An introduction to standards and standardization for nanotechnologies

1. An introduction to standards and standardization for nanotechnologies Dr Peter Hatto, Chairman UK NTI/1 and ISO TC 229 Nanotechnologies Standardization committees

2. Overview • Why standards for nanotechnologies are important • Standards and standardization • Why is nanotechnology important? • What needs standardizing and why? • Current standardization committees • Existing standards, standardization projects and proposals; • Pre- and co-normative research to support future needs; • Support for possible regulation

3. Why standards for nanotechnologies are important • Standards will help to ensure that nanotechnology is • developed and commercialised in an open, safe and • responsible manner by supporting: • safety testing, legislation and regulation • worker, public and environmental safety • commercialisation and procurement • patenting and IPR • communication about the benefits, opportunities and potential problems associated with nanotechnologies • This will be achieved by providing agreed ways of: • Naming, describing and specifying things • Measuring and testing things • Health and environmental safety testing, risk assessment and risk management

4. Standards • Standards can be of two types: • Metrological standards: length, mass, time, quantity of matter – primary and secondary standards • Written standards • Written Standards provide agreed ways of: • Naming, describing and specifying things • Measuring and testing things • Managing things e.g. quality and environmental management: ISO 9001 and ISO 14000 • Reporting things as in e.g. proposed ISO 26000 (Social Responsibility) • To: • support commercialisation and market development • provide a basis for procurement based on technical requirements and quality/environmental management • support appropriate legislation/regulation • Can be NORMATIVE, defining what MUST be done in e.g. a specific test • method, or INFORMATIVE, providing information only. • Standards are VOLUNTARY unless called in a contract or regulation. • Standards provide a means of “validated quantification”

5. Standards • Standards are: • Ubiquitous – covering such things as shoe sizes, nuts and bolts, petrol grades, warning signs, pipes and fittings, fire extinguishers, gas cylinders, electrical sockets and plugs, steel specifications,………….. • Virtually invisible to “the man in the street” – there are over 15,000 International Standards, many with multiple parts; • But are absolutely critical to our modern way of life – covering things such as CDs/DVDs, internet protocols, credit cards, pin numbers, quality and environmental management,…………………………….

6. and standardization • Standards can be: • FORMAL – developed by independent experts working under the auspices of a National, Regional or International standards body • AFNOR, BSI, DIN, JIS, ………………… • CEN, CENELEC, ETSI….. • ISO, IEC & ITU • INFORMAL – developed by a SDO (Standards Development Organisation) • ASTM, IEEE, SAE, SEMI, VDI…(>600 SDOs IN US) • PRIVATE – developed by a company or trade association FORMAL standards are: • PROPOSED, DEVELOPED AND APPROVED by the members of the standards body • Based on CONSENSUS (i.e. no sustained opposition) not necessarily unanimity.

7. Functions of standards • Standards can perform any of the following four functions: • Interoperability/Compatibility • as with e.g. nuts and bolts, railway gauges, electrical plugs and outlets, and interoperability standards for computers and telecommunications systems • Quality • Fitness for purpose or safety • Variety reduction/optimization (based on best practice) • E.g. shoe sizes, suit sizes – leading to mass production and price reduction • Information/Measurement • Test and measurement methods for describing, quantifying and evaluating product attributes such as material, processes and functions • DIN has reported that in Europe standardization adds approximately 1% to the value of gross domestic product and that the added value generated by standardisation is at least as important as the value generated by patents! – see “Economic benefits of standardization” Published by DIN German Institute for Standardization e. V.

8. E E WG E E Standardization projects Extent of ISO System 151 full-time posts More than 14941 ISO Standards Secretary Chairman 734 Secretariats held by 37 countries About 190 TCs Ch C E 544 SCs Convenor C Standardization projects 2188 WGs version 3, Jan 10 2007 4176 active projects (30 June 2005)

9. Development of International Standards Process accommodates special needs NWIP from member organisation Approval – at least 5 P members agree to participate and >50% of members in favour Also ISO/TR for informative documents version 3, Jan 10 2007

