1、BS ISO 19430:2016Particle size analysis - Particle tracking analysis(PTA) methodBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 19430:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 19430:2016. The UK participation i
2、n its preparation was entrusted to TechnicalCommittee LBI/37, Particle characterization including sieving.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are
3、 responsible for its correctapplication. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 85568 9ICS 19.120Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStanda
4、rds Policy and Strategy Committee on 31 December 2016.Amendments/Corrigenda issued since publicationDate Text affectedBS ISO 19430:2016 ISO 2016Particle size analysis Particle tracking analysis (PTA) methodAnalyse granulomtrique Mthode danalyse de suivi de particule (PTA)INTERNATIONAL STANDARDISO194
5、30First edition2016-12-15Reference numberISO 19430:2016(E)BS ISO 19430:2016ISO 19430:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwi
6、se in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh.
7、de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 19430:2016ISO 19430:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols and abbreviated terms . 45 Principles . 45.
8、1 General . 45.2 Key physical parameters. 55.3 Detection limits 55.3.1 Lower size limit . 55.3.2 Upper size limit . 65.3.3 Sample and sampling volume . 65.3.4 Maximum particle number concentration . 65.3.5 Minimum particle number concentration . 75.4 Measurement precision and uncertainties . 75.4.1
9、General 75.4.2 Measurement precision . 75.4.3 Size range . 85.4.4 Counting efficiency 85.4.5 Sizing accuracy 95.4.6 Size resolution 96 Apparatus 107 Procedure117.1 General 117.2 Sample preparation . 127.3 Instrument set-up and initialisation . 127.4 Measurement . 137.4.1 Sample delivery 137.4.2 Samp
10、le illumination .137.4.3 Particle imaging and tracking 147.4.4 Track analysis 147.5 Results evaluation . 147.5.1 General. 147.5.2 Particle size evaluation 147.5.3 Distribution analysis147.5.4 Data analysis and reporting 148 System qualification and quality control .158.1 General 158.2 System install
11、ation requirements 158.3 System maintenance . 158.4 System operation . 158.5 System qualification 169 Data recording .1710 Test report 17Annex A (informative) Theory20Annex B (informative) Apparatus settings and best practice 23Bibliography .25 ISO 2016 All rights reserved iiiContents PageBS ISO 194
12、30:2016ISO 19430:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in
13、a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commissi
14、on (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents shoul
15、d be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for iden
16、tifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the conveni
17、ence of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the
18、 following URL: www.iso.org/iso/foreword.htmlThe committee responsible for this document is Technical Committee ISO/TC 24, Particle characterization including sieving, Subcommittee SC 4, Particle characterization.iv ISO 2016 All rights reservedBS ISO 19430:2016ISO 19430:2016(E)IntroductionRegulatory
19、, scientific and commercial requirements for nanomaterial characterization or characterization of particulate suspensions where particle sizing and counting is required provide a strong case for further development of techniques such as Particle Tracking Analysis (PTA), also known as Nanoparticle Tr
20、acking Analysis (NTA) 14. Due to the fact that the term PTA covers a larger size range and is more generic1), the term PTA is used throughout this document to refer to NTA and PTA. For all aims and purposes, the term PTA also means NTA in this document.PTA is based on measuring the diffusion movemen
21、t of particles in a suspension by means of laser illumination, imaging of scattered light, particle identification and localization, and individual particle tracking2). In this case, suspension is an even dispersion of particles, gas bubbles or other liquid droplets. The hydrodynamic diameter of the
22、 individual particles, droplets or bubbles is related to Brownian motion parameters via the StokesEinstein equation.In recent years the academic community working in fields such as liposomes and other drug delivery vehicles, nanotoxicology, viruses, exosomes, protein aggregation, inkjet inks, pigmen
23、t particles, cosmetics, foodstuffs, fuel additives and fine bubbles began using the PTA technology for characterization. An ASTM standard guide (E283412) 10was developed to give guidance to the measurement of particle size distribution by means of Nanoparticle Tracking Analysis. The present document
24、 aims to broaden the scope of the specification and to introduce system tests for PTA operation.This document outlines the theory and basic principles of the particle tracking analysis method along with its limitations and advantages. It also describes commonly used instrument configurations and mea
25、surement procedures as well as system qualifications and data reporting. One of the key aspects is the meaning of the data and its interpretation. It should be noted that the key measurand obtained from PTA measurement is the number-based particle size distribution where the size is taken to mean th
26、e hydrodynamic diameter (3.11) of the particles in the sample. This size can be different from other sizes obtained with different techniques such as dynamic light scattering 6or electron microscopy 4.1) NTA is the most recognised abbreviation for the technique described in this document. However th
27、e Particle Tracking Analysis (PTA) includes NTA in its size range of measurements.2) For the purpose of this document “tracking” will mean “following in terms of particle x and y position” and the “track” will mean “the path of that particle defined by such x and y coordinates of each step” ISO 2016
28、 All rights reserved vBS ISO 19430:2016BS ISO 19430:2016Particle size analysis Particle tracking analysis (PTA) method1 ScopeThis document describes the evaluation of the numberbased particle size distribution in liquid dispersions (solid, liquid or gaseous particles suspended in liquids) using the
29、particle tracking analysis method for diffusion velocity measurements.2 Normative referencesThere are no normative references in this document.3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in
