1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationPigments and extenders Methods of dispersion and assessment of dispersability in plasticsPart 6: Determination by film testBS EN 13900-6:2012National forewordThis British Standar
2、d is the UK implementation of EN 13900-6:2012.The UK participation in its preparation was entrusted to Technical CommitteeSTI/1, Pigments.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary pr
3、ovisions of acontract. Users are responsible for its correct application. The British Standards Institution 2012Published by BSI Standards Limited 2012ISBN 978 0 580 72655 2ICS 83.040.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was publishe
4、d under the authority of the StandardsPolicy and Strategy Committee on 30 November 2012.Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS EN 13900-6:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13900-6 October 2012 ICS 83.040.30 English Version Pigments and
5、 extenders - Methods of dispersion and assessment of dispersability in plastics - Part 6: Determination by film test Pigments et matires de charge - Mthodes de dispersion et valuation de laptitude la dispersion dans les plastiques - Partie 6: Dtermination par essai de film Pigmente und Fllstoffe - D
6、ispergierverfahren und Beurteilung der Dispergierbarkeit in Kunststoffen - Teil 6: Bestimmung mit dem Folientest This European Standard was approved by CEN on 8 September 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Eu
7、ropean Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versi
8、ons (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria,
9、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, Slovakia, Slovenia, Spain, Sweden, Sw
10、itzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members
11、. Ref. No. EN 13900-6:2012: EBS EN 13900-6:2012EN 13900-6:2012 (E) 2 Contents Page Foreword 31 Scope 42 Terms and definitions .43 Principle 64 Materials .75 Apparatus .86 Preparation of test mixtures .86.1 General 86.2 Test mixture 87 Procedure .97.1 Calibration 97.2 Size ranges and resolution .97.3
12、 Pre-conditioning . 107.4 Test procedure 117.4.1 Production of the test polymer film 117.4.2 Production of the test mixture film . 118 Evaluation 129 Test report . 1210 Precision 12Bibliography . 13BS EN 13900-6:2012EN 13900-6:2012 (E) 3 Foreword This document (EN 13900-6:2012) has been prepared by
13、Technical Committee CEN/TC 298 “Pigments and extenders”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by April 2013, and conflicting national standards sha
14、ll be withdrawn at the latest by April 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. EN 13900, Pigments and extenders Methods
15、of dispersion and assessment of dispersibility in plastics, contains the following parts: Part 1: General introduction; Part 2: Determination of colouristic properties and ease of dispersion in plasticized polyvinyl chloride by two-roll milling; Part 3: Determination of colouristic properties and ea
16、se 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 two-roll milling; Part 5: Determination by filter pressure value test; Part 6: Determination by film test (th
17、e present document). According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of M
18、acedonia, 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 Kingdom. BS EN 13900-6:2012EN 13900-6:2012 (E) 4 1 Scope This European Stan
19、dard 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 like gels, black spe
20、cks, holes in the test film etc. are not in the scope of this standard. 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 prepar
21、ation methods of concentrates or compounds are not specified in this standard. 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. 2 Terms and de
22、finitions For the purposes of this document, the following terms and definitions apply. 2.1 speck defect caused by agglomerates, aggregates and primary particles of the colorant and/or extender, impurities of basic test polymer 2.2 primary particle of the colorant smallest single unit detectable by
23、physical methods Note 1 to entry: Suitable physical methods are, for example, optical and electron microscopy. 2.3 aggregate particle 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 i
24、ndividual components Note 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 ter
25、med primary particles. SOURCE: ISO/TS 27687:2008, 3.3 2.4 agglomerate collection of weekly bound particles or aggregates or mixtures of the two where the resulting external surface area is similar to the sum of the surface areas of the individual components Note 1 to entry: The forces holding an agg
26、lomerate together are weak forces, for example van der Waals forces, or simple physical entanglement. 1) For the definition of colorant see, ISO 4618:2006, 2.58 colouring material. BS EN 13900-6:2012EN 13900-6:2012 (E) 5 Note 2 to entry: Agglomerates are also termed secondary particles and the origi
