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Here, we directly test this assumption by comparing immersion\u2013emersion, droplet-based contact, and pressure-driven intrusion\u2013extrusion electrification using the same hydrophobic nanoporous silicon monolith and isotopically substituted liquids (H2O and D2O). Despite identical surface chemistry, isotopic substitution produces qualitatively different electrical responses depending on the wetting regime. Immersion\u2013emersion experiments show polarity inversion between H2O and D2O, while droplet measurements reveal distinct charge evolution and periodic opposite-polarity events. In contrast, forced nanopore intrusion preserves polarity but strongly enhances electrical output for D2O. These results demonstrate that wetting of surface nanoroughness during droplet, vs immersion\u2013emersion, vs complete nanopores wetting upon intrusion\u2013extrusion correspond to fundamentally different electrification states. By using isotope substitution as a controlled probe, this work establishes a general framework for disentangling protocol-dependent effects in solid\u2013liquid contact electrification and triboelectric energy conversion.<\/jats:p>","DOI":"10.1021\/acs.jpcc.6c04134","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T13:14:01Z","timestamp":1785849241000},"page":"12748-12756","source":"Crossref","is-referenced-by-count":0,"title":["Distinct Electrification\nRegimes at Solid\u2013Liquid\nInterfaces Revealed by Water Isotope Substitution"],"prefix":"10.1021","volume":"130","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-1972-0318","authenticated-orcid":true,"given":"Mesude Z.","family":"Arkan","sequence":"first","affiliation":[{"name":"University of Silesia , , ,","place":["Katowice, Poland, 40-006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9649-1470","authenticated-orcid":true,"given":"Luis","family":"Bartolome\u0301","sequence":"additional","affiliation":[{"name":"Basque Research and Technology Alliance (BRTA) , , Alava Technology Park, Albert Einstein 48 , ,","place":["Vitoria-Gasteiz, Spain, 01510"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6134-2624","authenticated-orcid":true,"given":"Raivis","family":"Egli\u0305tis","sequence":"additional","affiliation":[{"name":"Riga Technical University , , P. 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