1、BSI Standards PublicationBS ISO 23900-6:2015Pigments and extenders Methods of dispersion andassessment of dispersibility inplasticsPart 6: Determination by film testBS ISO 23900-6:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 23900-6:2015.The UK particip
2、ation in its preparation was entrusted to Technical Committee STI/1, Pigments.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 responsible for its corre
3、ct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 86266 3ICS 87.060.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strate
4、gy Committee on 30 April 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 23900-6:2015 ISO 2015Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics Part 6: Determination by film testPigments et matires de charge Mthodes de dis
5、persion et valuation de laptitude la dispersion dans les plastiques Partie 6: Dtermination par essai de filmINTERNATIONAL STANDARDISO23900-6First edition2015-05-01Reference numberISO 23900-6:2015(E)BS ISO 23900-6:2015ISO 23900-6:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO
6、2015All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise 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 reque
7、sted from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 23900-6:2015ISO 23900-6:2015(E)Foreword i
8、v1 Scope . 12 Terms and definitions . 13 Principle 34 Materials . 44.1 Concentrate 44.2 Basic test polymer 44.3 Test mixture . 45 Apparatus . 56 Preparation of test mixtures 56.1 General . 56.2 Test mixture . 57 Procedure. 57.1 Calibration 57.2 Size ranges and resolution 67.3 Pre-conditioning 77.4 T
9、est procedure . 87.4.1 Production of the test polymer film 87.4.2 Production of the test mixture film 88 Evaluation 99 Test report . 910 Precision . 9Bibliography .10 ISO 2015 All rights reserved iiiContents PageBS ISO 23900-6:2015ISO 23900-6:2015(E)ForewordISO (the International Organization for St
10、andardization) 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 a subject for which a technical committee has been established has the rig
11、ht 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 Commission (IEC) on all matters of electrotechnical standardization.The procedures
12、 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 should be noted. This document was drafted in accordance with the editorial rul
13、es 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 identifying any or all such patent rights. Details of any patent rights identi
14、fied 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 convenience of users and does not constitute an endorsement.For an explanation on
15、 the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), see the following URL: Foreword Supplementary information .The committee responsible for this document is I
16、SO/TC 256, Pigments, dyestuffs and extenders.ISO 23900 consists of the following parts, under the general title Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics: Part 1: General introduction Part 2: Determination of colouristic properties and ease of dispersi
17、on in plasticized polyvinyl chloride by two-roll milling Part 3: Determination of colouristic properties and ease of dispersion of black and colour pigments in polyethylene by two-roll milling Part 4: Determination of colouristic properties and ease of dispersion of white pigments in polyethylene by
18、 two-roll milling Part 5: Determination by filter pressure value test Part 6: Determination by film testiv ISO 2015 All rights reservedBS ISO 23900-6:2015Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics Part 6: Determination by film test1 ScopeThis part of IS
19、O 23900 specifies a method assessing the degree of dispersion of colorants1)and/or extenders in a thermoplastic polymer.The method is suitable for testing colorants and/or extenders in the form of concentrates or compounds in all polymers used for extrusion processes.NOTE Defects such as gels, black
20、 specks, holes in the test film are not in the scope of this part of ISO 23900.The film test result determined according to this method is valid only for the equipment, conditions and test polymer being used. The use of test conditions differing from those specified might give different results. The
21、 preparation methods of concentrates or compounds are not specified in this part of ISO 23900. The results obtained for individual colorants and/or extenders are therefore comparable only when the same conditions of preparation for concentrates or compounds and a comparable detection system are used
22、.2 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.2.1speckdefect caused by agglomerates, aggregates and primary particles of the colorant and/or extender, impurities of basic test polymer2.2primary particle of the colorantsmallest single unit detect
23、able by physical methodsNote 1 to entry: Suitable physical methods are, for example, optical and electron microscopy.2.3aggregateparticle comprising strongly bonded or fused particles where the resulting external surface area may be significantly smaller than the sum of calculated surface areas of t
24、he individual componentsNote 1 to entry: 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 t
25、ermed primary particles.SOURCE: ISO/TS 27687:2008, 3.31) For the definition of colorant see ISO 4618:2014, 2.60 colouring material.INTERNATIONAL STANDARD ISO 23900-6:2015(E) ISO 2015 All rights reserved 1BS ISO 23900-6:2015ISO 23900-6:2015(E)2.4agglomeratecollection of weekly bound particles or aggr
26、egates or mixtures of the two where the resulting external surface 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 entr
27、y: Agglomerates are also termed secondary particles and the original source particles are termed primary particles.SOURCE: ISO/TS 27687:2008, 3.22.5total speck size rangespecified upper and lower limits of particle sizes2.6speck size classone or more categories defined by a minimum and maximum value
28、 of speck sizes within the total speck size range2.7inspected film areafilm area from the beginning to the end of the measurementNote 1 to entry: The unit is square metres.2.8speck area ratiototal speck area divided by inspected film areaNote 1 to entry: The unit is mm/m.2.9transmission illumination
29、illumination whereby light source and optical sensor are arranged on opposite sides of the film2.10pixelsmallest image-forming element to which a grey level is assignedSOURCE: ISO 21227-1:2003, 3.4.52.11grey levelshade of grey assigned to a pixelNote 1 to entry: The shades are usually positive integ
