62435 2025 eng 1 7 article Wiley VHC-Verlag 1 -- -- -- Knowledge of the structure–property relationships of functional nanomaterials, including, for example, their size- and composition-dependent photoluminescence (PL) and particle-to-particle variations, is crucial for their design and reproducibility. Herein, the Angstrom-resolution capability of an analytical ultracentrifuge combined with an in-line multiwavelength emission detection system (MWE-AUC) for measuring the sedimentation coefficient-resolved spectrally corrected PL spectra of dispersed nanoparticles is demonstrated. The capabilities of this technique are shown for giant-shell CdSe/CdS quantum dots (g-QDs) with a PL quantum yield (PL QY) close to unity capped with oleic acid and oleylamine ligands. The MWE-AUC PL measurements are calibrated and validated with certified fluorescence standards. The spectrally corrected and size-dependent PL spectra of the g-QDs derived from a single MWE-AUC experiment are then analyzed and compared with the results of single-particle spectroscopic studies, yielding the PL spectra, decay kinetics, and blinking behavior of individual g-QDs. This study underlines the vast potential of MWE-AUC with in-line optical detection for the characterization of advanced nanomaterials with a complex structure. Small Methods 10.1002/smtd.202401700 2366-9608 urn:nbn:de:kobv:b43-624357 publish 20.01.2025 false true Creative Commons - CC BY - Namensnennung 4.0 International L. M. S. Stiegler Karl David Wegner Florian Weigert W. Peukert Ute Resch-Genger J. Walter eng uncontrolled Quantum dots eng uncontrolled Analytical ultracentrifugation eng uncontrolled Photoluminescence eng uncontrolled Advanced nanomaterial characterization eng uncontrolled Calibrated fluorescence measurements eng uncontrolled Reference materials Analytische Chemie Ingenieurwissenschaften und zugeordnete Tätigkeiten 1 Analytische Chemie; Referenzmaterialien 1.2 Biophotonik Material Chemie und Prozesstechnik Chemische Charakterisierung und Spurenanalytik 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/62435/Wegner_Small Methods_2025.pdf