Nanotechnologies - Guidance on detection and identification of nano-objects in complex matrices

This document sets requirements for sampling and treatment of the complex matrices in order to obtain a liquid dispersion with sufficiently high concentration of the nano-objects of interest.
This document provides guidelines for detection and identification of specific nano-objects in complex matrices, such as liquid environmental compartments, waste water and consumer products (e.g. food, cosmetics). This document requires for the identification a priori knowledge of the nature of the nano-objects like their chemical composition. The selected detection and identification methods are based on a combination of size classification and chemical composition analysis. Identification can also be supported, e.g. by additional morphology characterization. Currently only Field Flow Fractionation, Electron Microscopy and single particle Inductively Coupled Plasma – Mass Spectrometry fulfil this combination condition.

Nanotechnologien - Leitfaden für die Detektion und Identifizierung von Nanoobjekten in komplexen Matrizen

In diesem Dokument werden Anforderungen an Probenahme und Behandlung der komplexen Matrizen festgelegt, damit eine flüssige Dispersion mit ausreichend hoher Konzentration der zu untersuchenden Nanoobjekte erhalten wird.
Dieses Dokument stellt einen Leitfaden für die Detektion und Identifizierung von spezifischen Nanoobjekten in komplexen Matrizen, wie z. B. flüssige Umweltmedien, Abwasser und Konsumgüter (z. B. Lebensmittel, Kosmetik) zur Verfügung. Dieses Dokument erfordert für die Identifizierung a priori-Wissen über die Art der Nanoobjekte, wie z. B. ihre chemische Zusammensetzung. Die gewählten Detektions  und Identifizierungs¬verfahren basieren auf einer Kombination aus Größenklassifikation und Analyse der chemischen Zusammensetzung. Die Identifizierung kann z. B. auch durch zusätzliche morphologische Charakterisierung unterstützt werden. Derzeit erfüllen nur Feld Fluss Fraktionierung, Elektronenmikroskopie und Einzelpartikel Massenspektrometrie mit induktiv gekoppeltem Plasma diese Kombinationsbedingung.

Nanotechnologies - Document d’orientation pour la détection et l’identification des nano-objets dans les matrices complexes

Le présent document spécifie les exigences relatives à l’échantillonnage et au traitement des matrices complexes afin d’obtenir une dispersion liquide ayant une concentration suffisamment élevée de nano objets présentant un intérêt.
Le présent document fournit des lignes directrices pour la détection et l’identification de nano-objets spécifiques dans les matrices complexes, telles que les compartiments environnementaux liquides, les eaux usées et les biens de consommation (aliments et cosmétiques, par exemple). Pour l’identification, le présent document nécessite de connaître au préalable la nature des nano-objets, telle que leur composition chimique. Les méthodes de détection et d’identification choisies sont fondées sur une combinaison de classification de taille et d’analyse de composition chimique. La caractérisation de la morphologie peut, par exemple, également venir à l’appui de l’identification. À l’heure actuelle, seules les techniques de fractionnement d’écoulement de champ (FFF), de microscopie électronique (ME) et de spectroscopie de masse à plasma à couplage inductif à particule unique (spICP-MS) remplissent cette condition de combinaison.

Nanotehnologija - Navodilo za odkrivanje in identifikacijo nanopredmetov v kompleksnih matrikah

Ta dokument določa zahteve za vzorčenje in obdelavo kompleksnih matrik za pridobivanje tekoče disperzije z dovolj visoko koncentracijo nanopredmetov, ki nas zanimajo.
Ta dokument vsebuje smernice za odkrivanje in identifikacijo določenih nanopredmetov v kompleksnih matricah, kot so vsebniki s tekočinami, odpadna voda in potrošniški izdelki (npr. hrana, kozmetika). Ta dokument zahteva identifikacijo vnaprejšnjega poznavanja narave nanopredmetov, kot je njihova kemična sestava. Izbrane metode odkrivanja in identifikacije temeljijo na kombinaciji klasifikacije velikosti in analize kemijske sestave. Identifikacijo lahko podpiramo na primer tudi z dodatno morfološko karakterizacijo. Trenutno izpolnjujejo ta pogoj kombinacije samo frakcioniranje v tokovnem polju, elektronska mikroskopija in masna spektrometrija z induktivno sklopljeno plazmo.

General Information

Status
Published
Publication Date
18-Dec-2018
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
08-Sep-2022

