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Time-of-flight mass spectrometry under ultra-high-vacuum conditions in conjunction with ultraviolet laser irradiation is employed to investigate photocatalytic water (D2O) splitting and its coupling with methyl iodide (CH3I) fragments on TiO2(100). Direct detection of elusive intermediates, such as D, OD, and OOD species, unequivocally provides experimental evidence for the elementary steps of photocatalytic water splitting under ultra-high-vacuum conditions. In the presence of CH3I, additional pathways emerge, leading to methane (CH3D) and methanol (CH3OD) formation via reactions between photogenerated water and methyl iodide fragments. Temperature-dependent measurements indicate that photocatalytic water splitting proceeds most efficiently at room temperature, whereas density functional theory calculations elucidate the underlying mechanisms that govern surface reactions. These results reveal molecular-level pathways of light-driven reactivity and provide a framework for controlling selective photocatalytic transformations at semiconductor interfaces.<\/jats:p>","DOI":"10.1021\/acs.jpclett.6c02227","type":"journal-article","created":{"date-parts":[[2026,9,23]],"date-time":"2026-09-23T14:01:45Z","timestamp":1790172105000},"page":"11532-11538","source":"Crossref","is-referenced-by-count":0,"title":["Direct Detection\nof Reactive Intermediates in Photocatalytic\nWater Splitting with Small Carbon Species on TiO2(100)"],"prefix":"10.1021","volume":"17","author":[{"given":"Aakash","family":"Gupta","sequence":"first","affiliation":[{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Syeda Faiza","family":"Sherazi","sequence":"additional","affiliation":[{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6391-8757","authenticated-orcid":true,"given":"Duy","family":"Le","sequence":"additional","affiliation":[{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]},{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christopher","family":"Sweatman","sequence":"additional","affiliation":[{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mihai V.","family":"Putz","sequence":"additional","affiliation":[{"name":"West University of Timisoara , , Str. Pestalozzi No. 16 , ,","place":["Timisoara, Romania, 300115"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Talat S.","family":"Rahman","sequence":"additional","affiliation":[{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]},{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2017-7757","authenticated-orcid":true,"given":"Mihai E.","family":"Vaida","sequence":"additional","affiliation":[{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]},{"name":"University of Central Florida , , , ,","place":["Orlando, Florida, United States, 32816"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,23]]},"reference":[{"issue":"6174","key":"2026100811163169100_cit1","doi-asserted-by":"publisher","first-page":"1239176","DOI":"10.1126\/science.1239176","article-title":"Solar synthesis: prospects in visible light photocatalysis","volume":"343","author":"Schultz","year":"2014","journal-title":"Science"},{"issue":"7","key":"2026100811163169100_cit2","doi-asserted-by":"publisher","first-page":"2891","DOI":"10.1021\/cr0500535","article-title":"Titanium Dioxide Nanomaterials: Synthesis, Properties,\nModifications, and Applications","volume":"107","author":"Chen","year":"2007","journal-title":"Chem. 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