30、standardization at the following addresses: ISO Online browsing platform: available at http:/www.iso.org/obp IEC Electropedia: available at http:/www.electropedia.org/3.1nanoscalelength range approximately from 1 nm to 100 nmNote 1 to entry: Properties that are not extrapolations from larger sizes a
31、re predominantly exhibited in this length range.SOURCE: ISO/TS 80004-1:2015, 2.13.2nano-objectmaterial with one, two or three external dimensions in the nanoscale (3.1)Note 1 to entry: The second and third external dimensions are orthogonal to the first dimension and to each other.SOURCE: ISO/TS 800
32、04-1:2015, 2.53.3nanoparticlenano-object (3.2) with all three external dimensions in the nanoscale (3.1)Note 1 to entry: If the lengths of the longest to the shortest axes of the nano-object differ significantly (typically by more than three times), the terms nanofibre or nanoplate are intended to b
33、e used instead of the term nanoparticle.SOURCE: ISO/TS 80004-4:2011, 2.43.4particleminute piece of matter with defined physical boundariesNote 1 to entry: A physical boundary can also be described as an interface.INTERNATIONAL STANDARD ISO 19430:2016(E) ISO 2016 All rights reserved 1BS ISO 19430:201
34、6ISO 19430:2016(E)Note 2 to entry: A particle can move as a unit.Note 3 to entry: This general particle definition applies to nano-objects (3.2).SOURCE: ISO/TS 80004-6:2013, 2.93.5agglomeratecollection of weakly bound particles or aggregates or mixtures of the two where the resulting external surfac
35、e area is similar to the sum of the surface areas of the individual componentsNote 1 to entry: The forces holding an agglomerate together are weak forces, for example van der Waals forces, or simple physical entanglement.Note 2 to entry: Agglomerates are also termed secondary particles and the origi
36、nal source particles are termed primary particles.SOURCE: ISO/TS 80004-4:2011, 2.83.6aggregateparticle comprising strongly bonded or fused particles where the resulting external surface area may be significantly smaller than the sum of calculated surface areas of the individual componentsNote 1 to e
37、ntry: The forces holding an aggregate together are strong forces, for example covalent bonds, or those resulting from sintering or complex physical entanglement.Note 2 to entry: Aggregates are also termed secondary particles and the original source particles are termed primary particles.SOURCE: ISO/
38、TS 80004-4:2011, 2.73.7particle sizelinear dimension of a particle (3.4) determined by a specified measurement method and under specified measurement conditionsNote 1 to entry: Different methods of analysis are based on the measurement of different physical properties. Independent of the particle pr
39、operty actually measured, the particle size can be reported as a linear dimension, e.g. as an equivalent spherical diameter.SOURCE: ISO/TS 80004-6:2013, 3.1.13.8particle size distributiondistribution of particles (3.4) as a function of particle size (3.7)Note 1 to entry: Particle size distribution m
40、ay be expressed as cumulative distribution or a distribution density (distribution of the fraction of material in a size class, divided by the width of that class).SOURCE: ISO/TS 80004-6:2013, 3.1.23.9equivalent diameterdiameter of a sphere that produces a response by a given particle-sizing method,
41、 that is equivalent to the response produced by the particle being measuredNote 1 to entry: The physical property to which the equivalent diameter refers is indicated using a suitable subscript ISO 9276-1:1998.Note 2 to entry: For discrete-particle-counting, light-scattering instruments, an equivale
42、nt optical diameter is used.2 ISO 2016 All rights reservedBS ISO 19430:2016ISO 19430:2016(E)Note 3 to entry: Other material constants like density of the particle are used for the calculation of the equivalent diameter like Stokes diameter or sedimentation equivalent diameter. The material constants
43、, used for the calculation, should be reported additionally.Note 4 to entry: For inertial instruments, the aerodynamic diameter is used. Aerodynamic diameter is the diameter of a sphere of density 1 000 kg m3that has the same settling velocity as the irregular particle.SOURCE: ISO/TS 80004-6:2013, 3
44、.1.53.10light scatteringchange in propagation of light at the interface of two media having different optical propertiesSOURCE: ISO 13320:2009, 3.1.173.11hydrodynamic diameterequivalent spherical diameter of a particle in a liquid having the same diffusion coefficient as the real particle in that li
45、quidSOURCE: ISO/TS 80004-6:2013, 3.2.63.12particle tracking analysisPTAmethod where particles undergoing Brownian motion in a liquid suspension are illuminated by a laser and the change in position of individual particles is used to determine particle sizeNote 1 to entry: Analysis of the time-depend
46、ent particle position yields translational diffusion coefficient and hence the particle size as hydrodynamic diameter using the Stokes-Einstein relationship.Note 2 to entry: Nanoparticle Tracking Analysis (NTA) is often used to describe PTA. NTA is a subset of PTA since PTA covers larger range of pa
47、rticle sizes than nanoscale (3.1).SOURCE: ISO/TS 80004-6:2013, 3.2.8, modified Nanoparticle tracking analysis has been removed from the term, and Notes 1 and 2 have been modified.3.13nanomaterialmaterial with any external dimension in the nanoscale (3.1) or having internal structure or surface struc
48、ture in the nanoscaleSOURCE: ISO/TS 80004-1:2015, 2.43.14diluentnon-volatile homogeneous liquid which is used to decrease the number concentration of particles (3.4) in a suspension without any deleterious effects such as changing particle total number, state of aggregation, particle size (3.7) or s
49、urface chemistry3.15viscositymeasure of the resistance to flow or deformation of a liquidSOURCE: ISO 3104:19943.16percentilevalue of a variable below which a certain percentage of observations fallSOURCE: ISO 11064-4:2013, 3.7 ISO 2016 All rights reserved 3BS ISO 19430:2016ISO 19430:2016(E)4 Symbols and abbreviated termsFor the purposes of this document, the following symbols and abbreviated terms apply.CCD Charge Coupled DeviceCMOS Complementary Metal Oxide SemiconductorCV Coefficient of Variation (st
