1、Nanotechnologies Guidance on measurands for characterising nano-objects and materials that contain them PD CEN/TS 17010:2016 BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06National foreword This Published Document is the UK implementation of CEN/TS 17010:2016. The
2、UK participation in its preparation was entrusted to Technical Committee NTI/1, Nanotechnologies. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are resp
3、onsible for its correct application. The British Standards Institution 2017. Published by BSI Standards Limited 2017 ISBN 978 0 580 94088 0 ICS 07.120 Compliance with a British Standard cannot confer immunity from legal obligations. Amendments/corrigenda issued since publication Date Text affected P
4、UBLISHED DOCUMENT PD CEN/TS 17010:2016 This published Document was published under the authority of the Standards Policy and Strategy Committee on 31 January 2016. TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 17010 December 2016 ICS 07.120 English Version Nanotechno
5、logies - Guidance on measurands for characterising nano-objects and materials that contain them Nanotechnologies - Guide sur les mesurandes pour la caractrisation de nano-objects et des matriaux les contenant Nanotechnologien - Leitfaden ber Messgren zur Charakterisierung von Nanoobjekten und von We
6、rkstoffen, die welche enthalten This Technical Specification (CEN/TS) was approved by CEN on 12 October 2016 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, particul
7、arly 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
8、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
9、 Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE
10、NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 17010:2016 E PD CEN/TS 17010:2016CEN/TS 17010:2016 (E) 2 Content
11、s Page European foreword . 7 Introduction 8 1 Scope 9 2 Normative references 9 3 Terms and definitions . 9 3.1 General core terms 10 3.2 Measurand terms . 10 4 Symbols and abbreviations 15 5 Approaches to identify measurands to characterize nano-objects and their agglomerates and aggregates, and mat
12、erials containing nano-objects . 17 5.1 Method . 17 5.2 Types of measurands 17 5.3 State of nano-objects . 18 Table 1 Different states of Nano-objects 18 6 Measurands related to size and shape measurement of nano-objects and their agglomerates and aggregates 18 6.1 Introduction . 18 6.2 Measurands r
13、elated to size and shape measurement . 19 6.3 Measurands related to size and shape measurement in aerosols 19 6.3.1 Overview . 19 Table 2 Measurands related to the size and shape measurement in aerosols . 20 6.3.2 General relevant standard 21 6.3.3 Electrical low-pressure impaction (ELPI) . 21 6.3.4
14、 Cascade impactors . 22 6.3.5 Differential mobility analysing system (DMAS) 22 6.3.6 Relevant standards 22 6.3.7 Optical Particulate Counters (OPC) . 23 6.3.8 Relevant standards 23 6.3.9 Aerodynamic Particle Sizing (APS) 23 6.3.10 Transmission electron microscopy (TEM) combined with TEM grid sampler
15、s 23 6.3.11 Relevant standards 24 6.3.12 Scanning electron microscopy (SEM) 24 6.3.13 Relevant standards 24 6.4 Measurands related to size and shape measurement in powders . 25 6.4.1 Overview . 25 Table 3 Measurands related to the size and shape measurement in powders . 25 6.4.2 Relevant standards 2
16、6 6.4.3 Scanning electron microscopy (SEM) 26 6.4.4 Relevant standards 26 6.4.5 Gas adsorption, the BET method 26 6.4.6 Relevant standards 26 6.4.7 Laser diffraction (LD) . 26 6.4.8 Relevant standards 27 6.4.9 X-ray diffraction (XRD) 27 PD CEN/TS 17010:2016CEN/TS 17010:2016 (E) 3 6.4.10 Relevant sta
