qNMR for standardised measurements of surface functionalities on nanoparticles

  • Engineered nanoparticles have a large application potential in fields such as medicine, sensing, catalysis, energy storage, and opto-electronics [1]. The applicability and performance of engineered nanoparticles is largely determined by their surface chemistry, i.e. functional groups and ligands on the particle surface. However, documented standards to quantify functional groups and ligands currently do not exist. Such standards are required to support quality control of nanomaterial production and surface modification processes, and safe-by-design concepts and to meet regulatory requirements. Here, this issue is addressed by developing and standardizing quantitative Nuclear Magnetic Resonance (qNMR) methods for the characterization of surface functionalized nanoparticles which specifically address the determination of the amount and chemical composition of surface functionalities and coatings. This work is being developed under the EMP project 23NRM02 SMURFnano - StandardisedEngineered nanoparticles have a large application potential in fields such as medicine, sensing, catalysis, energy storage, and opto-electronics [1]. The applicability and performance of engineered nanoparticles is largely determined by their surface chemistry, i.e. functional groups and ligands on the particle surface. However, documented standards to quantify functional groups and ligands currently do not exist. Such standards are required to support quality control of nanomaterial production and surface modification processes, and safe-by-design concepts and to meet regulatory requirements. Here, this issue is addressed by developing and standardizing quantitative Nuclear Magnetic Resonance (qNMR) methods for the characterization of surface functionalized nanoparticles which specifically address the determination of the amount and chemical composition of surface functionalities and coatings. This work is being developed under the EMP project 23NRM02 SMURFnano - Standardised measurements of surface functionalities on nanoparticles. qNMR competence of 7 qNMR laboratories involved in the project was first tested with a molecular model sample i.e. citrate, to be assessed in terms of purity. Citrate is often used as hydrophilic surface ligand for different nanoparticles. Then, the first nanoparticle samples, here a set of aminated SiO2 NPs [1] with a particle size of 100 nm and two amino group densities, prepared and characterized by BAM regarding size and surface charge as well as stability over 21 months with an optical assay and qNMR, were assessed in an international interlaboratory comparison (ILC) on qNMR. Thereby, the amount of surface amino groups introduced by grafting of the silica cores with different amounts of 3-aminopropyl)triethoxysilane (APTES) was quantified by each participant following a sample preparation protocol previously developed by BAM and NRC.The results of the ILC were then used to refine the protocol for sample preparation and to identify critical points for qNMR measurement and data analysis. This work will contribute to the development of a Preliminary Work Item (PWI) 19257 (ISO/TC 229) on surface functional groups and coatings on nano-objects. Also, it will lay the groundwork to perform ILCs on the quantification and determination of the amount of surface functional groups under the roof of VAMAS TWA2 (Surface Chemical Analysis) for different types of nanomaterials possessing industry-relevant surface functionalities using qNMR. These ILCs will be complemented by other techniques like X-Ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS).zeige mehrzeige weniger

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  • Portesi_UR_BERM qNMR_for PUBLICA_0406_2025.pdf
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  • Portesi_UR_qNMR summit 2025_SmurfNano abstract_0403_2025.pdf
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Metadaten
Autor*innen:C. Portesi
Koautor*innen:M. Torrelli, Isabella TavernaroORCiD, Sarah-Luise AbramORCiD, C. Clarkson, S. Ra, L. Johnston, A. Brinkmann, Klas Meyer, M. Reithofer, R. Richstein, M. Maurer, V. Cornel, P. Schmid, Ute Resch-GengerORCiD, Jörg RadnikORCiD
Dokumenttyp:Vortrag
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2025
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.2 Biophotonik
1 Analytische Chemie; Referenzmaterialien / 1.4 Non-Target-Analytik
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:Advanced materials; Characterization; Electron microscopy; Interlaboratory comparison; Metrology; Nano; Optical assay; Particle; Quality assurance; Silica; Standardization; Surface; Synthesis; Validation; qNMR
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
Chemie und Prozesstechnik / Chemische Charakterisierung und Spurenanalytik
Material
Material / Advanced Materials
Veranstaltung:BERM
Veranstaltungsort:Halifax, Canada
Beginndatum der Veranstaltung:01.06.2025
Enddatum der Veranstaltung:04.06.2025
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:19.06.2025
Referierte Publikation:Nein
Eingeladener Vortrag (wissenschaftliche Konferenzen):Nein
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