nanodefine guidance for the implementation of the definitionimplementation: objectives pooling...
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NanoDefine Guidance for the implementation of the definition
Hubert Rauscher European Commission Joint Research Centre
Institute for Health and Consumer Protection
Nanobiosciences
• The NanoDefine Methods Manual
• The “NanoDefiner” eTool
• Recommendations on the revision of the definition
NanoDefine: Implementation , Brussels 17 June 2015
Implementation: objectives
Pooling project results together to:
Design a decision making framework to select the most cost-efficient
methodology for a given task, nanomaterial and matrix
Prepare a hands-on manual on the recommended use of methods
specified by purpose and quality requirements, including performance
characteristics
Establish the NanoDefiner e-tool for method selection, data evaluation
and size-related classification of particulate materials according to the
definition
Make recommendations on a revision of the definition based on
analytical possibilities
Assess the performance of the NanoDefine e-tool and manual through real
world scenarios of chemical, pigment, cosmetics and food/feed industry
(case studies)
NanoDefine: Implementation, Brussels 17 June 2015
Sample preparation options
Nano / non-nano ?
Plausibility check?
Material properties
Require-ments
Purpose
Methods characteri-
sation
Existing data
Nano Non-Nano
Nano / non-nano ?
Plausibility check?
Tier 1: Screening method options
Tier 2: Confirmatory method options, if required
Entry pathways (input)
• Material classification • Purpose Requirements • Available methods - characteristics • Existing data
Sample preparation - SOPs
E-tool (software) • User-friendly • Semi-automated • Open for amendments
Methods Manual • Practical, coherent
guidance • Print and online
NanoDefine Products
Tiered approach
• Tier 1: "screening methods" • Tier 2: "confirmatory methods"
Including
• Performance criteria • Method evaluation against - uniform criteria • Method development (selected techniques)
Decision-support flow system
NanoDefine: Implementation, Brussels 17 June 2015 NanoDefine: Implementation, Brussels 17 June 2015
Main criteria
Material classification system
• Depending on the type, the
material is classified according to
several parameters
• Will link to recommendations for
• Sample preparation
• Measurement methods
NanoDefine: Implementation, Brussels 17 June 2015
Material classification system
Main criteria continued
NanoDefine: Implementation, Brussels 17 June 2015
Material classification system
Example: Multiwall carbon nanotubes
Chemical composition
Inorganic materials
Carbon-based
Organic, particulate
Organic, non- particulate
Biological
Composite
Core/shell
Multiple coatings
A mix of two or more different materials Other/ Unknown
Form and Shape
Nanoscaled dimensions
1
2
3
Mixture of different nanoscaled materials
Shape
Sphere
Equiaxial
Elongated
Flat
Other/ Unknown
Mixture of different shaped particles
Presence of different types of particles
Unknown
Non-nano-component
Important presence of susnanomaterials
Important presence of subnanomaterials
Mo
no
-co
nst
itu
ent
sub
stan
ce
Mo
no
-co
nst
itu
ent
sub
stan
ce
Trade Form and Dispersibility
Trade Form
Powder
Suspension
Aerosol
Dispersibility
Dispersible in aqueous media
Dispersible in material-specific media and
protocols DMF
Can be aerosolized
Stability of particles during testing
E-beam Stable
Vacuum stability Stable
Release of ions/atoms/molecules
No
Heating After 750°C in air
Cooling stable
Specific properties
Electrically conductive Semi conductive
Magnetic properties No
Size-dependent absorption of photons /
fluorescence Raman for diameter
Functionalised No
Special characteristics of particles surface
Hydrphobic
Start
Start
NanoDefine: Implementation, Brussels 17 June 2015
Purpose
Legal
Dossier filling/ registration
REACH
Material type
Trade Form
Chemical Identification
Size distribution
Concentration
Surface area
Shape/ morphology
Cosmetic Legislation
French registration
Danish Registration
Belgian Registration
enforcement
Food Labelling
Cosmetic Labelling
Biocide Other R & D/
Quality
• Quantitative decision criteria are developed in the project
• Regulators' criteria used if available
• Required data quality
• Cost
• Example: REACH
Purpose Requirements
NanoDefine: Implementation, Brussels 17 June 2015
Sample preparation options
Nano / non-nano ?
Plausibility check?
Material properties
Require-ments
Purpose
Methods characteri-
sation
Existing data
Nano Non-Nano
Nano / non-nano ?
Plausibility check?
Tier 1: Screening method options
Tier 2: Confirmatory method options, if required
Sample preparation - SOPs
Tiered approach
• Tier 1: "screening methods" • Tier 2: "confirmatory methods"
Including
• Performance criteria • Method evaluation against - uniform criteria • Method development (selected techniques)
Decision-support flow scheme
NanoDefine: Implementation, Brussels 17 June 2015 NanoDefine: Implementation, Brussels 17 June 2015
• Substance-related criteria (applicability to different substance groups)
• Method-related criteria
• All characterisation methods are evaluated against uniform criteria
Methods Performance Criteria and Evaluation
Criteria Criteria - detail
Caracter
ization
(yes/no)
Notes
Working range
Size range > 1 nm
Lower range varies in
dependence on
instrument type,
sample type and
preparation
Concentration range “mono
layer”
EM measures
accurately only “dry”
particles deposited on
a substrate. Droplet
of 0.1-1 µL at 0.1%-
vol. conc. typically
sufficient.
