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The present study reports on results of analysis of the elemental composition of thin films by electron probe microanalysis with energy dispersive (ED-EPMA) X-ray spectrometry in conjunction with the dedicated thin-film analysis software package Stratagem and by X-ray fluorescence in its version with a micro-focus X-ray fluorescence (μ-XRF) source attached to a scanning electron microscope (SEM). Two thin-film systems have been analyzed: Fe1-xNix on silicon wafer and Si1-xGex on Al2O3 substrate, in both cases the layers being grown to a thickness of about 200 nm by ion beam sputter deposition. Samples of five different atomic fractions have been produced and analyzed for each thin-film system. Moreover, reference samples with certified elemental composition and thickness have been also available. This study is part of an interlaboratory comparison organized in the frame of standardization technical committee ISO/TC 201 “Surface chemical analysis.” Two laboratories have been analyzed by ED-EPMA (one laboratory standardless and one laboratory using both standardless and with standards variants) and one laboratory by μ-XRF (standardless and with standards). All the elemental compositions obtained with different methods are in very good agreement for the complete two sets of five samples each.
The characteristics of TiO2 coatings can greatly influence their final performance in large‐scale applications. In the present study, self‐assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with, for example, silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3‐aminopropyl)triethoxysilane (APTES) or (3‐aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino‐groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape, and specific surface area have been functionalized. Fourier‐transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), SEM/ energy‐dispersive X‐ray spectroscopy (EDS), XPS, Auger electron spectroscopy (AES), and Time‐of‐Flight (ToF)‐SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA.
This document is a collection of three JRC Technical Reports that together form the “NanoDefine Methods Manual”, which has been developed within the NanoDefine project ‘Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial’, funded by the European Union’s 7th Framework Programme, under grant agreement 604347. The overall goal of the NanoDefine project was to support the implementation of the European Commission Recommendation on the definition of nanomaterial (2011/696/EU). The project has developed an integrated empirical approach, which allows identifying a material as a nano- or not a nanomaterial according to the EC Recommendation. The NanoDefine Methods Manual consists of three parts: Part 1: The NanoDefiner Framework and Tools, which covers the NanoDefiner framework, general information on measurement methods and performance criteria, and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2: Evaluation of Methods, which discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3: Standard Operating Procedures (SOPs), which presents the 23 Standard Operating Procedures developed within the NanoDefine project. In this combined document, these three parts are included as stand-alone reports, each having its own abstract, table of contents, page, table and figure numbering, and references.
The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial'1 funded by the European Union's 7th Framework Programme, under grant agreement 604347.
In 2011 the European Commission (EC) published the recommendation (2011/696/EU) for a definition of the term 'nanomaterial'1, the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices.
The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano or non-nano material according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by:
- addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies.
Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the D50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context.
The NanoDefine Methods Manual consists of the following three parts:
Part 1: The NanoDefiner Framework and Tools
Part 2: Evaluation of Methods
Part 3: Standard Operating Procedures (SOPs)
Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool.
Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size.
Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 3.
The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial', funded by the European Union's 7th Framework Programme, under grant agreement 604347.
In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices.
The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by:
- addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms),
- developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies.
Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context.
The NanoDefine Methods Manual consists of the following three parts:
Part 1: The NanoDefiner Framework and Tools
Part 2: Evaluation of Methods
Part 3: Standard Operating Procedures (SOPs)
Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool.
Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size.
Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project.
The current document is part 2.
The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial', funded by the European Union's 7th Framework Programme, under grant agreement 604347.
In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices.
The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by:
- addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms),
- developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies.
Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context.
The NanoDefine Methods Manual consists of the following three parts:
Part 1: The NanoDefiner Framework and Tools
Part 2: Evaluation of Methods
Part 3: Standard Operating Procedures (SOPs)
Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool.
Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size.
Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project.
The current document is part 1.
This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775.
One of the objectives of the EU Project EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials & Nanotechnologies) was to test and benchmark the services in order to check their relevance to address identified stakeholder needs, but also to evaluate the governance of the structure delivering the proposed services. The aim is to demonstrate the technical relevance of the services and the overall open structure organisation, including governance rules and operating procedures, by answering relevant identified questions (case studies) selected by a panel of stakeholders. Therefore, a significant part of the project will be devoted to this demonstration of the operational and functional basis of the organized network.
Conclusions and perspectives
(2020)
This chapter briefly summarizes the methods selected within this book for the characterization of nanoparticles with regard to commonly accessible properties: nanoparticle size and size distribution, shape, surface area, surface charge, aggregation state, structure, chemical composition, surface chemistry, and nanoparticle number concentration. Current progress of measurement and analysis, as far as possible according to standard operation procedures, has been the focus of this work. A number of new and less commonly used methods have not been covered, and we outline some of these in this chapter. Future challenges such as automated measurement and analysis, read-across approaches for the prediction of properties, knowledge of measurement uncertainties, the need for certified reference materials, and the necessity to complement measurements methods to obtain more reliable results are covered, and the unmet measurement requirements for real-world nanoparticles are described.