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Single\u2010atom catalysts (SACs) are promising for catalyzing CO\n                    <jats:sub>2<\/jats:sub>\n                    reduction reactions (CO\n                    <jats:sub>2<\/jats:sub>\n                    RR) owing to the tunable electronic structures of their central metal atoms, which enable precise control over the adsorption energies of reactants and intermediates. Additionally, SACs bridge the gap between homogeneous and heterogeneous catalysts, offering an ideal platform to investigate the reaction mechanisms of CO\n                    <jats:sub>2<\/jats:sub>\n                    RR. Therefore, gaining a comprehensive understanding of the intrinsic structural evolution of SACs, along with the micro\u2010environmental changes around active sites and electrode interfaces under operational conditions, is crucial for designing effective electrocatalysts and devices for CO\n                    <jats:sub>2<\/jats:sub>\n                    RR. This review introduces the fundamentals underlying the electrocatalytic CO\n                    <jats:sub>2<\/jats:sub>\n                    RR. Subsequently, the key techniques for SACs identification and validation are thoroughly analyzed, laying a theoretical basis for the case studies. Third, the latest development of in situ and operando analytical techniques of SACs toward CO\n                    <jats:sub>2<\/jats:sub>\n                    RR are summarized, including infrared spectroscopy (IR), Raman spectroscopy, X\u2010ray absorption spectroscopy (XAS), and transmission electron microscopy (TEM). Finally, several issues are raised and possible solutions are offered regarding the in situ and operando analytical techniques of SACs for the CO\n                    <jats:sub>2<\/jats:sub>\n                    RR.\n                  <\/jats:p>","DOI":"10.1002\/smtd.202500516","type":"journal-article","created":{"date-parts":[[2025,6,13]],"date-time":"2025-06-13T02:07:53Z","timestamp":1749780473000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":28,"title":["In Situ and Operando Analytical Techniques of Single\u2010Atom Catalysts for Electrocatalytic CO\n                    <sub>2<\/sub>\n                    Reduction"],"prefix":"10.1002","volume":"9","author":[{"given":"Rongbo","family":"Sun","sequence":"first","affiliation":[{"name":"Sinochem Holdings Corporation Ltd. Sinochem Energy High\u2010tech Corporation Ltd.  2 West Tieying Middle Rd., Fengtai District Beijing 100031 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xingyun","family":"Liu","sequence":"additional","affiliation":[{"name":"Division of Life Sciences and Medicine Department of Oncology The First Affiliated Hospital of USTC Center for Advanced Interdisciplinary Science and Biomedicine of IHM University of Science and Technology of China  Hefei Anhui 230601 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jingyao","family":"Huang","sequence":"additional","affiliation":[{"name":"Sinochem Holdings Corporation Ltd. 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