DIN EN 13900-6-2013 Pigments and extenders Methods of dispersion and assessment of dispersability in plastics Part 6 Determination by film test German version EN 13900-6 2012《颜料和填充.pdf

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1、January 2013 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 83.040.30!$“1936190www.din.deDDIN EN 13900-6Pigments and extenders Methods of dispersion and assessment of dispersability in plastics Part 6: Determination by film test;English version EN 13900-6:2012,English translation of DIN EN 13900-6:2013-01Pigmente und Fllstoffe Dispergierverfahren und Beurt

3、eilung der Dispergierbarkeit in Kunststoffen Teil 6: Bestimmung mit dem Folientest;Englische Fassung EN 13900-6:2012,Englische bersetzung von DIN EN 13900-6:2013-01Pigments et matires de charge Mthodes de dispersion et valuation de laptitude la dispersion dans les plastiques Partie 6: Dtermination p

4、ar essai de film;Version anglaise EN 13900-6:2012,Traduction anglaise de DIN EN 13900-6:2013-01www.beuth.deDocument comprises 17 pagesIn case of doubt, the German-language original shall be considered authoritative.12.12 DIN EN 13900-6:2013-01 2 A comma is used as the decimal marker. National forewo

5、rd This document (EN 13900-6:2012) has been prepared by Technical Committee CEN/TC 298 “Pigments and extenders” (Secretariat: DIN , Germany), Working Group WG 1 Colouring materials in plastics. The responsible German body involved in its preparation was the Normenausschuss Pigmente und Fllstoffe (Pi

6、gments and Extenders Standards Committee), Working Committee NA 078-00-05 AA Farbmittel fr Kunststoffe. EN 13900-6:2012 is one of a series of European Standards dealing with pigments and extenders. DIN EN 13900 consists of the following parts, under the general title Pigments and extenders Methods o

7、f dispersion and assessment of dispersibility in plastics: 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 ease of dispersion of black and col

8、our 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 The DIN Standards corresponding to the

9、International Standards referred to in this document are as follows: ISO 4618 DIN EN ISO 4618 ISO 21227-1 DIN EN ISO 21227-1 ISO/TS 27687 DIN ISO/TS 27687 (DIN SPEC 1121) DIN EN 13900-6:2013-01 3 National Annex NA (informative) Bibliography DIN EN ISO 4618, Paints and varnishes Terms and definitions

10、 DIN EN ISO 21227-1, Paints and varnishes Evaluation of defects on coated surfaces using optical imaging Part 1: General guidance DIN ISO/TS 27687 (DIN SPEC 1121), Nanotechnologies Terminology and definitions for nano-objects Nanoparticle, nanofibre and nanoplate DIN EN 13900-6:2013-01 4 This page i

11、s intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13900-6 October 2012 ICS 83.040.30 English Version Pigments and extenders - Methods of dispersion and assessment of dispersability in plastics - Part 6: Determination by film test Pigments et matires de charge - Mthodes de di

12、spersion et valuation de laptitude la dispersion dans les plastiques - Partie 6: Dtermination par essai de film Pigmente und Fllstoffe - Dispergierverfahren und Beurteilung der Dispergierbarkeit in Kunststoffen - This European Standard was approved by CEN on 8 September 2012. CEN members are bound t

13、o comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European 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-C

14、ENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (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

15、the same status as the official versions. 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, Luxe

16、mbourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, 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

17、 All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13900-6:2012: ETeil 6: Bestimmung mit dem Folientest EN 13900-6:2012 (E) 2 Contents Page Foreword 31 Scope 42 Terms and definitions .43 Principle 64 Materials .75 Apparatus .86 Preparati

18、on of test mixtures .86.1 General 86.2 Test mixture 87 Procedure .97.1 Calibration 97.2 Size ranges and resolution .97.3 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 1

19、2Bibliography . 13DIN EN 13900-6:2013-01 EN 13900-6:2012 (E) 3 Foreword This document (EN 13900-6:2012) has been prepared by 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, eith

