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Reference Material Needs to Support Nanometrology and Risk ReferenceReference materialmaterial needsneeds toto supportsupport nanometrologynanometrology andand riskrisk assessmentassessment ofof engineeredengineered nanoparticlesnanoparticles MartinMartin HassellHassell öövv EnvironmentalEnvironmental NanochemistryNanochemistry group,group, DepartmentDepartment ofof Chemistry,Chemistry, UniversityUniversity ofof Gothenburg,Gothenburg, SwedenSweden OutlineOutline Nanotechnology and nanomaterials Brief intro and definitions Benefits and risks Nanometrology Measurement needs in risk assessment Physico-chemical characterization and analysis • Which properties and measurands? Reference nanomaterials Needs in nanometrology • Calibration artifacts and reference nanoparticles • State-of-the-art - what´s special about nano-CRMs • Future needs Reference material needs for toxicology NanotechnologyNanotechnology Solid matter change properties and behavior at the small nanometer scale Optical, electronic, interfacial, crystalline properties often change Specific surface area, reactivitiy, catalitic activity Can be utilized in novel functional materials Energy production & storage, IT, paint & coatings, cosmetics, food, health & medicin Nanotechnology is also much more than new nanomaterials Incl. instrumentation to study these small scales PropertyProperty changechange asas functionfunction ofof sizesize Smallest Largest Cadmium Selenide Felice Frankel Felice “Quantum Dots” © SomeSome ISOISO definitionsdefinitions Nanotechnology: application of scientific knowledge to manipulate and control matter in the nanoscale in order to make use of size- and structure-dependent properties and phenomena, as distinct from those associated with individual atoms or molecules or with bulk materials Nanomaterials: material with any external dimension in the nanoscale (~1-100nm) or having internal structure or surface structure in the nanoscale Nanostructured materials • Aggregates, nanoporous, ceramics, surface nanostructured etc Nanoobjects • Nanoparticles (all three dimensions in nanoscale) • Nanofibres (2 dimensions in nanoscale) • Nanoplates BenefitsBenefits Nanotechnologies are forecasted to have a major impact in all areas of the future society Contribute to solve the grand challenges Energy production (e.g. Photovoltaics) Energy storage (e.g. Batteries and fuel cells) Carbon capture Lighter and stronger vehicles Faster and smaller computers (e.g quantum or spintronics) Water treatment Greener chemical production Efficient healthcare (e.g. better treatments and diagnostics) But you have to know what you are producing Measure, image, analyse Tasks for the Nanometrology field NanometrologyNanometrology Nanometrology is the science of measurement at the nanoscale level. “Nanometrology must be seen as indispensable part of all kinds of nanotechnology” Novel subfield of metrology that has large expectations from the needs of nanotechnol. and nanomanufacturing Accurate, high-precision, traceable measurements of size, length and other physicochemical properties at the nanoscale Reference materials and methods Critical for nanometrology Also standard methods, protocols, strategies all through the analytical chain are needed AUS NMI 3 slides ToxicToxic potentialpotential ofof nanomaterialsnanomaterials Enhanced reactivity compared to bulk Reactivity may give adverse biological effects Small enough to be mobile in air, water and organisms Some have been shown to penetrate biological barriers Nanomaterials comparable in size to many protein structures in cells Peristent nature MeasurementMeasurement needsneeds inin riskrisk assessmentassessment ofof engineeredengineered nanoparticlesnanoparticles Environmental and human health risk assessment consists of Hazard assessment (how t oxic) and Exposure assessment (how high concentration of X) Both requires analysis and physicochemical characterization Nanometrology needs in environmental risk assessment At a recent horizon scanning workshop with ~60 international experts, metrology development was put at highest importance and where current knowledge were lacking, thus one of the most urgent priorities (Alvarez et al. Research Priorities to Advance Eco-Responsible Nanotechnology. ACS Nano, Vol 3, p 1616-1619 (2009) Agglomeration State Concentration Shape Surface Speciation Size Surface Charge + + + + + Surface Size Functionality Distribution Porosity / Structure / Hassellöv and Surface Area Composition Crystallinity Kaegi, 2009 Similar chemistry (all ZnO) – potentially different behavior (benefits & risks) PhysicochemicalPhysicochemical CharacterizationCharacterization Essential to link hazard to physical structure or chemical composition or surface chemistry Structure-Activity-Relationships! There are currently a number of standardization