12/06/2020

SEM image

SEM image of Al2O3-coated TiO2 nanoparticles obtained from the JRC repository (Lot ID JRC NM 62001a). A primary particle size of ca. 20 nm was observed.

Source: BAM division 6.1

Project period

01/01/2017 - 31/12/2020

Project type

EU project

Project status

Current

Topics

Description

The goal of the ACEnano project is to introduce confidence, adaptability and clarity into nanomaterial risk assessment by developing a widely implementable and robust tiered approach to nanomaterial physicochemical characterisation.

Location

Bundesanstalt für Materialforschung und -prüfung (BAM)
Richard-Willstätter-Straße 11
12489 Berlin

ACEnano logo

Source: ACEnano project

Nanomaterials are widely used in consumer products as well as in industry. Due to the increasing prevalence of these materials their impact on health and environment is becoming more and more relevant; simultaneously, their unique chemical and toxicological properties due to their size and surface area are not yet fully established. In order to safely classify and regulate these materials, both specific physicochemical information as well as an understanding of their structural-toxicological relationship are required.

Stilisierter Programmablaufplan

Source: BAM

Different spectroscopic and microscopic techniques such as single particle inductively coupled mass spectrometry (SP-ICP-TOF-MS), atomic force microscopy (AFM), Raman and electron microscopy, time-of-flight secondary ion mass spectrometry (TOF-SIMS) will be optimised for nanomaterial characterisation. Additionally, size separation techniques like field flow fractionation (FFF) are implemented in analytical systems; one focus is the coupling of different techniques. Another focus is the optimization and automatization of nanoparticle preparation.

Ein Pfeil in der Mitte einer Zielscheibe

Source: BAM

New techniques, instrumentation and equipment have been developed, and established techniques/ instrumentation optimised for the testing of nanomaterial properties. All these developments are being embedded into a quality assurance and risk assessment framework. The innovations and outcomes will be disseminated, especially to small and medium enterprises (SMEs), and used for new standards for regulation (e.g. OECD) and standardisation (e.g. ISO, CEN) bodies.

Händeschütteln

Source: BAM

24 European and 4 non-European partners from 12 countries, including universities, research centres, governmental institutions and small and medium enterprises.

Interlaboratory comparison - Call for participation

BAM and BfR have launched a VAMAS interlaboratory comparison on "Surface analysis of oxide nanoparticles" for new standards in ISO/IC 201.

Interested? Contact Joerg.Radnik@bam.de or harald.jungnickel@bfr.bund.de

Objectives

ACEnano constructs a quality assurance and risk assessment framework for nanomaterials by constructing a methodology for nanomaterial characterisation. This project optimises, miniaturises, simplifies and verifies a carefully selected set of analytical techniques, instrumentation and equipment for testing nanomaterial properties and characteristics, as well as supporting their use by small and medium enterprises (SMEs) through training and documentation. The result is the “ACEnano toolbox”: a user-friendly decision tool available on the ACEnano website, which helps users to simplify the choice of appropriate experimental methods for reliable characterisation of nanomaterials. These advances in methodology are linked to an ontology framework to ensure that the data obtained with these methods complies with the “FAIR” standards (Findable, Accessible, Interoperable, Reusable). These outcomes are then embedded into a quality assurance and risk assessment framework which includes method validations and interlaboratory comparisons, and which sets criteria for benchmarking of future innovation in this field. The innovations and outcomes from the project will be disseminated to the scientific community and to SMEs and used for new standards for regulation (e.g. OECD) and standardisation (e.g. ISO, CEN) bodies.

Impact

The development of standard operating procedures for nanomaterial analysis will allow greater consistency in analysis as well as comparability of data. Automatized systems, especially for sample preparation, will simplify the application and lead to a better reproducibility of the procedures. Additionally, the machine readability of the data obtained in this project will help to identify key descriptors and to reveal correlations associated with health and environment impacts. Effective analysis of the structure-property relationships of nanomaterials, particularly regarding their toxicological properties, will enable more accurate and efficient regulation and increase the confidence in both nanomaterial analysis and nanosafety studies with these methods.