20、er by publication of an identical text or by endorsement, at the latest by April 2013, and conflicting national standards shall 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 C

21、ENELEC shall not be held responsible for identifying any or all such patent rights. EN 13900, Pigments and extenders Methods of dispersion and assessment of dispersibility in plastics, contains the following parts: Part 1: General introduction; Part 2: Determination of colouristic properties and eas

22、e of dispersion 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

23、polyethylene by two-roll milling; Part 5: Determination by filter pressure value test; Part 6: Determination by film test (the present document). According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European St

24、andard: 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, Slovakia, Slovenia,

25、Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 13900-6:2013-01 EN 13900-6:2012 (E) 4 1 Scope This European Standard 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

26、extenders in the form of concentrates or compounds in all polymers used for extrusion processes. NOTE Defects like gels, black specks, 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, conditio

27、ns and test polymer being used. The use of test conditions differing from those specified might give different results. The preparation methods of concentrates or compounds are not specified in this standard. The results obtained for individual colorants and/or extenders are therefore comparable onl

28、y when the same conditions of preparation for concentrates or compounds and a comparable detection system are used. 2 Terms and definitions 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 c

29、olorant and/or extender, impurities of basic test polymer 2.2 primary particle of the colorant smallest single unit detectable by 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

30、particles where the resulting external surface area may be significantly smaller than the sum of calculated surface areas of the individual components Note 1 to entry: The forces holding an aggregate together are strong forces, for example, covalent bonds, or those resulting from sintering or comple

31、x physical entanglement. Note 2 to entry: Aggregates are also termed secondary particles and the original source particles are termed 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 extern

32、al surface area is similar to the sum of the surface areas of the individual components Note 1 to entry: The forces holding an agglomerate 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

33、 material. DIN EN 13900-6:2013-01 EN 13900-6:2012 (E) 5 Note 2 to entry: Agglomerates are also termed secondary particles and the original 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 s

34、peck size class one or more categories defined by a minimum and maximum value of speck sizes within the total speck size range 2.7 inspected 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

35、by inspected film area Note 1 to entry: The unit is mm/m. 2.9 transmission illumination illumination whereby light source and optical sensor 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 gre

36、y level shade of grey assigned to a pixel Note 1 to entry: The shades are usually positive integer values taken from the grey scale. SOURCE: 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 corre

37、sponds 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 length 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. DIN EN 13900-6:2013-01 E

38、N 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 21227-1:2003, 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 wit

39、h specified amount of defects which has already been assessed Note 1 to entry: It is used to check the reproducibility and repeatability of 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

40、 fitted with a blown film unit or a cast film unit followed by appropriate downstream equipment. After 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 pr

41、esence of particles (primary particles, aggregates, agglomerates), are assessed using appropriate software. Figure 1 illustrates the principle construction of the apparatus. DIN EN 13900-6:2013-01 EN 13900-6:2012 (E) 7 Key 1 extruder 2 die 3 take off unit2)4 data processing 5 camera system 6 diffuse

42、r, optional 7 light source 8 speed determination3)9 winder Figure 1 Scheme for cast film extrusion 4 Materials 4.1 Concentrate Homogeneous preparation 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

43、between the interested parties, preferably of a film grade. NOTE The development work on this standard was carried out in low density polyethylene (LDPE). 2) Take off units with two rollers are also possible. 3) Different kinds of speed controller systems are possible. DIN EN 13900-6:2013-01 EN 1390

44、0-6:2012 (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. 5 Apparatus 5.1 Extruder An extruder without dispersing elements should be used. No filter should be used in the extrusion line. For laboratory testin

45、g 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 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 repr

46、oducibility of results when examining highly transparent films. 6 Preparation of test mixtures 6.1 General The 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.

47、 The viscosities of concentrate and test polymer should be compatible in order to get a homogeneous distribution. The test polymer and the processing 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

48、 therefore be agreed between the interested parties prior to testing. If the produced film made from the test 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 = 1 % in the test mixture). E