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While methane (CH<jats:sub>4<\/jats:sub>) is widely regarded as a valuable target product in CO<jats:sub>2<\/jats:sub> reduction studies, the reliability of such measurements can be compromised by unintended CH<jats:sub>4<\/jats:sub> generation from solvent or sacrificial reagent decomposition during photoreactions. Herein, we systematically evaluate the stability of seven common solvents and five sacrificial reagents under visible\u2010light irradiation (\u03bb &gt;420\u2005nm) in CO<jats:sub>2<\/jats:sub>\u2010, air\u2010, and N<jats:sub>2<\/jats:sub>\u2010saturated atmosphere, employing three distinct photosensitizers. Notably, acetone, dimethyl sulfoxide (DMSO), and triethylamine (TEA) were identified as high\u2010risk reagents prone to photodecomposition, generating substantial CH<jats:sub>4<\/jats:sub> yields of up to 2770\u2005\u03bcmol\u2009\u22c5\u2009h<jats:sup>\u22121<\/jats:sup>\u2009\u22c5\u2009L<jats:sup>\u22121<\/jats:sup>. Isotopic labeling experiments conclusively demonstrated that the source of CH<jats:sub>4<\/jats:sub> originated from the solvents or sacrificial reagents rather than CO<jats:sub>2<\/jats:sub>. These findings highlight critical pitfalls in experimental design for photocatalytic CO<jats:sub>2<\/jats:sub> reduction and emphasize the necessity of rigorous reagent screening to avoid artifactual methane production.<\/jats:p>","DOI":"10.1002\/chem.202500403","type":"journal-article","created":{"date-parts":[[2025,3,11]],"date-time":"2025-03-11T17:11:01Z","timestamp":1741713061000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":4,"title":["Systematic Analysis of False\u2010Positive CH<sub>4<\/sub> Production in Photocatalytic CO<sub>2<\/sub> Reduction: The Role of Solvent and Reagent Decomposition"],"prefix":"10.1002","volume":"31","author":[{"ORCID":"https:\/\/orcid.org\/0009-0008-4724-4690","authenticated-orcid":false,"given":"Lingxuan","family":"Chen","sequence":"first","affiliation":[{"name":"State Key Laboratory of Organometallic Chemistry and Shanghai-Hong Kong Joint Laboratory in Chemical Synthesis Shanghai Institute of Organic Chemistry University of Chinese Academy of Sciences Chinese Academy of Sciences  Shanghai 200032 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2345-8511","authenticated-orcid":false,"given":"Jiangshan","family":"Zhang","sequence":"additional","affiliation":[{"name":"Department of Chemistry Fudan University  2205 Songhu Road Shanghai 200438 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3954-0015","authenticated-orcid":false,"given":"Zhan\u2010Ting","family":"Li","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Organometallic Chemistry and Shanghai-Hong Kong Joint Laboratory in Chemical Synthesis Shanghai Institute of Organic Chemistry University of Chinese Academy of Sciences Chinese Academy of Sciences  Shanghai 200032 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8339-0563","authenticated-orcid":false,"given":"Jia","family":"Tian","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Organometallic Chemistry and Shanghai-Hong Kong Joint Laboratory in Chemical Synthesis Shanghai Institute of Organic Chemistry University of Chinese Academy of Sciences Chinese Academy of Sciences  Shanghai 200032 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,3,18]]},"reference":[{"key":"e_1_2_9_1_1","unstructured":"\u00a0"},{"key":"e_1_2_9_2_2","doi-asserted-by":"publisher","DOI":"10.1002\/adfm.202309060"},{"key":"e_1_2_9_3_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.8b00400"},{"key":"e_1_2_9_4_1","unstructured":"\u00a0"},{"key":"e_1_2_9_5_2","doi-asserted-by":"publisher","DOI":"10.1038\/s43586-023-00243-w"},{"key":"e_1_2_9_6_2","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.0c00478"},{"key":"e_1_2_9_7_2","author":"Shixing L.","year":"2024","journal-title":"Sci. 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