organizations and initiatives try to agree on descriptors/properties OECD working party on nanomaterials ISO TC 229 - Nanotechnologies Informal: www.characterizationmatters.org Characterization is not only static Diffusion Collisions Attachement Detachement Dissolution Sedimentation Agglomeration ””DDeetteerrmmiinnee RRaatteess ooff CChhaannggee” ” BatteryBattery ofof availableavailable methodsmethods inin thethe analyticalanalytical toolbox,toolbox, e.g:e.g: Size TEM, SEM, AFM, SLS, DLS, FFF, NTA, SEC, LasDiff,... Shape For further reading: Microscopy or DLS-SLS Hassellöv, M., Readman, J., Ranville, J. and Tiede, K. Agglomeration Nanoparticle analysis and characterization methodology in environmental risk assessment of engineered Same as size nanoparticles. Ecotoxicology 2008. Vol. 17, p. 344–361 Composition Bulk: ICPMS, spectroscopy, MS Tiede, K., Boxall, A., Lewis, J., David, H., Tear, S. and Single particle comp: EM-EDX, EM-EELS Hassellöv M. Detection and characterization of engineered nanoparticles in food and the environment – a Particle concentration review. Food Additives and Contaminants 2008, Vol. 25, Mass conc: e.g. FFF-spectroscopy p. 1-27. Number conc: Microscopy, NTA, LIBD Crystal structure Hassellöv M. and Kaegi, R. Analysis and Characterization Bulk: XRD of Manufactured Nanoparticles in Aquatic Environments. Single particle: TEM-SAED In: Nanoscience and Nanotechnology: Environmental and human health implications. (Eds. Lead J.R. and Smith E.) Surface area Wiley 2009, p. 211-266 Powders: Nitrogen adsorption with BET sorption isotherm calculation Surface charge/potential Surface charge: Potentiometric titrations Zeta-potential: Elektrokinetic measurements Surface redox state XPS Surface functionalization SPR But...forBut...for complexcomplex environmentalenvironmental oror biologicalbiological samples...samples... Free nanoparticles, aggregates, mixed agglomerates of engineered NP with background nanomaterials (e.g. proteins or humic substances), dissolved ions of the same element, biological cells... Broad size distributions Heterogeneity in several physicochemical properties Such samples has very different requirements on sample preparation and analysis methods than typical nanomaterial analysis. Method Size (nm) PSD Shape A Agglomeration Concentr. Surface Structure / Single Dynamics Level of C 1 10 100 1000 capability capability state range Chemistry / Crystallinity part./ capability perturbation B capability Charge / Area population + − + AFM ppb ppm + sp medium + + SSA BET powder pp high Centrifugation det. dep. pp low Dialysis det. dep. pp low DLS ppm pp minimum Electrophor. ppm + + + pp minimum + + EELS/EDX ppm in sp sp high ESEM − ppb ppm sp medium Filtration det dep pp low-medium Flow FFF UV: ppm, pp low Sed FFF ICPMS: ppb HDC det. dep. pp low − ICP-MS ppt ppb pp N/A LIBD ppt sp minimum NTA ppb-ppm sp minimum SEC det dep pp medium SEM ppb − ppm sp high SLS ppm pp minimum SAED sp high Spectrometry ppb − ppm pp minimum TEM ppb − ppm (HR) sp high Turbidimetry ppb − ppm pp minimum Ultrafiltration det. dep. pp medium XPS powder pp From Hassellöv and Kaegi, 2009 XRD powder pp high Electron microscopy detection modes Electron beam (parallell in Characteristic TEM, focussed in S-TEM and X-rays Back scattered SEM electrons Secondary electrons TEM interaction volume SEM interaction volume Elastically scattered Inelastically electrons scattered electrons Electron energy loss Transmitted beam spectroscopy ESEMESEM –– BackscatteredBackscattered electronelectron detectiondetection BSE detection: high contrast for high atomic numbers Selectivity for heavy metal NPs Example: Characterization of earthworm toxicity test 10 nm Ag NP Yields aggregates in 50 - 4000 nm size range ESEM -BSE ESEM -SE NP Emissions (Samsung silver washing machine) Scanning TEM-High Angle Annular Dark Field: high contrast for heavy elements NanoparticleNanoparticle trackingtracking analysisanalysis NanoparticleNanoparticle trackingtracking analysisanalysis NanoparticleNanoparticle TrackingTracking AnalysisAnalysis Advantages Miminum perturbing Sensitive Not as biased by scattering intensity of larger particles as DLS Limitations Not fully validated Sizes below ~20-40nm (depending on mtrl) is invisible Results are biased by subjective choice of optimum conditions Conc. responses to some extent material-dependant FieldField --FlowFlow FractionationFractionation (FFF)(FFF) Field Flow To Detector PS 0.05 33nm PS 82nm 0.04 Diffusion Diffusion Separates according to hydrodynamic diameter 0.03 (diffusion) PS 0.02 196nm Size range ~1nm - 800 nm Detector response Suitable for fractionations of complex samples 0.01 Limitations mainly in compatiblity of sample, 0.00 membrane & eluent 0 10 20 30 40 Retention time (min) CouplingCoupling ofof FFFFFF toto differentdifferent
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