Minimum needed
sample 0.1 µL
Minimum 500 NPs for
a monodisperse/
monomodal sample
(Motzkus et al., 2013)
Limits of
detection/quantification
1 nm to
10 nm
Depending on
instrument, sample
type and preparation,
etc.
… …
Criteria Criteria - detail
Caracter
ization
(yes/no)
Substance
Nature
Inorganic yes
Carbon based Yes
Organic, particulate Yes
Organic, non-particulate Yes
Composite Yes
Other yes
Shape of
nanoparticles
Sphere or assimilated yes
Equiaxial Yes
Tubes, fibres, rods Yes
Flakes and discs No
Other Yes
Thermal
degradation
sensitivity
Above 0° No
Sensitivity above 37°C Yes
Sensitivity above 50°C Yes
…
Sample
dispersity and
modality
Monodisperse sample Yes
Polydisperse sample Yes
… …
Example: electron microscopy – selected fields (SEM, TEM and STEM)
NanoDefine: Implementation, Brussels 17 June 2015
Tier 1: (validated) rapid screening methods
Tier 2: (validated) in depth confirmatory methods
Sample preparation options
Nano / non-nano ?
Plausibility check?
Material properties
Require-ments
Purpose
Methods characteri-
sation
Existing data
Nano Non-Nano
Nano / non-nano ?
Plausibility check?
Tier 1: Screening method options
Tier 2: Confirmatory method options, if required
Methods Evaluation
NanoDefine: Implementation, Brussels 17 June 2015
TIER 1
(Screening
methods)
TIER 2
(Confirmatory
methods)
Methods for direct
validation or
standardisation
PTA/DUM
sp ICP-MS
AC
DMAS
DLS
TRPS
SAXS
USSp
EM
FFF
EM
AFM
PTA/DUM
sp ICP-MS
FFF
AC
Tier 1 and tier 2 methods
NanoDefine: Implementation, Brussels 17 June 2015
Sample preparation options
Nano / non-nano ?
Plausibility check?
Material properties
Require-ments
Purpose
Methods characteri-
sation
Existing data
Nano Non-Nano
Nano / non-nano ?
Plausibility check?
Tier 1: Screening method options
Tier 2: Confirmatory method options, if required
E-tool (software) • User-friendly • Semi-automated • Open for amendments
Methods Manual • Practical, coherent
guidance • Print and online
NanoDefine Products
NanoDefine Products
NanoDefine: Implementation, Brussels 17 June 2015
NanoDefine Methods Manual
• First edition (June/July 2015) includes:
• Material classification system
• Methods performance criteria
• Sampling and sample preparation, SOPs
• Technical guidance on use and applicability of methods
• Introduction to techniques
• Recommendations use
(strengths, limitations)
• Updated edition (project end)
• All new developments
NanoDefine: Implementation, Brussels 17 June 2015
NanoDefine: Implementation, Brussels 17 June 2015
work flow
Substance Properties Edit Delete Ag Chemical composition => inorganic
Nanoscale dimensions => 3 Shape => Sphere Presence of different sized particles => unknown Trade form => Powder Dispersibility => Dispersible in aqueous media Expected size range => 10 – 30 nm E-beam sensitivity => Unknown Vacuum stability => Unknown Heating stability => Yes => >150°C Cooling stability => Yes => <-195°C
Project definition Material definition Decision making Import data
NanoDefiner e-Tool
• Guides the user through the decision-
making process
• User-friendly
• Recommendations on measurements
• Reporting with reasoning
NanoDefine: Implementation, Brussels 17 June 2015
NanoDefine: Implementation, Brussels 17 June 2015
Recommendations
• External dimensions of individual particles
• Particle size distribution, number median size
• Data conversion
• Polydispersity, irregular/non-spherical shape
• Aggregates, agglomerates
• Role of VSSA
• Specific challenges for colloids, multi-constituent
substances, mixtures, NM in products
Recommendations on a revision of the definition based on analytical possibilities
NanoDefine: Implementation, Brussels 17 June 2015
NanoDefine: Implementation, Brussels 17 June 2015 NanoDefine: Implementation, Brussels 17 June 2015
Material classification system
• Starting point: material type
• Monoconstituent substance
• multiconstituent substance,
mixture
• article, consumer product
• Depending on the type, the material is
classified according to several
parameters
• Will link to recommendations for
• Sample preparation
• Measurement methods
Implementation: Outline
Decision support flow scheme
Case studies Performance assessment of NanoDefiner
NanoDefiner: e-tool
e-tool software
NanoDefiner manual
(document)
Material
classification
Purpose
Requirements
Methods
Performance
Characterisation
Existing data