1、November 2010 Translation by DIN-Sprachendienst.English price group 9No 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 75.140; 91.100.50!$lF“1733588www.din.deDDIN EN 13632Bitumen and bituminous binders Visualisation of polymer dispersion in polymer modified bitumenEnglish translation of DIN EN 13632:2010-11Bitumen und bitumenhaltige Bindemittel Visualisierung der Polymerverteilung in polymermodifiziertem BitumenEn
3、glische bersetzung von DIN EN 13632:2010-11Bitumes et liants bitumineux Visualisation de la dispersion des polymres dans les bitumes modifis par des polymresTraduction anglaise de DIN EN 13632:2010-11SupersedesDIN EN 13632:2004-03www.beuth.deDocument comprises pagesIn case of doubt, the German-langu
4、age original shall be considered authoritative.1211.10 DIN EN 13632:2010-11 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 336 “Bituminous binders” (Secretariat: AFNOR, France). The responsible German bodies involved in its prep
5、aration were the Normenausschuss Materialprfung (Materials Testing Standards Committee) and the Normenausschuss Bauwesen (Building and Civil Engineering Standards Committee), Joint Committee NA 062-03-32 GA Bitumen; Prfverfahren und Anforderungen fr die Bindemittel. Amendments This standard differs
6、from DIN EN 13632:2004-03 as follows: a) 4.7 “Temperature regulated sand bath” has been added; b) the standard has been editorially revised. Previous editions DIN EN 13632: 2004-03 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13632 May 2010 ICS 75.140; 91.100.50 Supersedes EN 13632:2003Eng
7、lish Version Bitumen and bituminous binders - Visualisation of polymer dispersion in polymer modified bitumen Bitumes et liants bitumineux - Visualisation de la dispersion des polymres dans les bitumes modifis par des polymres Bitumen und bitumenhaltige Bindemittel - Visualisierung der Polymervertei
8、lung in polymermodifiziertem Bitumen This European Standard was approved by CEN on 23 April 2010. CEN members are bound to 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
9、-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN 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 unde
10、r the responsibility of a CEN member into its own language and notified to the CEN Management Centre has 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, France, Germany,
11、 Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Man
12、agement Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13632:2010: EEN 13632:2010 (E) 2 Contents age Foreword 31 Scope 42 Normative references 43 Principle 44 Apparatus . 45 Preparati
13、on of test samples 56 Procedure . 57 Expression of results 58 Test report 5Annex A (informative) Bitumen modified by polymers . 7DIN EN 13632:2010-11 PEN 13632:2010 (E) 3 Foreword This document (EN 13632:2010) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secretariat
14、of which is held by AFNOR/BNP. 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 November 2010, and conflicting national standards shall be withdrawn at the latest by November 2010. Attention is dra
15、wn 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. This document supersedes EN 13632:2003. Annex A is informative. According to the CEN/CENELEC Internal
16、Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg
17、, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 13632:2010-11 EN 13632:2010 (E) 4 1 Scope This European Standard specifies a method for visualisation of the polymer distribution in polymer modified bitumen by fluo
18、rescent microscopy. The method is applicable for most of the commercially used polymers, but before the method is used it should be examined whether the test is applicable for the actual polymer. The method should only be used for identification purposes, i.e. in connection with production control.
19、NOTE Sample preparation and treatment have an important influence on the test results and it is essential to follow strictly the method described to achieve comparable results. WARNING The use of this European Standard can involve hazardous materials, operations and equipment. This European Standard
20、 does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The foll
21、owing referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 58, Bitumen and bituminous binders Sampling bituminous
22、 binders EN 12594, Bitumen and bituminous binders Preparation of test samples 3 Principle A sample of polymer modified bitumen is homogenised by gentle stirring and poured into a preheated mould. After a controlled cooling procedure to ambient temperature the sample is cooled below 20 C for a minimu
23、m period of time. The bitumen layer is broken into small pieces and the freshly broken surface is viewed through a microscope with a magnification of 25 times to 500 times. The views can be stored photographically or electronically. 4 Apparatus 4.1 Epifluorescence microscope, (incident light excitat
24、ion) with an appropriate light source and filter systems. NOTE Examples of light source and filter system are given in Annex A. 4.2 Freezer or solid carbon dioxide. 4.3 Sharp tool. Scissors shall not be used. 4.4 Aluminium basin, disposable, approximate height 35 mm, approximate diameter 70 mm. 4.5
25、Porcelain evaporating basin, diameter 150 mm, height 63 mm (approximate volume: 600 ml). DIN EN 13632:2010-11 EN 13632:2010 (E) 5 4.6 Fine aggregate (sand). 4.7 Temperature regulated sand bath. 5 Preparation of test samples Take the sample in accordance with EN 58. Prepare it in accordance with EN 1
26、2594. Homogenise the sample by gentle hand stirring for at least 1 min and not more than 5 min. Pour the material into the aluminium basin placed in a sand bath (4.7) preheated to the same temperature as the sample during homogenising. The sand bath is an evaporating basin (4.5) containing sand (4.6
27、). The aluminium basin (4.4) shall be totally surrounded by the sand and there shall be 20 mm of sand between the bottom of aluminium basin and the evaporating basin. The sample is cooled to ambient temperature by switching off the heating of the sand bath. After cooling to ambient temperature, cool
28、 the sample to 20 C or lower if the sample needs to become brittle. Using a freezer (4.2), a cooling time of 3 h minimum is required; using solid carbon dioxide (4.2) in a dewar, 10 min is sufficient. NOTE The cooling procedure can be essential for the morphology. By cooling in the sand bath, a stea
