Validated and standardized measurements and quantification of surface functionalities on nanoparticles
- Surface-functionalized organic and inorganic engineered nanomaterials (NMs) are widely applied in the life and materials sciences. NM performance depends on key factors such as particle size and shape, crystal phase, morphology, chemical composition, and surface chemistry, i.e., surface coatings, functional groups (FGs), and ligands.1 The latter controls their processability and interaction with the environment and largely their possible toxicity. Thus, methods for FG quantification are important tools for quality control of NM production processes and can foster the sustainable development of functional and safe(r) NMs. This underlines the importance of validated and standardized analytical methods for surface analysis and reference materials.2 This encouraged us to explore simple and versatile tools for quantifying common bioanalytically relevant FGs such as optical assays, electrochemical titration methods, quantitative nuclear magnetic resonance spectroscopy (qNMR), and X-RaySurface-functionalized organic and inorganic engineered nanomaterials (NMs) are widely applied in the life and materials sciences. NM performance depends on key factors such as particle size and shape, crystal phase, morphology, chemical composition, and surface chemistry, i.e., surface coatings, functional groups (FGs), and ligands.1 The latter controls their processability and interaction with the environment and largely their possible toxicity. Thus, methods for FG quantification are important tools for quality control of NM production processes and can foster the sustainable development of functional and safe(r) NMs. This underlines the importance of validated and standardized analytical methods for surface analysis and reference materials.2 This encouraged us to explore simple and versatile tools for quantifying common bioanalytically relevant FGs such as optical assays, electrochemical titration methods, quantitative nuclear magnetic resonance spectroscopy (qNMR), and X-Ray photoelectron spectroscopy (XPS) and to perform a first interlaboratory comparison (ILC) on surface FG quantification.3,4 In a follow-up ILC, BAM and NRC explored qNMR sample preparation, measurement, and data evaluation protocols for commercial and custom-made aminated SiO2 NPs with sizes of 20-100 nm, different amounts of surface amino FGs, and different porosity.5,6 First, the number of amino FGs accessible for a dye reporter was determined with a cost-efficient, automated optical fluorescamine assay. Then, qNMR workflows and protocols were stepwise fine-tuned. The qNMR ILC was complemented by joint XPS measurements. BAM also examined the applicability of fast and automatable potentiometric titrations to screen the total amount of (de)protonable FGs on aminated SiO2 NPs. Our results underline the need to evaluate protocols for FG quantification in ILCs and the advantages of multi-method characterization strategies for efficient method cross validation.…


| Autor*innen: | Isabella TavernaroORCiD, Sarah-Luise AbramORCiD, Christian Homann, Lena Scholtz, Jörg RadnikORCiD, Ute Resch-GengerORCiD |
|---|---|
| Dokumenttyp: | Vortrag |
| Veröffentlichungsform: | Präsentation |
| Sprache: | Englisch |
| Jahr der Erstveröffentlichung: | 2025 |
| Organisationseinheit der BAM: | 1 Analytische Chemie; Referenzmaterialien |
| 1 Analytische Chemie; Referenzmaterialien / 1.2 Biophotonik | |
| 6 Materialchemie | |
| 6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse | |
| DDC-Klassifikation: | Naturwissenschaften und Mathematik / Chemie / Analytische Chemie |
| Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten | |
| Freie Schlagwörter: | Calibration; Digital certificate; Fluorescence; Metrology; Nano; Particle; Potentiometry; QNMR; Quality assurance; Reference data; Reference material; Reference product; Surface analysis; Traceability; XPS |
| Themenfelder/Aktivitätsfelder der BAM: | Chemie und Prozesstechnik |
| Chemie und Prozesstechnik / Chemische Charakterisierung und Spurenanalytik | |
| Material | |
| Material / Advanced Materials | |
| Material / Materialdesign | |
| Umwelt | |
| Veranstaltung: | Surface and Micro/Nano Analysis Working Group |
| Veranstaltungsort: | Paris, France |
| Beginndatum der Veranstaltung: | 08.04.2025 |
| Enddatum der Veranstaltung: | 09.04.2025 |
| Verfügbarkeit des Dokuments: | Datei im Netzwerk der BAM verfügbar ("Closed Access") |
| Datum der Freischaltung: | 16.04.2025 |
| Referierte Publikation: | Nein |
| Eingeladener Vortrag (wissenschaftliche Konferenzen): | Nein |

