64729 2025 eng 1 7 article American Chemical Society (ACS) 1 -- -- -- Over the past decade, energy-dispersive X-ray spectrometry (EDS) with scanning electron microscopy (SEM) has advanced to enable the accurate analysis of light elements such as C, N, or O. For this reason, EDS is becoming increasingly interesting as an analytical method for the elemental analysis of functionalized graphene and could be an attractive alternative to Xray photoelectron spectroscopy (XPS), which is considered the most important method for elemental analysis. In this study, comparative XPS and EDS investigations under different excitation conditions are carried out on commercially available powders containing graphene particles with different morphologies. The slightly different XPS/HAXPES and EDS results can be explained by the different information depths of the methods and the functionalization of the particle surfaces. For the material with smaller graphene particles and higher O/C ratios, all methods reported a lower O/C ratio in pellets compared with the unpressed powder samples. This clearly shows that sample preparation has a significant influence on the quantification results, especially for such a type of morphology. Overall, the study demonstrates that EDS is a reliable and fast alternative to XPS for the elemental quantification of functionalized graphene particles, provided that differences in the information depth are taken into account. Particle morphology can be examined in parallel with quantitative element analysis, since EDS spectrometers are typically coupled with SEM, which are available in a huge number of analytical laboratories. ACS Omega 2470-1343 10.1021/acsomega.5c07830 urn:nbn:de:kobv:b43-647294 true journal-article https://creativecommons.org/licenses/by/4.0/ crossref PersonAuthorFirstName_1,PersonAuthorLastName_1,PersonAuthorFirstName_2,PersonAuthorLastName_2,PersonAuthorIdentifierOrcid_2,PersonAuthorFirstName_3,PersonAuthorLastName_3,PersonAuthorIdentifierOrcid_3,PublisherName,TitleMain_1,Language,TitleParent_1,ArticleNumber,PublishedYear,IdentifierIssn,Enrichmentlocal_crossrefLicence doi-import 17.11.2025 Creative Commons - CC BY - Namensnennung 4.0 International Giovanni Chemello Jörg Radnik Vasile-Dan Hodoroaba eng uncontrolled Graphene oxide eng uncontrolled SEM/EDS eng uncontrolled XPS/HAXPES eng uncontrolled Elemental composition eng uncontrolled Functionalization Ingenieurwissenschaften und zugeordnete Tätigkeiten 6 Materialchemie 6.1 Oberflächen- und Dünnschichtanalyse Material Verlagsliteratur Datei für die Öffentlichkeit verfügbar ("Open Access") Wissenschaftliche Artikel der BAM Advanced Materials Bundesanstalt für Materialforschung und -prüfung (BAM) https://opus4.kobv.de/opus4-bam/files/64729/ChemelloEtal_2025_ACSO_XPS-SEM-EDSTandem.pdf