulting with the equipment supplier, it appears that the rotator itself is operating as expected. Since the same issues are observed even when running experiments without rotation, the current thinking is that the problem may be related to the electrochemical setup, electrode connections, reference electrode condition, measurement parameters, or potentiostat configuration rather than the rotator itself. This brings me to a question for the community: ❓ *Has anyone successfully integrated a CHI 660 potentiostat with a Pine Research MSR for RDE experiments?*

I would greatly appreciate insights on: ✅ Compatibility between the CHI 660 and Pine MSR systems ✅ Wiring, grounding, shielding, or configuration tips ✅ Common causes of noisy signals and unusually low currents ✅ Best practices when validating a new RDE setup with a Pt/C benchmark catalyst ✅ Typical troubleshooting steps for ORR measurements in alkaline electrolytes Current setup: 🔹 CHI 660 Potentiostat 🔹 Pine Research MSR Rotator 🔹 Glassy Carbon Working Electrode with 20 wt% Pt/C catalyst 🔹 Ag/AgCl (4 M KCl) Reference Electrode 🔹 Pt Counter Electrode 🔹 0.1 M KOH Electrolyte

I'm also relatively new to the electrochemistry field and am always looking to improve my practical and theoretical understanding.

GRAPHS DISPLAYED IN CHI SOFTWARE
RDE SETUP
CV curves
LSV of Pt/C
inconsistent Cv curves

attached are some of the pictures of my setup.


r/electrochemistry • • Sep 07 '26

Am I doing an incorrect approach to EIS

2 Upvotes

So basically I designed an electrode container out of polypropylene, and inside of it is an agar media made of many things, but in particular Murashige and Skooge (3g/L) which provides many ions in the media. The agar media is for cloning plant tissues, and has a cactus inside of it.

There are graphite electrodes inside of the container, but only 2 (I don't have a reference electrode), when I read online that EIS usually involves a reference electrode. The reason why I did this was because I was thinking I could measure frequency-impedance response just by using a function generator, and measuring voltage drop across a series resistor as my schematic shows.

Anyways, I did this for four days and collected really good data, but am not sure how good or replicable the data is because I did not use a professional potentiostat, or a reference electrode at all. But this is because I just want to know the current applying through the media at a given frequency of ac voltage for an experiment later.

I'm wondering how bad my approach was. (Oh an also I couldn't calculate phase shift because my oscilloscope is only one channel)

The substrate age refers to how old the media is. There is no tendency for the data so far. The trendline was assuming normal capacitance instead of CFE.