In this review published in Catal, we provide a practical guide to the precise acquisition, analysis, and interpretation of X-ray Absorption Spectroscopy (XAS) data for catalysis research. Drawing on both synchrotron-based and laboratory-based XAS studies, we discuss common experimental and analytical pitfalls and present best practices for obtaining reliable information on oxidation states, spin states, local structures, and catalytic mechanisms.
Key Insights
- Comprehensive guidance for XAS experiments, covering sample preparation, energy calibration, normalization, and the selection of appropriate detection modes to ensure reliable and reproducible measurements.
- Common pitfalls and best practices for data interpretation, including self-absorption effects, detector dead time, EXAFS fitting, and spectral normalization that can significantly affect conclusions if not handled properly.
- Reliable strategies for determining oxidation states, spin states, local symmetry, and coordination environments using complementary soft and hard XAS techniques.
- Advanced analytical approaches, including multiple-scattering simulations, wavelet-transform EXAFS, PCA, and MCR-ALS, for investigating complex catalytic systems and transient intermediates.
- Practical considerations for operando XAS studies, highlighting the impact of catalyst particle size, active-layer depth, and surface-to-bulk contributions on mechanistic interpretation.
- Recent advances in laboratory-based XAS instrumentation, demonstrating increasing accessibility and performance for routine characterization, in situ studies, and catalyst development.
Significance of This Work
In this work, we emphasize that obtaining meaningful mechanistic insights from XAS requires not only advanced instrumentation but also rigorous experimental design and data analysis. By integrating fundamental principles with practical recommendations, we provide a comprehensive framework for the reliable application of XAS in catalysis research. We hope this review will serve as a valuable resource for both newcomers and experienced researchers seeking to uncover catalyst structure-performance relationships and reaction mechanisms with greater confidence.
Authors & Affiliations
Hao Zhang†, Yalei Fan†, Jianqiu Zhu, Haisheng Yu, Jian-Qiang Wang, Zhiwei Hu*, and Linjuan Zhang*
† These authors contributed equally to this work.
Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China
University of Science and Technology of China, Hefei 230026, China
National Innovation Scientific Instruments (Suzhou) Co., Ltd, Suzhou 215100, China
Max Planck Institute for Chemical Physics of Solids, Dresden 01187, Germany
Corresponding Authors
Prof. Zhiwei Hu ✉ Zhiwei.hu@cpfs.mpg.de
Prof. Linjuan Zhang ✉ zhanglinjuan@sinap.ac.cn
How to Cite This Article
Zhang, H., Fan, Y., Zhu, J. et al. Precise analysis and proper application of X-ray absorption spectroscopy. Catal 2, 18 (2026). https://doi.org/10.1007/s44422-026-00030-0