10. Why is nanotechnology important? US Interagency Working Group on Nano Science, Engineering and Technology (IWGN) workshop on Nanotechnology Research Directions (Sept. ’99): “nanotechnology will be a strategic branch of science and engineering for the 21st century, one that will fundamentally restructure the technologies currently used for manufacturing, medicine, defence, energy production, environmental management, transportation, communication, computation and education.” US NSF report on “SOCIETAL IMPLICATIONS OF NANOSCIENCE AND NANOTECHNOLOGY” March 2001: “the impact of nanotechnology in the 21st century is likely to be at least as significant for health, wealth and security as the combined influences of antibiotics, integrated circuits and polymers.” Projected world-wide market for n-t enabled products will be >$500 Billion but <$3 trillion by 2015 “It is estimated thatNanotechnology is presently at a level of development similar to that of computer/information technology in the 1950s” (Nanostructure Science and Technology: A Worldwide Study, WTEC Panel report, 1999)

11. The challenges The Interagency Working Group on Nanotechnology workshop in 1999 concluded: “while recognizing nanotechnology’s potential to spawn an industrial revolution in coming decades, the consensus was that the challenges ahead in basic discovery, invention and eventual manufacturing are formidable. New methods of investigation at the nanoscale, novel scientific theories, and different fabrication paradigms are critical.” • “Nanotechnolgy will only become a coherent field of endeavour through the confluence of three important technological streams: • New and improved control of the size and manipulation of nanoscale building blocks; • New and improved characterization (spatial resolution, chemical sensitivity, etc) of materials at the nanoscale; • New and improved understanding of the relationship between nanostructure and properties and how these can be engineered” • And don’t forget safety and consumer acceptance!!

12. Needs for standardization • To support commercialisation and market development • To provide a basis for procurement – technical/quality/environmental management • To support appropriate legislation/regulation Challenges: currently there are: • No internationally agreedterminology/definitions for nanotechnology(ies). • No internationally agreedprotocols for toxicity testing of nanoparticles. • Nostandardized protocols for evaluating environmental impact of nanoparticles. • Existing “methods of test” may not be suitable for nanoscale devices and nanoscale dimensions. • Measurement techniques and instruments need to be developed and/or standardized. • New calibration procedures and certified references materials are neededfor validation of test instruments at the nanoscale. • Multifunction nanotechnology systems and devices will need new standards. Partial solutions • But some existing standards may be applicable e.g. for chemical analysis and imaging (ISO TCs 201 and 202) and particle detection/sizing (ISO TC 24) • Hence there is a need for a dedicated committee to coordinate standards development with relevant TCs, and to develop standards where no TC exists, or where the existing TC does not have the necessary resources.

13. A brief history of standardization for nanotechnologies • 12/03: - China establishes United Working Group for Nanomaterials standardization - UK proposes CEN/BTWG to develop strategy for European standardization in nanotechnologies. • 03/04: Proposal for CEN/BTWG approved – UK awarded secretariat • 05/04: UK establishes NTI/1 national committee • 08/04: ANSI forms Nanotech Standards Panel in response to a request from OSTP • 10/04: UK starts work on PAS 71 - vocabulary for nanoparticles • 11/04: Japan establishes study group for nanotech. standardization • 12/04: China publishes 7 national nanotech standards • 01/05: UK submits proposal for an ISO committee • 04/05: - China implements published nanotech standards - ASTM International approves establishment of E56 committee - ISO ballot on UK proposal approved – 30 votes to nil

14. 06/05: - ISO confirms establishment of TC 229 – UK secretariat & chair. - UK publishes PAS 71, vocabulary – nanoparticles (free from www) - CEN/BT/WG 166 delivers European strategy to CEN/BT • 11/05: - Inaugural meeting of ISO TC 229 in London. - CEN establishes CEN/TC 352 – Nanotechnologies – UK Chair & Secretariat • 01/06: UK submits first NWIP to TC 229 – vocabulary for nanoparticles • 03/06: IEC receives proposal for new TC for Nanotechnologies • 04/06: First meeting of CEN/TC 352 (agreed to collaborate closely with ISO/TC 229) • 05/06: IEC agrees to establish TC 113 in the field of nanotechnologies– issue of coordination with ISO/TC 229 • 06/06: 2nd meeting of ISO/TC 229, Tokyo • 12/06: 3rd meeting of ISO/TC 229, Seoul • 06/07: 4th meeting of ISO/TC 229, Berlin • 12/07: 5th meeting of ISO/TC 229, Singapore (jointly with IEC/TC 113) To date national committees established in Australia, Canada, China, France, Germany, India, Iran, Italy, Japan, Korea, Russia, Singapore, Thailand, UK, US………,