17、ndards 27 6.4.11 Raman spectroscopy 27 6.5 Measurands related to size and shape measurements of nano-objects in liquid dispersions. 27 6.5.1 Overview 27 Table 4 Measurands related to the size and shape measurement in liquids . 28 6.5.2 Centrifugal liquid sedimentation (CLS) 29 6.5.3 Relevant standar
18、ds 29 6.5.4 Dynamic light scattering (DLS) 30 6.5.5 Relevant standards 30 6.5.6 Laser diffraction (LD) 30 6.5.7 Relevant standards 30 6.5.8 Small angle X-ray scattering (SAXS) . 30 6.5.9 Relevant standards 31 6.5.10 Particle tracking analysis (PTA) 31 6.5.11 Relevant standards 31 6.5.12 Electron mic
19、roscopy 31 6.6 Measurands related to size and shape measurement on surfaces (microscopy techniques). 31 6.6.1 Overview 31 Table 5 Measurands related to the size and shape measurement on surfaces . 32 6.6.2 Scanning electron microscopy (SEM) 32 6.6.3 Atomic force microscopy (AFM) 32 6.6.4 Relevant st
20、andards 33 7 Measurands related to chemical analysis of nano-objects and their agglomerates and aggregates 33 7.1 Introduction 33 7.2 Measurands related to surface chemical analysis of nano-objects and their agglomerates and aggregates . 34 7.2.1 Measurands . 34 Table 6 Measurands related to the sur
21、face chemical analysis of nano-objects and their agglomerates and aggregates . 34 7.2.2 Auger electron spectroscopy (AES) 35 7.2.3 Relevant standards 35 7.2.4 Electron energy loss spectroscopy (EELS) . 36 7.2.5 Relevant standards 36 7.2.6 Secondary ion mass spectroscopy (SIMS) 36 7.2.7 Relevant stan
22、dards 36 7.2.8 X-ray fluorescence spectroscopy (XRF) 36 7.2.9 Relevant standards 37 7.2.10 X-ray diffraction (XRD) . 37 7.2.11 Relevant standards 37 7.2.12 X-ray photoelectron spectroscopy (XPS) . 38 7.2.13 Relevant standards 38 7.2.14 Energy dispersive X-ray spectroscopy (EDS or EDX) . 38 7.3 Measu
23、rands related to the chemical analysis of nano-objects as bulk samples 39 7.3.1 Measurands . 39 Table 7 Measurands related to the chemical analysis of nano-objects and their agglomerates and aggregates . 39 7.3.2 Differential scanning calorimetry (DSC) 41 7.3.3 Relevant standards 41 PD CEN/TS 17010:
24、2016CEN/TS 17010:2016 (E) 4 7.3.4 Fourier transform infrared spectroscopy (FTIR) . 41 7.3.5 Relevant standards 42 7.3.6 Thermal analysis with evolved gas analyser (EGA) plus FTIR or QMS . 42 7.3.7 Relevant standards 42 7.3.8 Ultravioletvisible spectroscopy (UV-Vis) 42 7.3.9 Relevant standards 43 7.3
25、.10 Raman spectroscopy . 43 7.3.11 Inductively coupled plasma (ICP) techniques . 43 7.3.12 Contact Angle . 43 8 Measurands related to mass and density 43 8.1 Introduction . 43 8.2 Aerosols . 44 8.2.1 Measurands 44 Table 8 Measurands associated with mass and density measurement of nano-objects in an
26、aerosol 44 8.2.2 Relevant standards 44 8.2.3 Aerosol particle mass analyser (APM) . 44 8.2.4 Time of flight mass spectrometry 44 8.3 Powders . 45 8.3.1 Measurands 45 Table 9 Measurands associated with mass and density measurement of nano-objects in powder form 45 8.3.2 Pycnometry 45 8.3.3 Relevant s
27、tandards 45 8.4 Liquid dispersions . 45 8.4.1 Measurands 45 Table 10 Measurands related to mass and density for nano-objects in liquid dispersions. 46 8.4.2 Relevant standards 46 8.4.3 Centrifugal liquid sedimentation (Isopycnic method) . 46 8.4.4 Static light scattering (SLS) . 47 8.4.5 Resonant ma
28、ss measurement (RMM) . 47 9 Measurands related to charge - Liquid dispersions 47 9.1 Measurands 47 Table 11 Measurands related to charge . 47 9.2 Relevant standards 48 9.3 Electrophoretic light scattering 48 9.4 Electroaccoustic phenomena measurements 48 10 Measurands related to crystallinity 48 10.
