Developing Nano-Measurements And Standards The NIST Role

Developing Nano-Measurementsand StandardsThe NIST RoleAngela R. Hight Walker, Ph.D.angela.hightwalker@nist.govNational Institute of Standards and Technology

NIST: The National Measurement Institute for the USATo promote U.S. innovation and industrial competitiveness byadvancing measurement science, standards, and technology in waysthat enhance economic security and improve our quality of lifeNational Institute of Standards and Technology

NIST Nano EHS Program GoalsIn consultation and collaboration with our stakeholders,academia, government agencies and industry, we will: Provide a scientific basis to discover the health andenvironmental effects of nanotechnology Enable US industry to safely develop, exploit,commercialize nanotechnologiesNational Institute of Standards and Technology

NIST Motivation Health and environmental risks ofnanomaterials (real and perceived) areroadblocks for innovation andcommercialization of nanotechnology. Data quality inhibits the ability tounderstand, predict, and managepotential risks of engineerednanoscale materials. Lack of certainty in nanoscalemeasurements impacts regulatory andpolicy decisions.National Institute of Standards and Technology

NIST: Key Part of the Federal PlanNNI strategy addressing priority research on the environment,health, and safety (EHS) aspects of nanomaterials that have beenidentified in previous reports.NIST identified as the lead agency for:Instrumentation, Metrology andAnalytical Methods1. Develop methods to detect nanomaterials in biological matrices, the environment and theworkplace2. Understand how chemical and physical modification affect the properties of nanomaterials3. Develop methods for standardizing assessment of particle size, size distribution, shape structureand surface area.4. Develop certified reference materials for chemical and physical characterization ofnanomaterials5. Develop methods to characterize a nanomaterial’s spatio-chemical composition, purity, andheterogeneityNational Institute of Standards and Technology

Proposed NIST Workplan for NanoEHS1. Research and Innovation,*under development2. Nanomaterial Characterization, and Materials and measurement protocols for quantifying the typeand amount of nanomaterials in biological matrices, theenvironment, and the workplace Methods to understand the effect of modifications on theproperties of nanomaterials Measurement science for standardizing assessment ofnanoparticle size and size distribution, shape, structure, andsurface area Innovative technology to characterize a nanomaterial's spatiochemical composition, purity, and heterogeneity3. Validation of Toxicological Methods.National Institute of Standards and Technology

NIST ApproachReference MaterialsDocumentary StandardsMeasurement ScienceNational Institute of Standards and Technology

DefinitionsReference Material (RM):Material sufficiently homogeneous and stable with respect to one ormore specified properties, which has been established to be fit forits intended use in a measurement process.Certified Reference Material (CRM): (SRM NIST)Reference materials characterized by a metrologically validprocedure for one or more specified properties, accompanied by acertificate that provides the value of the specified property, itsassociated uncertainty, and a statement of metrological traceability.Property values are certified as traceable to an accurate realization ofthe unit in which the property values are expressed.Definition from the international organization for Standards (ISO)National Institute of Standards and Technology

Procedure for NIST (S)RM DevelopmentResearch Customer needs and market assessment indicate an(S)RM is required to address barriers to innovation Underpinning measurement science andtechnology Select materials and source, define property values,select measurement methods, establish testing planDevelopment Develop a prototype whose reference values are notnecessarily traceableProduction Process and package material, heterogeneity testing,generate certified, references and informationvalues, perform statistical analyses Generate COA or ROI and release (S)RMDevelopment and production stages typically take 2 yearsNational Institute of Standards and Technology

NIST Nano Reference MaterialsPresently Available:Polystyrene (down to 60 nm)Dimensional features on substratesMost Recent Addition:Gold nanopartcilesthree sizes; 10 nm, 30 nm, 60 nmNear Future:Single-walled carbon nanotubes (SWCNTs)likely three types; powder, pellet, liquidTiO2Future:Many under considerationNational Institute of Standards and Technology*Co-funded by NCI

NIST ApproachReference MaterialsDocumentary StandardsMeasurement ScienceNational Institute of Standards and Technology

International Standards LandscapeDifferent tools for different market needs: National participation models Treaty organizations; ISO, IEC Formality in process One country, one vote Direct participation models ASTM International, SAE, IEEE, etc. Direct link between technical experts and SDOs Corporate participation models Consortia and fora Wide range of processes and procedures allows flexibilityNational Institute of Standards and Technology

The Alphabet Soup of Nano StandardsNIST hosted a workshop in February 2008 to coordinatedocumentary standards development relevant to nanotechnology aswell as identify immediate and medium-term standards needs. ASTM International: E42, E56 IEC: TC113 IEEE-SA ISO TCs: 24/SC4, 146, 194, 201, 209, 213, 229 OECD–WPMN: Steering Groups 3, 6, 7 and 8 National Metrology Institutes (NMIs) SEMI Versailles Project on Advanced Materials and Standards (VAMAS)National Institute of Standards and Technology

