NanoDefine Guidance for the implementation of the definitionImplementation: objectives Pooling...

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



Main criteria continued



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


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



Nano / non-nano ?

Plausibility check?

Material properties

Require-ments

Purpose

Methods characteri-

sation

Existing data

Nano Non-Nano

Nano / non-nano ?

Plausibility check?



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


• 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)


Tier 1: (validated) rapid screening methods

Tier 2: (validated) in depth confirmatory methods


Nano / non-nano ?

Plausibility check?

Material properties

Require-ments

Purpose

Methods characteri-

sation

Existing data

Nano Non-Nano

Nano / non-nano ?

Plausibility check?



Methods Evaluation


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



Nano / non-nano ?

Plausibility check?

Material properties

Require-ments

Purpose

Methods characteri-

sation

Existing data

Nano Non-Nano

Nano / non-nano ?

Plausibility check?



E-tool (software) • User-friendly • Semi-automated • Open for amendments

Methods Manual • Practical, coherent

guidance • Print and online

NanoDefine Products

NanoDefine Products


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



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



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



• 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

NanoDefine Guidance for the implementation of the definitionImplementation: objectives Pooling...

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