BAM contribution

With an information depth of about 1 nm, a lateral resolution of ca. 100 nm and a low detection limit in the ppb region, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is a unique tool in surface analytics which requires great care in sample preparation and measuring. Additionally, the unique properties of nanomaterials, particularly their extremely high surface area, require particular sample preparation techniques depending on their state (powder or suspension), purity (presence of contaminants), material (metal/inorganic/organic), structure (solid or biological), and sensitivity to handling methods (organic coatings, agglomerates, biological structures).
The BAM contribution focuses on areas such as (1) ToF-SIMS analysis of TiO2 nanoparticles with and without sensitive organic coatings using different sample preparation methods, to determine the effect of the preparation method on the results, and (2) comparison of ToF-SIMS spectra of various coated and uncoated nanoparticles, to determine the ability of ToF-SIMS coupled with multivariate statistical analysis (in this case using Principal Component Analysis) to differentiate between TiO2 particles of different structure, coating and synthesis methods.

Scores plot from the Principal Component analysis for four different kinds of titania nanoparticles

Scores plot from the Principal Component analysis for four different kinds of titania nanoparticles (NM103: coated with a hydrophobic capping, NM104: coated with a hydrophilic capping, NM105: mixed anatase-rutile and BAM P100: pure anatase) NPs in the negative ion mode, showing the ability to clearly differentiate particles of different structure, synthetic methods and surface coatings based on ToF-SIMS analysis. Coloured ellipses indicate 95% confidence intervals.

Source: BAM, Division 6.1

To meet all these challenges, BAM (together with the project partners Helmholtz Centre for Environmental Research, Leipzig, and the Bundesinstitut für Risikobewertung (BfR), Berlin) have optimised procedures for the preparation, measurement and data reduction for ToF-SIMS of nanomaterials.  This work includes testing, optimisation and determination of suitable and unsuitable preparation methods for a variety of nanomaterials (metallic, inorganic, organic, and biological). These methods will form the basis for upcoming standardisation activities for ToF-SIMS investigations of nanoparticles. For the next step in the standardisation process, BAM and BfR have launched  an interlaboratory comparison (ILC) in the framework of the Versailles Project on Advanced Materials and Standards (VAMAS). These ILCs provide a technical basis for harmonised measurements, testing, specifications and standards which are necessary for acceptance of the procedures used in risk assessments. Following publication of the ILC in scientific journals, they will be included in standard measurement procedures submitted as standardisation projects to ISO.

Due to BAM’s expertise in standardisation and method validation, as well as participation in national and international standardisation activities, BAM is a key project partner for integrating the methods and technologies developed in ACEnano into the quality assurance framework. This includes advising and supporting project partners in all questions regarding validation, standardisation and regulation, as well as acting as a contact point for standardisation activities (CEN, ISO).

Project coordination

University of Birmingham

Partner organisations

University of Birmingham
Universität Wien
UK Research and Innovation
Edelweiss Connect
Postnova Analytics
Centre Suisse d’Electronique et de Microtechnique
Stichting Wageningen Research
Eidgenoessische Technische Hochschule Zürich
PerkinElmer
Swedish University of Agricultural Science
TOFWERK
Helmholtz Centre for Environmental Research
Vitrocell
Malvern Instrument
Horiba
Biolin Scientific
Sciex
University of Oxford
Nanofuture
IDONIAL
BioNanoNet
Hanyang University
National Center for Nanoscience and Technology, China
Bundesinstitut für Risikobewertung
Bundesanstalt für Materialforschung und -prüfung (BAM)
TO21
Joint Research Centre – European Commission

Oscube

Publications

F. Bennet, A. Müller, J. Radnik, Y. Hachenberger, H. Jungnickel, P. Laux, A. Luch, J. Tentschert Preparation of Nanoparticles for ToF-SIMS and XPS Analysis Journal of Visualised Experiments (2020) (submitted)

Funding

This project has received funding from European Union Horizon 2020 Programme (H2020) under grant agreement nº 720952.

Horizon 2020 Logo

Source: The European Union's Horizon 2020 research and innovation programme