15. UK NTI/1 Committee (as of September 2006) • Established May 2004 - second (after China) national committee to be formed • Develops national standards and other standardization documents – 1 published “Publicly Available Specification” (PAS) – PAS 71 vocabulary – nanoparticles; currently preparing 2 Published Documents (Guide to safe handling and disposal of nanoparticles and Guide to specification of nanomaterials) and 7 PASs (Guide to labelling, Terminologies for medical, health and personal care applications of nanotechnologies, nanomaterials, carbon nanostructures, nanofabrication, measurement terms, and the bio-nano interface). • Provides UK input to international committees: ISO/TC 229, IEC/TC 113 and CEN/TC 352 • Meets four times per year • Members represent key stakeholders from Defra, DTI, EA, FSA, HSE,HSL, IOM, ION, IoP, RSC, Durham University, NIA, CERAM, Qinetiq, …………. • For further details contact the secretary Ms Anne Cassidy anne.cassidy@bsi-global.com or see www.bsi-global.com/nanotechnologies

16. European Committee for Standardization committee CEN/TC 352 - Nanotechnologies • Established November 2005 following proposal from UK and recommendations from CEN/BTWG 166 • UK Chair and Secretariat • Works closely with ISO/TC 229 and “topics of mutual interest will be developed under the ‘Vienna Agreement’ with ISO lead”. • Developing work programme in areas of specific interest to Europe and areas that will be relevant to European legislation. • Currently 3 New projects: • Format for reporting the engineered nanomaterials content of products (to be published as a CEN/TS); • Guide to nanoparticle measurement methods and their limitations (CEN/TR) • Guide to methods for nano-tribology measurements (CEN/TR).

17. International Organisation for Standardization committee ISO/TC 229 - Nanotechnologies • Established in June 2005 with UK Chair and Secretariat • 37 members – 29 “P” and 8 “O” (see http://www.iso.org/iso/en/stdsdevelopment/tc/tclist/TechnicalCommitteeList.TechnicalCommitteeList) • Liaisons with 15 other ISO TCs and 6 external bodies – IEC/TC 113, CEN/TC 352, Asia Nano Forum, EC JRC, OECD and VAMAS • Exploring additional external liaisons for emerging economies

18. International Electrotechnical Commission committee IEC/TC 113 – “Nanotechnology standardization for electrical and electronic products and systems” • Established June 2006 with US Chair and German secretariat • 26 members - 15 “P” and 11 “O” • First meeting March 2007 • Agreed to establish two Joint Working Groups with ISO TC/229: • JWG 1 – Terminology and nomenclature • JWG2 – Measurement and characterization • Together with a third Working Group: • WG3 – Performance

19. ISO TC 229 adopted Scope: • “Standardization in the field of nanotechnologies that includes either or • both of the following: • Understanding and control of matter and processes at the nanoscale, typically, but not exclusively, below 100 nanometres in one or more dimensions where the onset of size-dependent phenomena usually enables novel applications; • Utilizing the properties of nanoscale materials that differ from the properties of individual atoms, molecules, and bulk matter, to create improved materials, devices, and systems that exploit these new properties • Specific tasks include developing standards for: • terminology and nomenclature; metrology and instrumentation, including • specifications for reference materials; test methodologies; modelling and • simulation; and science-based health, safety, and environmental • practices.” • Note: Scope is further defined by the TC’s “Strategy Statement”

20. TC 229 – Structure/working areas SUPPORT FOR “REGULATION” PRODUCT AND PROCESS (sc) PRODUCT AND PROCESS (sc) PRODUCT AND PROCESS (sc) Terminology and Nomenclature (WG 1) “what you call it” - Convened by Canada Measurement and Characterization (WG 2) “How you measure/test it” – Convened by Japan Health, Safety and Environment (WG 3) “what effect it might have on health and the environment” – Convened by USA

21. TC 229 Work programme • Currently work items: • “Terminology for nanoparticles” for publication as an ISO/TS (WG 1) • “Health and safety practices in occupational settings relevant to nanotechnologies” for publication as an ISO/TR (WG 3) • “Endotoxin test on nanomaterial samples for in vitro systems” for publication as an International Standard (WG 3) New projects: • The Use of Transmission Electron Microscopy in the Characterization of Single-walled Carbon Nanotubes • The use of Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Analysis (EDXA) of Single Wall Carbon Nanotubes (SWCNTs) • Technical Specification for the Use of UV-Vis-NIR absorption spectroscopy in the Characterization of Single-Walled Carbon Nanotubes (SWCNTs) • Technical Specification for the use of NIR-Photoluminescence (NIR-PL) Spectroscopy in the Characterization of Single-Walled Carbon Nanotubes (SWCNTs) • Generation of silver nanoparticles for inhalation toxicity testing • Monitoring of silver nanoparticles in inhalation exposure chambers for inhalation toxicity testing