Workshop Outcomes Greater communication and coordination within and between the various standardsdevelopment organizations and with interested metrology laboratories; The development of a centralized, maintained, searchable and freely accessiblerepository of information on existing standards and standardization projects in thefield; The development and introduction of a freely accessible and searchableterminology and definitions database; Wider participation of stakeholders in identifying and verifying standards needs; Consideration of all available standardization instruments from WorkshopAgreements through to full consensus standards and their equivalents in order toprovide stakeholders with relevant documents in a timely manner; Urgent and detailed consideration of the instruments needed to address currentconcerns and challenges in investigating the implications for human health andenvironmental safety of manufactured nanomaterials.National Institute of Standards and Technology

Nanotechnology Documentary StandardsISO TC 229: Nanotechnologies – established 2004Chair and Secretariat with UKThree working groups:WG 1: Terminology and nomenclature (Canada- Chair)WG 2: Measurement and characterization (Japan- Chair)WG 3: Health, Safety and Environmental Aspects ofNanotechnologies (USA/NIST – Chair)IEC TC 113: Nanotechnology standardization for electrical andelectronics products and systems – established 2006Secretariat: Germany, and Chair: USUS TAG recently formedEmphasis on strong liaison with ISO TC 229National Institute of Standards and Technology

Nanotechnology Documentary StandardsASTM E56: Standards and guidance for nanotechnology andnanomaterials - established 2004Six sub-committees:E56.01 Terminology & NomenclatureE56.02 Characterization: Physical, Chemical, and Toxicological PropertiesE56.03 Environment, Health, and SafetyE56.04 International Law & Intellectual PropertyE56.05 Liaison & International CooperationE56.90 ExecutiveE56.91 Strategic Planning and ReviewIEEE: Standards activities under IEEE Nanotechnology Counciladdressing materials, devices and system-level interoperabilityPart of IEEE Nanoelectronics Standards Roadmap initiative – March 2006Anticipatory standards philosophyStandards for nanoelectronics: IEEE P1650 standard test method for measurement of electrical properties of CNTsstandard approved and adopted in 2005 Work underway on development of standard method for characterization of CNTs usedas additives in bulk materials (IEEE P1690)National Institute of Standards and Technology

Nanotechnology Standards Examples 1ISO TC 229/WG2Matrix: Purity & Structural Properties, SWCNTsMethodPropertyCategoryMorphologyPurityLength (Lead:Japan)Wall structure,Tube structure,amorphous carbon,bundle thickness,metal catalystorientationcoatingsNon-carbon content(Quantitative)Non-carbonimpuritiesTube surfacecleanlinessNanotube and nonnanotube ength anddiameterTube diameter,metal cluster ead: USA, Colead:Korea)Chirality(Semi conductingtubes)Tub bundling orseparation (solution)Tube bundlingTube d:USA)Tube bundlingNon-CNT resAdditionalOther ParticipantsChinaChina, KoreaKoreaTBD:Canada and GermanyNational Institute of Standards and TechnologyKoreaUSAChinaNon-carbon res

Nanotechnology Standards Examples 2ISO TC 229/WG3TABLE 2. Focused List of Physico-Chemical Characteristics of EngineeredNano-Objects for Toxicological AssessmentMay 28, 2008 version Agglomeration state / Aggregation Composition (e.g., chemical composition and structure) Particle size / size distribution Purity/impurity Shape Solubility (hydrophobicity, lipo solubility, water solubility) Stability Surface area Surface chemistry Surface ChargeNational Institute of Standards and Technology

Nanotechnology Standards Examples 2ISO TC 229/WG3TABLE 2, Focused List of Physico-Chemical Characteristics of EngineeredNano-Objects for Toxicological AssessmentMay 28, 2008 version Agglomeration state / Aggregation Composition (e.g., chemicalcomposition and structure) Particle size / size distribution Purity/impurity Shape Solubility (hydrophobicity, liposolubility, water solubility) Stability Surface area Surface chemistry Surface ChargeProject 4Physical Chemical properties necessary pre-requisite properties – review existing non-OECDTesting methods (national testing methods, ISO, CEN, ASTM, JISetc. Agglomeration/ aggregation Length Catalytic propertiesCompositionConcentration (needs to be defined)Crystalline phaseDustiness PurityShapeSpecific surface areaSurface chargeSurface chemistry Fat solubility/ oleophilicityGrain sizeHydrodynamic size/particle sizemeasurement/ distribution Water solubility/hydrophilicityZeta potential2008 May @ISO TC229WG3National Institute of Standards and Technology for Official Use Only

NIST ApproachReference MaterialsDocumentary StandardsMeasurement ScienceNational Institute of Standards and Technology

Nanomaterial CharacterizationEnvironment Matters!More than ONE measurement is necessary!Characterization along the entire nanoparticle pathway is criticalfor scientific understanding toxicology responseWhat is it?How much of “it” is there? As received As dispersed As inhaled In matrix In cells In organs In bodiesNational Institute of Standards and Technology

Nanomaterial CharacterizationIdentify the fundamental properties ofthe nanomaterialsIsolate the nanomaterial for studyNational Institute of Standards and Technology

Intrinsic PropertiesQuantum DotsClustering and coatings change PLC1C3C5C7C11C13C15C20C25C30C35C40C501000Intensity [A.U.]900800700600500400300200Length matters1000Carbon Nanotubes540560580600620640660Wavelength [nm]Magnetic NanopartcilesCooperative behavior and stabilityNational Institute of Standards and Technology