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Technical specification
TS CEN/TS 17273:2019
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SLOVENSKI STANDARD
01-marec-2019
Nanotehnologija - Navodilo za odkrivanje in identifikacijo nanopredmetov v
kompleksnih matrikah
Nanotechnologies - Guidance on detection and identification of nano-objects in complex
matrices
Nanotechnologien - Leitfaden für die Detektion und Identifizierung von Nanoobjekten in
komplexen Matrizen
Nanotechnologies - Guide pour la détection et l'identification des nano-objets dans des
matrices complexes
Ta slovenski standard je istoveten z: CEN/TS 17273:2018
ICS:
07.120 Nanotehnologije Nanotechnologies
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TS 17273
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
December 2018
TECHNISCHE SPEZIFIKATION
ICS 07.120
English Version
Nanotechnologies - Guidance on detection and
identification of nano-objects in complex matrices
Nanotechnologies - Document d'orientation pour la Nanotechnologien - Leitfaden für die Detektion und
détection et l'identification des nano-objets dans les Identifizierung von Nanoobjekten in komplexen
matrices complexes Matrizen
This Technical Specification (CEN/TS) was approved by CEN on 28 September 2018 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17273:2018 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 8
4 Symbols and abbreviations . 9
5 Possible tasks and measuring techniques . 11
5.1 Examples for detection and identification tasks in complex matrices . 11
5.2 Overview of measurement techniques . 11
6 Guidance on sample preparation, particle detection and identification of nano-
objects in complex matrices. 12
6.1 Approach for “Detection and Identification of a relevant population of nano-objects
based on a priori knowledge” (guidance chart) . 12
6.2 Information about the targeted nano-objects . 15
6.3 Information about the sample matrix . 16
6.4 Sample Preparation Process Quality assessment . 16
6.4.1 Suspension, dispersion with recovery evaluation and property assessment . 16
6.4.2 Initial size distribution measurement and mass concentration measurement of all
isolated nano-objects . 16
6.5 Measurement of the targeted nano-objects and evaluation . 18
7 Selected measuring techniques for the detection and identification of nano-
objects . 18
7.1 Field-Flow-Fractionation (FFF) technique. 18
7.1.1 General. 18
7.1.2 Fractionation principle and theory — Fractionation principle . 19
7.1.3 Detection principle . 20
7.1.4 Performance . 21
7.1.5 Sample preparation . 22
7.1.6 Analysis report and interpretation of results . 23
7.2 Electron Microscopy (EM) technique . 23
7.2.1 General. 23
7.2.2 Measuring principle of Electron Microscopy . 24
7.2.3 Performance of Electron Microscopy . 25
7.2.4 Specimen preparation for Electron Microscopy . 26
7.2.5 Interpretation of Electron Microscopy results . 27
7.3 Single particle Inductively Coupled Plasma Mass Spetrometry (spICP-MS) . 28
7.3.1 Measuring principle . 28
7.3.2 Performance . 28
7.3.3 Sample preparation . 30
7.3.4 Interpretation of results . 30
8 List of reporting requirements on sample preparation, detection and identification
of nano-objects in complex matrixes . 32
8.1 General reporting . 32
8.2 Sample preparation reporting, explained in Clause 6 . 32
8.3 Measurement reporting, explained in Clause 7 . 33
Annex A (informative) Indicative ranges of size and concentration of selected measuring
techniques . 34
Annex B (normative) Theory of F4 separations, precautions when separating broad particle
size distributions and sample preparation . 36
B.1 Theory of F4 separations . 36
B.2 F4 calibration using F4 theory or external references . 37
B.3 Approaches to prepare complex samples for FFF. 39
Annex C (informative) Example: Analysis of the release of particles from the coating of
silver-coloured pearls by a combination of descriptive TEM analysis, electron
diffraction, analytical TEM and quantitative TEM . 41
C.1 Approach and methodology . 41
C.2 Results . 42
Annex D (informative) Example: Single particle ICP-MS for sizing and quantitative
determination of nano-silver in chicken meat. 45
D.1 Introduction . 45
D.2 Method Description . 45
D.2.1 Materials and Methods . 45
D.2.2 Sample Preparation . 45
D.2.3 Instrumental Analysis . 45
D.2.4 Data Processing . 46
D.3 Results and Discussion . 46
D.3.1 Sample enzymatic digestion: soft conditions to preserve particle characteristics . 46
D.3.2 Study Design and Results of Validation . 47
D.3.3 Repeatability, reproducibility, and trueness . 47
D.3.4 Linearity and LOD/LOQ, Robustness, specificity/selectivity . 48
Annex E (informative) Overview of alternative detection methods. 50
E.1 General . 50
E.2 Particle Tracking Analysis (PTA) . 51
E.3 Tracer methods by using stable isotopic labelled nano-objects . 52
E.4 HyperSpectral Imaging System (HSIS) by scattering in a dark-field background . 53
E.5 Size evaluation by UV-vis spectroscopy . 53
E.6 Sizing nano-objects in liquids using differential mobility analysing system (DMAS) 53
E.7 Laser-Induced Breakdown Detection (LIBD) . 54
E.8 Hydrodynamic chromatography ICP-MS (HDC-ICP-MS) and size exclusion ICP-MS
(SEC-ICP-MS) . 55
Bibliography . 56

European foreword
This document (CEN/TS 17273:2018) has been prepared by Technical Committee CEN/TC 352
“Nanotechnologies”, the secretariat of which is held by AFNOR.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Introduction
Nanotechnology is a rapidly developing field of science and technology that focuses on processes and
materials at the nanoscale size (particle dimensions that are approximately 1 nm to 100 nm). It is a highly
multidisciplinary field with a wide range of materials and applic
...

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