Micro-Volume Electrochemical Experiments: A Faster, More Efficient Approach

By Zimmer Peacock

Introduction

When it comes to electroanalytical or electrosynthetic experiments, researchers often use large volumes—5 mL, 50 mL, or even 500 mL. But what if we could achieve the same results with just 50 microliters?

In this post, I’ll explain why smaller volumes can lead to higher throughput, better statistical data, and reduced solvent waste, all while maintaining the integrity of electrochemical experiments.

The Problem with Traditional Electrochemical Cells

A typical electrochemical setup includes:

• A potentiostat

• A laptop

• A bulky electrochemical cell (often 50 mL or more)

Setting up these experiments can be time-consuming—aligning electrodes, clipping connectors, and filling the cell with solvent. For researchers, time is a precious resource, and inefficiencies in setup can slow down progress.

Key Challenges:

✅ Time-intensive – Manual electrode placement and cell assembly take effort.
✅ High solvent consumption – Large volumes mean more waste.
✅ Limited repeatability – Fewer replicates due to setup constraints.

A Better Alternative: Screen-Printed Electrodes (SPEs)

At Zimmer Peacock, we leverage screen-printed electrodes (SPEs), a technology widely used in in vitro diagnostics, for electrochemical research.

Why SPEs?

✔ All-in-one design – Working, counter, and reference electrodes on a single substrate.
✔ Ultra-low cost – Less than €0.50 per electrode (comparable in USD, GBP, etc.).
✔ Minimal setup time – Just place a drop (~50 µL) and start measuring in seconds.

Applications Beyond Electroanalysis

While SPEs are common in electroanalytical work, they can also be used for:
🔹 Electrosynthesis
🔹 Electrocatalysis
🔹 Parallel experimentation

How It Works: From CV to Electrosynthesis

1. Cyclic Voltammetry (CV) in Micro-Volumes

• A 50 µL drop on an SPE provides high-quality CV data without complex setups.

• No need for glass cells, cables, or manual electrode alignment.

2. Electrosynthesis & Electrocatalysis

• Quick CV scouting → Identify optimal potential.

• Fixed-potential experiments → Monitor current decay over time.

• Minimal sample consumption → Take a 1 µL aliquot for HPLC/LCMS analysis.

Why this works:

• Modern analytical instruments (HPLC, LCMS) are highly sensitive.

• Dilute small samples without losing data quality.

Scaling Up: Flow Cells & Robotic Automation

While micro-volume experiments accelerate discovery, scaling up is still possible:

1. Flow Cells for SPEs

• Continuous flow setups allow for larger-scale reactions while maintaining efficiency.

• Customizable dwell times for reaction optimization.

2. Robotic Parallelization

• Our robotic system enables 6 parallel experiments at 50 µL each.

• Higher statistical power – More replicates in less time.

Key Takeaways

🔹 Smaller volumes (50 µL) = Faster setup, less waste, more replicates.
🔹 SPEs = Affordable, easy-to-use, and compatible with existing potentiostats.
🔹 Data > Material – The goal is high-quality electrochemical data, not just product synthesis.
🔹 Automation & parallelization further accelerate research.