22. TC 229 Work programme - 2 New Work Item Proposals: • Terminology and nomenclature for nanotechnologies — Framework and core terms • Use of Thermo Gravimetric Analysis (TGA) in the purity evaluation of Single Walled Carbon Nanotubes (SWCNT) • Use of Evolved Gas Analysis-Gas Chromatograph Mass Spectrometry (EGA-GCMS) in the Characterization of Single-Walled Carbon Nanotubes (SWCNTs) In December 2007 ISO/TC 229 completed its first survey of Standardization needs which identified 110 “high priority” topics, of which • 2 were relevant to WG 1, • 54 were relevant to WG 2, • 31 were relevant to WG 3, • 5 were relevant to a new WG on materials specifications, and • 18 were relevant to other Technical Committees. These results will form the basis of a Road Map for the future work of the committee.

23. Current and potential liaisons for ISO/TC 229 ISO/TC 122 Packaging ISO/TC 206 Fine ceramics ISO/TC 217 Cosmetics ISO/TC 119 Powder metallurgy ISO/TC 215 Health Informatics ISO/TC 84 Devices for administration of medical products and intravascular catheters ISO/TC150 Implants for surgery ISO/TC 172 Optics and photonics ISO/TC 168 Prosthetics and orthotics ISO/TC 107 Metallic and other inorganic coatings ISO/TC 91 Surface active agents ISO/TC 59 Building construction ISO/TC 61 Plastics ISO/TC 212 Clinical laboratory testing and in vitro diagnostic test systems ISO/TC 35 Paints and varnishes ISO/TC 225 Market opinion and social research ISO/TC 34 Food products ISO/TC 38 Textiles ISO/TC 215 Environmental management ISO/TC 28 Petroleum and petroleum products ISO/TC 180 Solar energy ISO/TC 184 Industrial automation systems and integration ISO/TC 203 Technical energy systems BIOMEDICAL MATERIALS EXTERNAL LIAISONS RISK/HS&E NANO-PARTICLES METROLOGY AND CHARACTERIZATION ISO/TC 48 Laboratory equipment ENERGY version 3, Jan 10 2007 Version 4, Mar 2007

24. Current nanotechnology standards • Only National standards to date: • China – 12 National standards published and adopted: Terminology: • GB/T19619-2004 Terminology for nanomaterials Sizing: • GB/T13221-2004 Nanometer powder - Determination of particle size distribution - Small angle X-ray scattering method (ISO/TS13762) • GB/T19587-2004 Determination of the specific surface area of solids by gas absorption using the BET method (ISO 9277:1999) • GB/T19627-2005 Particle size analysis - Photon correlation spectroscopy (ISO 13321:1996) • GB/T 15445.2-2006 Representation of results of particle size analysis—Part 2:Calculation of average particle sizes/diameters and moments from particle size distributions（ISO 9276－2：2001,IDT） • GB/T 15445.4-2006 Representation of results of particle size analysis—Part 2:Characterization of a classification process（ISO 9276－4：2001,IDT） • GB/T 20307-2006 General rules for nanometer-scale length measurement by SEM • GB/T 20099-2006 Sample preparation dispersing procedures for powders in liquids Nano-material specificiations: • GB/T19588-2004 Nano-nickel power • GB/T19589-2004 Nano-zinc oxide • GB/T19590-2004 Nano-calcium carbonate • GB/T19591-2004 Nano-titanium dioxide • UK – PAS 71: 2005 – Vocabulary – Nanoparticles • Several standards (International, regional and national) that also apply to the nanoscale

25. Terminology and nomenclature for nanotechnologies • One current document specific to nanoparticles: • UK PAS 71 - available for free download at http://www.bsi-global.com/Manufacturing/Nano/Download.xalter • For fullerenes (nanoparticles or molecular structures???), there is a provisional nomenclature developed by IUPAC - http://www.chem.qmul.ac.uk/iupac/fullerene/#r3 • Chinese National standard for nanomaterials: GB/T19619-2004 Terminology for nanomaterials • ASTM E56 has published a terminology for nanotechnology: E2456-06 Terminology for Nanotechnology • Approach recommended by UK: • Develop series of terminologies/vocabularies in various topic areas, which together will form a terminology for nanotechnologies. This will : • allow consensus to be achieved more easily, allowing earlier publication; • enable changes in one topic area to be implemented without altering a substantial document; • allow documents to be developed in tandem with technology developments rather than trying to shoe horn a new technology into an existing terminology; • ISO TC 229 Work Item “Terminology and definitions for nanoparticles” approved April 2006.

