Current Research and Development of Nanometrology in Thailand “Experience and Practices in the Testing, Characterization, Standardization and Certification of Nanoproducts” Annop Klamchuen Head of Nano Characterization Laboratory (NCL) National Nanotechnology Center (NANOTEC), Thailand Outlines 1. Current Status of Nano Products 2. Nano Products Characterization - Guidelines & Best Practices from THAILAND – 3. Important of Traceability -Preliminary Work on Inter-Laboratory Comparison- 4. Certification -Best practices and experiences from THAILAND - Nano Products in Market Place Many nano products are being developed and marketed without detailed characterization nor prior review and approval of their efficacy and safety. Characterization & Regulatory Gaps of Nano Products • No agreed protocols for physico-chemical characterization • Existing ‘methods of test’ may not be suitable for nanoscale devices and dimensions • Measurement techniques and instruments need to be developed and/or standardized • Calibration procedures and CRMs needed for validation of test instruments at nanoscale Nanotechnology Value Chain Nanomaterials Nanointermediates Nano-enable products Finished goods Nanoscale structures in Intermediate incorporating unprocessed form products with nanoscale features nanotechnology … Needs !! Test methods, Instruments, Standards, Safety Nanotechnology may become a new non-tariff barrier LACK OF INFORMATION INFORMATION OF THE TEST ITEM • WHICH PART IS CLAIMED NANO ? • COMPOSITION OF THE NANO • FUNCTION CLAIMED WHERE IS MY NANOMATERIALS ? NATIVE STATE > > COMPLEX MATRIX NATIVE STATE > > COMPLEX MATRIX PURE NANOMATERIALS Sample 15 Sample 28 Sample 32 Sample 55 WHICH INSTRUMENT BEST ? DLS TEM SEM AFM WHICH STANDARD METHOD ? Test Method Titles ISO 22916: 2011 Antimicrobial products – Test for Antimicrobial Activity and Efficacy JIS Z 2801: 2006 Test for Antimicrobial Activity of Plastics AATCC 100 (2004) Assessment of Antimicrobial Finishes on Textile Materials Determining the Antimicrobial Activity of Immobilized Antimicrobial Agents under ASTM E2149-10 Dynamic Contact Conditions CLSI M7-A7 MIC (2006) Methods for Dilution Antimicrobial Susceptibility Tests for Bacteria that Grow Aerobically AATCC 147 (2011) Antibacterial Activity Assessment of Textile Materials: Parallel Streak Method JIS L 1902: 2008 Testing for Antibacterial Activity and Efficacy on Textile Products NCCLS M2-A6 (DISK) Antimicrobial Disk Susceptibility Tests NaIonal Advanced Nano7characterizaIon Center (NANC) Flagship OUR FACI,ITIES Advanced OpCcal Microscopy Nano Imaging Laboratory & Spectroscopy 0aboratory NanoparCcle DetecCon & Sizing 0aboratory Integrated NanoMaterials AnalyCcal NanoChemistry NanoProduct CuncConality & Characterizaon 0aboratory 0aboratory SpeciDcaon 0aboratory Nanoproduct safety Laboratory FlagshipD NanoMARKS 䇾Nanometrology䇿 & 䇾Nanosafety䇿 Co-R&D Nano-characterization Laboratory (NCL) Nano Safety and Risk Assessment Laboratory Flagship (SRA) NANC NANOTEC Protocol Standard E Stakeholder panel E Reference Materials E Sign an 䇾NDA䇿 E InterElab comparison E Representave from NAN8IEC E Gorkshop and Training E Gorkshop and training 䇾Micrometrology䇿 & 䇾Chemical safety䇿 Naonal Instute of Metrology Thailand Tesng of Products Containing Nanomaterials Thailand is presently establishing of standard tesCng and characterizaon services to speciDc reRuirements of targeted industrial sectors Food Cosmec Petrochem. Texle Assay Cascade Protocols 1. PhysicoEchemical characterizaon of nanomaterials 2. CuncConality N Performance of nanoproducts 3. Safety assessment of nanomaterials Test Parameters Size Composion AnC1acterial acCvity Skin irritaonN corrosion Shape Surface chemistry Gater repellent acCvity CytotoPicity Surface area Surface ac97ity