Best practices for in-situ and operando techniques within electrocatalytic systems

Area of Science:

• Heterogeneous electrocatalysis
• In-situ and operando spectroscopy
• Catalyst design

Background:

• In-situ and operando techniques are vital for linking catalyst structure to activity.
• Accurate execution and interpretation are critical for drawing strong conclusions.
• Most reviews focus on technique application, not optimal execution and insight analysis.

Purpose of the Study:

• To provide a nuanced discussion on the best practices for executing in-situ and operando techniques.
• To analyze the level of insight obtainable from various experimental setups and controls.
• To identify common pitfalls and offer strategies for avoidance and complementary experiments.

Main Methods:

• Focus on vibrational (IR, Raman) spectroscopy, X-ray absorption spectroscopy, and electrochemical mass spectrometry.
• Includes sections on reactor design and theoretical modeling applicable across techniques.
• Discusses complementary experiments to enhance analytical strength.

Main Results:

• Highlights common pitfalls in the application of in-situ and operando techniques.
• Provides guidance on optimizing the execution of these experiments.
• Identifies how to interpret results to maximize mechanistic understanding.

Conclusions:

• Emphasizes the critical role of proper technique execution and interpretation in heterogeneous electrocatalysis.
• Suggests complementary experiments and theoretical modeling to strengthen conclusions.
• Outlines remaining gaps and future innovations needed for in-situ and operando techniques.