27、nal source particles are termed primary particles. SOURCE: ISO/TS 27687:2008, 3.2 2.5 total speck size range specified upper and lower limits of particle sizes 2.6 speck size class one or more categories defined by a minimum and maximum value of speck sizes within the total speck size range 2.7 insp
28、ected film area film area from the beginning to the end of the measurement Note 1 to entry: The unit is square metres. 2.8 speck area ratio total speck area divided by inspected film area Note 1 to entry: The unit is mm/m. 2.9 transmission illumination illumination whereby light source and optical s
29、ensor are arranged on opposite sides of the film 2.10 pixel smallest image-forming element to which a grey level is assigned SOURCE: ISO 21227-1:2003, 3.4.5 2.11 grey level shade of grey assigned to a pixel Note 1 to entry: The shades are usually positive integer values taken from the grey scale. SO
30、URCE: ISO 21227-1:2003, 3.4.7 2.12 grey scale series of grey levels between white and black EXAMPLE 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, 3.4.8 2.13 resolution number of pixels per unit le
31、ngth on the surface of an object Note 1 to entry: If the resolution in the X- and Y-direction is different, both values have to be reported. BS EN 13900-6:2012EN 13900-6:2012 (E) 6 SOURCE: ISO 21227-1:2003, 3.4.6 2.14 brightness average grey level of a specified part of the image SOURCE: ISO 21227-1
32、:2003, 3.5.3 2.15 contrast difference between the grey levels of two specified parts of the image SOURCE: ISO 21227-1:2003, 3.5.4 2.16 calibration film film with specified amount of defects which has already been assessed Note 1 to entry: It is used to check the reproducibility and repeatability of
33、the parameter settings. 3 Principle The 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. After extrusion, the transmission illuminat
34、ion 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 software. Figure 1 illustrates the princip
35、le construction of the apparatus. BS EN 13900-6:2012EN 13900-6:2012 (E) 7 Key 1 extruder 2 die 3 take off unit2)4 data processing 5 camera system 6 diffuser, optional 7 light source 8 speed determination3)9 winder Figure 1 Scheme for cast film extrusion 4 Materials 4.1 Concentrate Homogeneous prepar
36、ation of colorants and/or extenders in an appropriate thermoplastic polymer. 4.2 Basic test polymer Thermoplastic polymer of a type and grade to be agreed between the interested parties, preferably of a film grade. NOTE The development work on this standard was carried out in low density polyethylen
37、e (LDPE). 2) Take off units with two rollers are also possible. 3) Different kinds of speed controller systems are possible. BS EN 13900-6:2012EN 13900-6:2012 (E) 8 4.3 Test mixture A homogeneous mixture of a concentrate (4.1) and the basic test polymer (4.2) or a compound as specified in Clause 6.
38、5 Apparatus 5.1 Extruder An extruder without dispersing elements should be used. 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 (length/diameter) to 30 L/D (length/diameter) is recomme
39、nded. 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 mixtures 6.1 General The concentrate (4.1) and the basic test po
40、lymer (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 distribution. The test polymer and the processing
41、should not influence the detection of specks. 6.2 Test mixture The 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 test mixture is not homogeneous, a compound s
42、hall 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 = 1 % in the test mixture). EXAMPLE 2 Inorgan
43、ic colorant: A total amount of 1000 g (100 %) contains 950 g polymer, 50 g colour concentrate with 40 % colorant content (contains 20 g inorganic colorant = 2 % in the test mixture). BS EN 13900-6:2012EN 13900-6:2012 (E) 9 7 Procedure 7.1 Calibration The 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 cal
45、ibration 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 uni
46、formity of the field of inspection shall be checked. 7.2 Size ranges and resolution The theoretical limit for resolution of objects by size using image analysis is 1 pixel. Defects should be assessed speck by speck with the minimum number of 4 pixel. EXAMPLE By the use of an optical resolution of 19
47、 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 the highest class is unlimited. For quantitative analysis, pixels
48、 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 deformation that will induce an image distortion caused by l
49、enticular light refraction (see Figure 2). BS EN 13900-6:2012EN 13900-6:2012 (E) 10 Key 1 deformation of the film surface by embedded speck 2 speck 3 refraction of light by the film surface 4 lights beam of a parallel light source 5 area with light refraction in the border speck area 6 area with brightness level 7 speck shadowing 8 cross section of a film 9 topographic view of a film Figure 2 Image distortion caused by lenticular light refraction of a speck 7.3 Pre-conditioning