Etc. PhototoPicity Agglomeraon state Crystal structure GenotoPicity Structure Solu1ility EcotoPicity CASCADE ANALTSIS OF NANOPROSUCT Sectors Assay Cascade Protocols FoodsM - Physical758emical characteriza/0n of nanomaterials - FuncIonality M Performance of nanoproducts Food AddiIves M - Release test Agricultural products - Biological and ce227based model assays - Cytotoxicity - AbsorpIon - MetabolismD interacIon with hepaIc enzyme - Immunotoxicity - Genotoxicity (Comet assay and micronucleus assay) - Physical758emical characteriza/0n of nanomaterials - FuncIonality M Performance of nanoproducts Paints / Coa/1g - Release test - Health: Cell‐based model assays - Penetra/0n test - Acute toxicity assay - Immunotoxicity assay - Genotoxicity (Comet assay and micronucleus assay) - Environment: Ecotoxicity CASCADE ANALTSIS OF NANOPROSUCT Sectors Assay Cascade Protocols Cosmecs/ Herbal • Physical758emical characteriza/0n of nanomaterials products M Medical • FuncIonality M Performance of nanoproducts - Biological and ce227based model assays Devices - Skin penetraIon test (in vitro) - Acute skin irritaIon test (in vitro) - Cytotoxicity (in vitro) - ROS assay (in vitro) - Immunotoxicity (in vitro) - Genotoxicity (Comet assay and micronucleus assay) Texles & Clothing - Physical758emical characteriza/0n of nanomaterials - FuncIonality M Performance of nanoproducts - Release test - Biological and ce227based model assays - Acute skin irritaIon test (in vitro) - Cytotoxicity (in vitro) - ROS assay (in vitro) - Immunotoxicity (in vitro) - Genotoxicity (Comet assay and micronucleus assay) CASCADE ANALTSIS OF NANOPROSUCT Sectors Assay Cascade Protocols - Physical758emical characteriza/0n of nanomaterials Petrochemicals - FuncIonality M Performance of nanoproducts - Release test - Biological and ce227based model assays - Cytotoxicity - AbsorpIon - MetabolismD interacIon with hepaIc enzyme - Immunotoxicity - Genotoxicity (Comet assay and micronucleus assay) Computer hardware & - Physical758emical characteriza/0n of nanomaterials Electronic devices - FuncIonality M Performance of nanoproducts - MicroM Nanostructure - Surface chemistry, - Chemical composi/0n - Contamina/0n - Failure analysis 5S Factor S Size S Shape S Surface area S Surface chemistry S Solubility Nanoparcle Characterizaon 7%Supplementary Comparison on NanoparIcle Size Organizer: Asia PaciXc Metrology Programme (APMP) NIMT Reference MaterialsD Gold Nanoparcle, Silver NanoparIcle, Polystyrene nanoparcles SpeciXc Measurements InstrucIons for S,S, TEM, SEM and AFM Comparison Results Inter7laboratory comparison on NanoparIcle Size Measurement (APMP.,7S5) Organizer: Asia PaciXc Metrology Programme (APMP) REFERENCE MATERIALSD GO,S NANOPARTIC,E SI,VER NANOPARTIC,E PO,TSTTRENE NANOPARTIC,ES Specific Measurements Instructions for DLS, SEM and AFM ISO/IEC 17025 Certification Categories Scope 1 : Particle size analysis -Dynamic light Scattering (DLS) Scope 2 : Plastics -Measurement of antibacterial activity on non-porous surfaces Scope 3 : Particle size analysis – Image analysis by Scanning Electron Microscope (SEM) VO,UNTARY CERTIFICATIOND Nano Q S Nano Q is a certified quality mark for nano products which are certified by Nanotechnology Association of Thailand. S Motivation to Have Nano Q S Increase Public Trust: Facilitate healthy development of nanotechnology S Protect Consumer: Avoid waste money S Protect Good Companies: Eliminate unfair competitions S Facilitate Trade: Stimulate economic growth CRITERIA FOR PROSUCT CERTIFICATION (NANO Q) MANSATORY CERTIFICATION MU,TI7STAKERO,SER ENGAGEMENT interlab. comparison NANOMETRO,OGT STANSARDIZATION TESTING ,AB REGU,ATION CERTIFICATION M ,ABE,ING REACR nanomaterials ICCR cosmec direcve NanoQ Textile / Paints/Coating / Plastics etc. .