26. Current UK (NTI/1) Work Items • 6 sector specific terminologies: • Medical, health and personal care applications of nanotechnology • The bio-nano interface • Carbon nanostructures • Nanomaterials • Nanofabrication • Common nanoscale measurement terms including instrumentation 3 guides • Guide to labelling of manufactured nanoparticles and products containing manufactured nanoparticles • Guide to safe handling and disposal of manufactured nanomaterials • Guide to specifying nanomaterials All documents will be published by the end of 2007 and will be made freely available on the www see www.bsi-global.com/nanotechnologies

27. Do we need a nomenclature for nanoparticles (nanomaterials)? • “a structured naming system that can allocate unique names to unique entities, which allows as-yet undiscovered entities to be similarly named, and which ideally allows the nature of all such entities to be determined from their name” • needs to provide recognisable added value in comparison to existing descriptions, without being so complex as to make it unusable; • must take account of range and complexity of nanoparticles / nanomaterials under consideration; • Perhaps easier to agree an ordered structure for describing nanoparticles containing e.g. • core composition and crystal structure; • composition of any deliberately applied surface layers; • any surface functionalization; • specific surface area; • particle shape descriptor; • and particle size distribution.

28. Pre- and co-normative research requirements: • Critical areas are risk/regulation: Development and delivery needed of: • test methods to detect and identify nanoparticles, and to characterize nanoscale materials and devices. • protocols for bio- and eco-toxicity testing, including protocols to evaluate effects of short term and long term dermal, nasal, oral and pulmonary exposure to, elimination of, and fate determination for nanomaterials and nanoscale devices. Work in these areas being undertaken by: SnIRC, INOS, ECVAM, CRM, EPA/NIOSH, Rice University, Nanosafe2, NANOTOX, etc. • protocols for whole life cycle assessment of nanoscale materials, devices and products. • risk assessment tools relevant to the field of nanotechnologies. • protocols for containment, trapping and destruction of nanoparticles and nanoscale entities. • occupational health protocols relevant to nanotechnologies, in particular for industries dealing with nanoparticles and nanoscale devices. • Collaboration with OECD Working Party for Manufactured Nanomaterials

29. Nanomaterial test methods needed for risk assessment/to support possible regulation Particle detection and measurement • Fast, accurate methods for particle “size” measurement in air, water, food and the environment: • Specific Surface Area (SSA) • Particle size distribution • Shape factor • Particulate density/Exposure • Work relevant to ISO TC 24 SC4 - Sieves, sieving and other sizing methods: Particle Characterisation, Size, Surface area and Zeta potential Identification of composition and surface functionalities, including any catalytic and enzymatic characteristics • “bulk” or “individual particle” measurements? • Work relevant to ISO TC 201 – Surface Chemical Analysis and ISO TC 202 – microbeam analysis

30. Other ISO TC’s with an interest in the area of risk and health effects of nanotechnologies • 34 - Food and food products • 94 - Personal safety – protective equipment • 122 - Packaging • 146 - Air quality (New TR published 2007: Workplace Atmospheres - Ultrafine, nanoparticle and nano-structured aerosols - Inhalation exposure characterization and assessment) • 147 - Water quality • 150 - Implants for surgery • 194 - Biological evaluation of medical devices • 207/SC 5 - Environmental management – life cycle assessment • 217- Cosmetics • TMB Working Group on Risk Management (Risk Terminology defined in ISO/IEC Guides 51 & 73)

31. The roles of ISO TC 229, IEC TC 113 and CEN TC 352 will be to identify requirements in cooperation with stakeholders, including industry, governments, regulators, OECD, the European Commission, and the public, to coordinate standards development with relevant TCs, and to develop standards where no TC exists, or where the existing TC does not have the necessary resources.