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Joint Research Centre the European Commission's in-house science service Serving society Stimulating innovation Supporting legislation The EU Commission's definition of nanomaterial: implementation and technical challenges Hubert Rauscher Madrid, 30 June 2016

JRC Role Facts & Figures The European Commission's science and knowledge service, established 1957 Independent, evidence-based scientific and technical support for many EU policies 6 directorates in 6 locations new structure as of 1 July 2016 [Nano: Directorate for Health, Consumers and Reference Materials, Ispra & Geel] Around 3000 staff, including PhDs and visiting scientists

Outline Nanomaterials in EU legislation - Regulatory definition of nanomaterial Challenges for the implementation - how to identify nanomaterials by measurements The NanoDefine project - an integrated approach supporting the implementation of the EC nanomaterial definition

Definition of Nanomaterial Regulatory context An EU wide regulatory definition is needed for to classify a class of materials of regulatory interest legal clarity across legislations Recommendation of the European Commission - 2011 Particulate materials, size is the only criterion (1-100 nm) 50% threshold (based on particle numbers) Derogation for: fullerenes, SWCNT, graphene flakes Volume specific surface area (>60m 2 /cm 3 ) additional possible criterion Review of the definition - 2016 Conclusions being finalised by the Commission Possible revision

Definition of Nanomaterial Implementation Implementation in Regulations Biocides Regulation - 2012 Medical Devices Regulation (proposal) REACH (Annexes) planned Amendment of existing regulatory nanomaterial definitions Cosmetics Regulation - 2009 Novel Food Regulation 2015 (see also Food Information Regulation) Guidance for practical implementation in development 2016-2017 Size measurement Particle size distribution

EU legislation with relevance for nanomaterials Regulatory framework Definition Approval procedure Safety assessment Labelling REACH (Chemicals) Regulation 1907/2006 Biocidal Products Regulation 528/2012 Cosmetic Products Regulation 1223/2009 Novel food Regulation (2015/2283) () Food additives Regulation 1333/2008 Plastic Food Contact Materials Reg. 10/2011 Active & Intelligent FCM Regulation 450/2009 Food Info Provisions Regulation 1169/2011 Medical Devices Proposal COM(2012) 542 Guidance H. Rauscher, Madrid, 30 June 2016

Some resulting measurement requirements "Nanomaterial" means a natural, incidental or manufactured material containing particles, in an unbound state or as an aggregate or as an agglomerate and where, for 50 % or more of the particles in the number size distribution, one or more external dimensions is in the size range 1 nm - 100 nm. Determination of the constituent particles of the material The constituent particles are often aggregated or agglomerated Determination of the external dimensions of the (constituent) particles Address particle size distribution (by number) e.g., Determination whether 50% or more of the particles have an external dimension in the size range 1-100 nm

Example: Size ZnO (NM 110) Method Size measurement on dry powders NM-110 [nm] TEM, Feret average 147 ± 149 SEM, Feret 151 ± 56 Size measurement on suspensions DLS, mean particle size 275 ± 4 CLS (in distilled water) 193 ± 3 XRD (crystallite size) 41.5 The size values are method-defined From: EUR 25066 EN Non-spherical, polydisperse, aggregated particles Issues: Representative sample Dispersion Sample preparation Statistical evaluation

Methods for measuring particle size distribution (by number) Counting methods (such as electron microscopy) measure particle by particle can provide number based size distribution high number of particle needs to be measured Ensemble methods (such as light scattering) intensity weighted sizes Conversion to number-based size distributions necessary Fractionation methods (such as field flow fractionation) Particles sorted by size can deal with polydisperse samples can be coupled with counting methods

LNE dossier P156452, 9 June 2016 (EM & ICP-OES) Biscuits chocolate glazing Guacamole spice mixture

Implementation of the EC nanomaterial definition: The need for an integrated and coherent approach Situation Methods have to meet certain requirements nanospecific aspects Available methods cover requirements to varying degree Material type / size range / agglomerates, aggregates / size distributions / No single method covers all requirements for all materials Combination of methods is promising Validated nanospecific methods & reference materials needed Proof that a material is not a nanomaterial (?) The way forward Develop a robust, broadly applicable and widely accepted implementation approach Develop available methods further with a view to the EC NM definition Develop practical guidance EUR 25404 EN

The NanoDefine project Goal: to provide the affected industries and regulatory agencies with the tools that support the implementation of the EC definition of nanomaterial in all relevant regulatory contexts. Definition issues addressed size range 1 100 nm agglomerates, aggregates complex materials number based size distribution; conversion from other metrics cost-efficiency Objectives Working on real world test materials (industrial raw materials, products) Comparative evaluation of techniques uniform criteria Development, validation, standardisation of key methods; targeted instrument + software improvements Guidance to end-users (manufacturers and regulators)

The NanoDefine project - Implementation Decision-support flow scheme Material properties Requirements Purpose Methods characterisation Existing data Input Material classification Available methods - characteristics Existing data Sample preparation options Sample preparation Tier 1: Screening method options Nano / nonnano? Plausibility check? Tier 2: Confirmatory method options, if required Tiered approach Tier 1: "screening methods" Tier 2: "confirmatory methods" Including Performance criteria Method evaluation Method development (selected techniques) Non- Nano Nano / nonnano? Plausibility check? Nano NanoDefine Products E-tool User-friendly Semi-automated Open for amendments Methods Manual Practical, coherent guidance Print and online

Decision support flow scheme with VSSA screening [under review for publication] 16

NanoDefine outputs Product The NanoDefiner e-tool: Standardised semiautomated procedure for method selection and NM classification for the most economic implementation of the definition The NanoDefine Methods Manual: Technical guidance on the use of available methodologies Standard operation procedures (SOPs) for analysis of materials and products Calibration standards and reference materials Technology transfer of developed methods to end users CEN/ISO work items for key methods Planned release Project end First edition available Final edition at project end first versions included in the Methods Manual at project end at project end and via workshops Latest: public workshop 17 June 2015, Brussels at project end

Outlook Review possibly revision of the NM definition REACH adaptation of annexes Novel food & cosmetics adaptation of the definition Guidance on implementation in development

The JRC Competence Group "Nanosafety and Regulatory Methods" Thank you!