30、er values taken from the grey scale.SOURCE: ISO 21227-1:2003, 3.4.72.12grey scaleseries of grey levels between white and blackEXAMPLE The 8-bit grey scale has 28(=256) grey levels. Grey level 0 corresponds to black, grey level 255 (the 256thlevel) to white.SOURCE: ISO 21227-1:2003, 3.4.82 ISO 2015 A
31、ll rights reservedBS ISO 23900-6:2015ISO 23900-6:2015(E)2.13resolutionnumber of pixels per unit length on the surface of an objectNote 1 to entry: If the resolution in the X- and Y-direction is different, both values have to be reported.SOURCE: ISO 21227-1:2003, 3.4.62.14brightnessaverage grey level
32、 of a specified part of the imageSOURCE: ISO 21227-1:2003, 3.5.32.15contrastdifference between the grey levels of two specified parts of the imageSOURCE: ISO 21227-1:2003, 3.5.42.16calibration filmfilm with specified amount of defects which has already been assessedNote 1 to entry: It is used to che
33、ck the reproducibility and repeatability of the parameter settings.3 PrincipleThe test mixture, consisting of a colour concentrate and a basic test polymer or the compound, is passed through an extruder fitted with a blown film unit or a cast film unit followed by appropriate downstream equipment.Af
34、ter extrusion, the transmission illumination enables the detection of specks within the film by means of a camera inspection system.The resulting variations in contrast or brightness, caused by the presence of particles (primary particles, aggregates, agglomerates), are assessed using appropriate so
35、ftware.Figure 1 illustrates the principle construction of the apparatus. ISO 2015 All rights reserved 3BS ISO 23900-6:2015ISO 23900-6:2015(E)Key1 extruder 6 diffuser, optional2 die 7 light source3 take off unita8 speed determinationb4 data processing 9 winder5 camera systemaTake off units with two r
36、ollers are also possible.bDifferent kinds of speed controller systems are possible.Figure 1 Scheme for cast film extrusion4 Materials4.1 ConcentrateHomogeneous preparation of colorants and/or extenders in an appropriate thermoplastic polymer.4.2 Basic test polymerThermoplastic polymer of a type and
37、grade to be agreed between the interested parties, preferably of a film grade.NOTE The development work on this part of ISO 23900 was carried out in low density polyethylene (LDPE).4.3 Test mixtureA homogeneous mixture of a concentrate (4.1) and the basic test polymer (4.2) or a compound as specifie
38、d in Clause 6.4 ISO 2015 All rights reservedBS ISO 23900-6:2015ISO 23900-6:2015(E)5 Apparatus5.1 Extruder, without dispersing elements. No filter should be used in the extrusion line.For laboratory testing a single screw extruder with a diameter between 19 mm and 30 mm and with a length of 20 L/D (l
39、ength/diameter) to 30 L/D (length/diameter) is recommended.5.2 Blown film unit or cast film unit.5.3 Camera detection system.5.4 Diffuser, if necessary.NOTE The usage of a diffuser can increase the reproducibility of results when examining highly transparent films.6 Preparation of test mixtures6.1 G
40、eneralThe concentrate (4.1) and the basic test polymer (4.2) are mixed together, for example in a glass or plastic container, to provide the test mixture (4.3). Alternatively, a compound can be used.The viscosities of concentrate and test polymer should be compatible in order to get a homogeneous di
41、stribution.The test polymer and the processing should not influence the detection of specks.6.2 Test mixtureThe test mixture depends on the type of colorant and/or extender and polymer. It should therefore be agreed between the interested parties prior to testing.If the produced film made from the t
42、est mixture is not homogeneous, a compound shall be produced prior to film extrusion.EXAMPLE 1 Organic colorant or carbon black: a total amount of 1000 g (100 %) test mixture contains 975 g polymer, 25 g colour concentrate with 40 % colorant content (contains 10 g organic colorant or carbon black =
43、1 % in the test mixture).EXAMPLE 2 Inorganic colorant: a total amount of 1 000 g (100 %) contains 950 g polymer, 50 g colour concentrate with 40 % colorant content (contains 20 g inorganic colorant = 2 % in the test mixture).7 Procedure7.1 CalibrationThe equipment shall be calibrated in order to gua
44、rantee the correct measurement of size and numbers of black dots on the calibration film.The whole system should be verified with a calibration film with printed or plotted black dots under operating conditions. Three different sizes of certified printed or plotted black dots should be used for cali
45、bration of the system within the range of interest, e.g. values near the expected maximum, average and minimum particle sizes to be measured with the system. Additionally, the calibration film shall include a printed black dot with a defined diameter of 25 % to 50 % of the inspection width. The unif
46、ormity of the field of inspection shall be checked. ISO 2015 All rights reserved 5BS ISO 23900-6:2015ISO 23900-6:2015(E)7.2 Size ranges and resolutionThe theoretical limit for resolution of objects by size using image analysis is 1 pixel. Defects should be assessed speck by speck with the minimum nu
47、mber of 4 pixel.EXAMPLE By the use of an optical resolution of 19 m/pixel, the theoretically minimum of equivalent circular diameter is 42 m based on an evaluation of minimum 4 pixel.It is necessary to specify speck size classes. This should be done by the interested parties.NOTE 1 The maximum of th
48、e highest class is unlimited.For quantitative analysis, pixels should be converted to length and area units prior to any reporting.NOTE 2 The determination of the real size of specks is not feasible in any case as their embedding in the film leads to optical imperfections. The speck may cause a film
49、 deformation that will induce an image distortion caused by lenticular light refraction (see Figure 2).6 ISO 2015 All rights reservedBS ISO 23900-6:2015ISO 23900-6:2015(E)Key1 deformation of the film surface by embedded speck2 speck3 refraction of light by the film surface4 lights beam of a parallel light source5 area with light refraction in the border speck area6 area with brightness level7 speck shadowing8 cross section of a film9 topographic view of a filmFigure 2 Image distortion caused by lenticula