29、1 Measurands 48 Table 12 Measurands related to crystallinity . 49 10.2 Small-angle/wide-angle X-ray scattering (SAXS/WAXS) . 50 10.3 X-ray diffraction (XRD) 50 10.4 Scanning/ electron microscopy (SEM) . 50 10.5 High-resolution transmission electron microscopy (HRTEM) 51 10.6 Electron diffraction . 5
30、1 10.7 Neutron diffraction 51 10.8 Electron backscatter diffraction (EBSD) 51 10.9 Reflection high-energy electron diffraction (RHEED) and low-energy electron diffraction (LEED). 51 10.10 Differential scanning calorimetry (DSC) . 52 PD CEN/TS 17010:2016CEN/TS 17010:2016 (E) 5 10.11 Nuclear magnetic
31、resonance (NMR) crystallography 52 10.12 Raman crystallography . 52 10.13 Relevant standards 52 11 Optical properties measurands . 52 11.1 Introduction 52 11.2 Measurands . 52 Table 13 Measurands for optical properties . 53 11.3 Spectroscopy techniques 53 11.4 Relevant standards 54 12 Electrical and
32、 electronic measurands . 54 12.1 Measurands . 54 Table 14 Measurands related to electrical and electronic measurements. 55 12.2 Techniques 56 12.2.1 2 or 4 point conductance measurements . 56 12.2.2 Angle-resolved ultraviolet photoemission spectroscopy (ARPES) . 56 12.2.3 Scanning tunnelling microsc
33、opy (STM) 56 12.2.4 Conductive atomic force microscopy . 56 12.2.5 Piezoforce microscopy (PFM) . 56 13 Magnetic measurands . 57 13.1 Introduction 57 13.2 Measurands . 57 Table 15 Measurands related to magnetic properties of solid nano-composite materials . 57 13.3 Techniques 58 13.3.1 Superconductin
34、g quantum interference device (SQUID) . 58 13.3.2 Vibrating sample magnetometer (VSM) . 59 13.3.3 Mssbauer spectroscopy 59 13.3.4 Electron paramagnetic resonance (EPR) spectroscopy 59 13.3.5 Magneto-optical Kerr-effect (MOKE) . 59 13.3.6 Magnetic force microscopy (MFM) . 59 13.3.7 Scanning Hall effe
35、ct microscopy 59 13.3.8 Spin-polarized scanning tunnelling microscopy (SP-STM) . 60 13.3.9 Relevant standards 60 14 Thermal measurands 60 14.1 Measurands . 60 Table 16 Measurands related to thermal properties . 61 14.2 Techniques 61 14.2.1 Measurement of specific heat capacity . 61 14.2.2 Scanning t
36、hermal microscopy (SThM) 61 15 Other performance related measurands 62 15.1 Introduction 62 15.2 Powders - Dustiness . 62 Table 17 Measurands related to Dustiness 62 15.3 Liquid dispersions 63 15.3.1 Introduction 63 Table 18 Measurands related to properties of suspension of nano-objects in liquids 6
37、3 15.3.2 Viscosity . 63 15.3.3 Dispersibility 65 15.3.4 Relevant standards 65 PD CEN/TS 17010:2016CEN/TS 17010:2016 (E) 6 15.3.5 Solubility and rate of dissolution . 65 15.3.6 Relevant standards 66 15.4 Mechanical properties 66 15.4.1 Introduction . 66 Table 19 Measurands related to mechanical prope
38、rties of solid nano-composite materials . 67 15.4.2 Measurement of elastic constants by static methods 68 15.4.3 Relevant standards 68 15.4.4 Measurement of elastic constants by dynamic methods . 68 15.4.5 Relevant standards 68 15.4.6 Measurement of elastic and plastic properties by instrumented ind
39、entation methods 68 15.4.7 Relevant standards 69 15.4.8 Measurement of surface properties and wear 69 15.4.9 Relevant standards 69 Bibliography . 70 PD CEN/TS 17010:2016CEN/TS 17010:2016 (E) 7 European foreword This document (CEN/TS 17010:2016) has been prepared by Technical Committee CEN/TC 352 “Na
40、notechnologies”, 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 m
41、andate given to CEN by the European Commission and the European Free Trade Association. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
42、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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kin
43、gdom. PD CEN/TS 17010:2016CEN/TS 17010:2016 (E) 8 Introduction The term “nano-object” applies to materials having one, two or three external dimensions in the nanoscale (therefore in the range of approximately 1 to 100 nanometres). Specific properties of nano-objects are usually exhibited in this si
44、ze range, even if they do not disappear abruptly beyond these limits. Nano-objects, either natural or manufactured, can then be found in the form of nanoplates (one dimension in the nanoscale), nanofibres (two dimensions, or the diameter, in the nanoscale), and nanoparticles (three dimensions in the
45、 nanoscale). Nano-objects exhibit higher specific surface areas than larger objects. They are particularly prone to aggregation and agglomeration phenomena due to attractive interactions during their life cycle. There is increasing use of nano-objects in research and development, industry and commer
46、cial applications. Characterization of nano-objects, and their agglomerates and aggregates (sometimes referred to as NOAA) plays an essential role in basic and applied research, through process and product quality control and commercialization to health and environmental protection. Characterization
47、 of nano-objects is key to determine their properties, performance and life-time. The methods available for characterization of larger scale materials are often difficult to apply to nano-objects, sometimes due to restrictions of the test systems (e.g. low sensitivity, inadequate resolution of equip
48、ment). This has resulted in new techniques and adapting old methods. One definition of “measurand” used in many ISO standards is the “quantity intended to be measured”. In nanotechnologies measurement and characterization this “intended quantity” could be size, shape, chemical composition, surface c
49、harge, etc. However, in reality, an instrument does not always directly measure this fundamental characteristic but measures something else, which is ultimately related to the intended quantity. This Technical Specification (TS) describes and defines the measurands, both the overarching intended measurands and those actually measured by the instruments, in order to elucidate which measurements can be compared with each other and under which conditions and assumptions. The Technical Specification is split into ten main clauses covering:
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