29、dy cooling rate is assured. 6 Procedure Prepare small pieces of the frozen material by breaking or cutting with appropriate sharp tool (4.3). This preparation shall be done rapidly to avoid warming the sample. Inspect the freshly broken or cut surface within 1 h. The inspection can be done through a
30、 protecting glass or directly on the surface. Using a protecting glass turn the freshly broken surface towards a microscope cover glass and arrange for the freshly broken or cut surfaces to stick to this without disturbing the surface by moving. Turn the cover glass over and place it on the hole of
31、the rigid support such that a perfectly horizontal and flat surface is observed through the glass. Select the magnification according to the particle size and distribution; magnifications of 25 to 500 are suitable. Analyse each polymer modified bitumen on a minimum of 3 independently prepared surfac
32、es scanning the entire surface before collecting the typical picture. Provide a reference scale with the picture. NOTE The picture can be obtained and stored by photographic or electronic systems. 7 Expression of results Express the binder morphology either as a picture, a picture number (according
33、to Annex A) or a combination of the characterisation letters shown in Annex A. Intermediate numbers are not allowed. If no fluorescent emission can be detected and the sample appears all black, note this as O. NOTE Numbers are used as a simple tool for comparing pictures and neither assessing the qu
34、ality, nor the performance of the binder. 8 Test report The test report shall contain at least the following information: a) type and complete identification of the sample under test; b) reference to this European Standard; DIN EN 13632:2010-11 EN 13632:2010 (E) 6 c) light source and filter system;
35、d) present the picture with a reference scale and if required a combination of the characterisation letters given in Annex A (see Clause 7); e) any deviation, by agreement or otherwise, from the procedure specified; f) date of the test. DIN EN 13632:2010-11 EN 13632:2010 (E) 7 Annex A (informative)
36、Bitumen modified by polymers A.1 Introduction Multiphase systems like bitumen polymer blends need a certain distribution of the discontinuous phase to maintain their structure over a long life time. The modification of bitumen with polymers can reach two principal phases. In the first case, the poly
37、mer is more or less dispersed in the bitumen matrix. Depending on the chemical composition of the materials, their compatibility and the input of dispersing energy as well as factors like molecular weight and polarity, the system remains homogenous over a certain period of time. The level of distrib
38、ution of the polymer phase has an important influence on the physical properties of the binder system. In the second case, the polymer phase becomes the continuous phase in which the bitumen is more or less finely dispersed, acting as a plasticiser or extender. Here the distribution of the bitumen i
39、n the polymer phase is of importance for the physical properties of the system. Beside the two principal cases, there are blends existing where phase inversion starts and both systems are visible at the same time. This phenomenon is also dependent on temperature and time. A way to assess the homogen
40、eity of a blend is to view it under a fluorescence microscope when illuminated by UV light: most of the polymers produce a yellow fluorescence while the bitumen remains dark. The particle size or distribution can be assessed under different magnifications. Special preparations are necessary to obtai
41、n a proper picture. The best way seems to be to cool the sample to a temperature of at least 20 C. Small pieces of the material are then broken or cut off, warmed up to ambient temperature and placed under the microscope for examination of the freshly broken surface. The distribution of the polymer
42、phase or bitumen can be assessed by measuring the particle size distribution or by comparison with standard pictures. If no structure is visible but a fine, homogeneous, slightly yellow light is detected, the product should be called homogeneous. Compatibility, stability and compliance can all be as
43、sessed by epifluorescence microscopy. It should be noted that fluorescence microscopy is not able to give a final quality assessment or indication of the binder performance. It provides important information for understanding of the system and parameters which might have an influence on the final qu
44、ality. A.2 Light source and filter system Example of light source and filter system: Light source: High pressure Xenon lamp, 75 W Excitation filter: BP 420/490 (transmit wavelengths from 420 nm 490 nm) Beam splitter filter: RKP 510 (reflects wavelengths shorter than 510 nm and transmits light of lon
45、ger wavelengths) DIN EN 13632:2010-11 EN 13632:2010 (E) 8 Barrier filter: LP 515 (transmits wavelengths longer than 515 nm) From the light source the light falls on the excitation filter, which transmits light from 420 nm to 490 nm. Light with this wavelength falls then on the surface of the specime
46、n. Unabsorbed exciting light and emitted light is then reflected to the chromatic beam splitter filter, which reflects light shorter than 510 nm and transmits light of longer wavelength. According to Stokes Law emitted light will have a longer wavelength than its exciting light, hence the beam split
47、ter filter effectively reflects exciting light and transmits emitted light, in this way separating the two. To eliminate any residual exciting light, the emitted/transmitted light with wavelength longer than 510 nm finally falls on the barrier filter, which has a high transmission for wavelengths lo
48、nger than 515 nm. A.3 Polymer bitumen pictures The following pictures show some typical dispersions of polymer in bitumen. The size of the pictures are 1,00 mm x 0,75 mm (approximately). The distribution can be described through a code of characterisation letters: Continuous phase: P: Continuous pol
49、ymer phase B: Continuous bitumen phase X: Both phases are continuous (inter twisted phases) Description of the phase: H: Homogeneous I: InhomogeneousDescription of size: S: small ( 100 m) Description of shape: r: roundish s: stripeso: other Some typical pictures are shown hereafter but not all possible morphologies are covered in these pictures. The pictures are characterised by a number and a letter code according to the system described above. DIN EN 13632:2010-11 EN 13632:2010 (E) 9 Figure A.1 P/I/L/r Figure A.2 B/
