EN 13632-2010 pdf download.Bitumen and bituminous binders – Visualisation of polymer dispersion in polymer modified bitumen.
This EN 13632 specifies a method for visualisation of the polymer distribution in polymer modified bitumen by fluorescent 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.
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 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 following 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 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 minimum penod 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 Eplfluorescence microscope, (incident light excitation) with an appropriate light source and filter
systems.
NOTE Examples of light source and filter system are given in Annex A.
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 12594. Homogenise the sample by gentle hand stirring for at least 1 mm and not more than 5 mm. 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). 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 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 mm is sufficient.
NOTE The cooling procedure can be essential for the morphology. By cooling in the sand bath, a steady 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 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 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 surfaces 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.EN 13632-2010 pdf download.