EN 14770:2005
(Main)Bitumen and bituminous binders - Determination of complex shear modulus and phase angle - Dynamic Shear Rheometer (DSR)
Bitumen and bituminous binders - Determination of complex shear modulus and phase angle - Dynamic Shear Rheometer (DSR)
This European Standard specifies a number of methods using a dynamic shear rheometer (DSR) capable of measuring the rheological properties of bituminous binders. The procedure involves determining the complex shear modulus and phase angle of binders over a range of test frequencies and test temperatures when tested in oscillatory shear.
From the test, the norm of the complex shear modulus, IG*I, and its phase angle, d, at a given temperature and frequency can be calculated, as well as the components G', G'', J' and J'' of the complex shear modulus and of the complex compliance.
This method is applicable to unaged, aged and recovered bituminous binders, cut-backs and bituminous binders stabilised from emulsions.
WARNING - The use of this standard can involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use.
Bitumen und bitumenhaltige Bindemittel - Bestimmung des komplexen Schermoduls und des Phasenwinkels - Dynamisches Scherrheometer (DSR)
Diese Europäische Norm legt eine Reihe von Verfahren, in denen ein dynamisches Scherrheometer (DSR)
zur Anwendung kommt, mit dem die rheologischen Eigenschaften von bitumenhaltigen Bindemitteln
gemessen werden können, fest. Die Durchführung beinhaltet die Bestimmung des komplexen Schermoduls
und des Phasenwinkels von Bindemitteln über einen Bereich von Prüffrequenzen und Prüftemperaturen bei
der Prüfung im Schwing-Schermodus.
Aus der Prüfung können sowohl der Betrag des komplexen Schermoduls, IG*I, und der zugehörige
Phasenwinkel, δ , für eine gegebene Temperatur und Frequenz als auch deren Komponenten G', G'', J' und J''
des komplexen Schermoduls und der komplexen Nachgiebigkeit berechnet werden.
Dieses Verfahren gilt für nicht gealterte, gealterte und wiedergewonnene bitumenhaltige Bindemittel sowie
aus Emulsionen stabilisierte verschnittene oder gefluxte bitumenhaltige Bindemittel.
WARNUNG — Die Anwendung dieser Norm kann gefährliche Substanzen, Arbeitsgänge und
Ausrüstung einschließen. In der Norm werden nicht alle Sicherheitsprobleme angesprochen, die mit
ihrer Anwendung verbunden sind. Es liegt in der Verantwortung des Anwenders dieser Norm,
geeignete Gesundheitsschutz- und Sicherheitsmaßnahmen vorzusehen und vorher zu klären, ob
einschränkende Vorschriften zu berücksichtigen sind.
Bitumes et liants bitumineux - Détermination du module complexe en cisaillement et de l'angle de phase - Rhéomètre à cisaillement dynamique (DSR)
La présente Norme européenne traite de plusieurs méthodes faisant appel à un rhéomètre à cisaillement
dynamique (DSR) capable de mesurer certaines caractéristiques rhéologiques des bitumes et liants bitumineux. La
procédure repose sur la détermination du module complexe en cisaillement et de l’angle de phase, de liants sur
une plage de fréquences et de températures d’essai, lorsqu’ils sont soumis à l’essai en mode de cisaillement
oscillatoire.
À partir des résultats de cet essai, il est possible de calculer la norme du module complexe en cisaillement, IG*I, et
son angle de phase, d, à une température et à une fréquence données, ainsi que les composantes G', G'', J' et J''
du module complexe en cisaillement et de la complaisance complexe.
La méthode est applicable aux liants bitumineux neufs, après vieillissement artificiel ou récupérés d’un enrobé,
ainsi qu’aux liants bitumineux fluidifiés ou fluxés et aux liants bitumineux stabilisés à partir d’une émulsion.
AVERTISSEMENT — L'utilisation de la présente norme implique l'intervention de produits, d'opérations et
d'équipements à caractère dangereux. La présente norme n'est pas censée aborder tous les problèmes de
sécurité concernés par son usage. Il est de la responsabilité de l'utilisateur de consulter et d'établir des
règles d'hygiène et de sécurité appropriées et de déterminer l'applicabilité des restrictions réglementaires
avant utilisation.
Bitumen in bitumenska veziva – Ugotavljanje kompleksnega strižnega modula in faznega kota – Dinamini strižni reometer (DSR)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2005
Bitumen in bitumenska veziva – Ugotavljanje kompleksnega strižnega modula in
faznega kota – Dinamini strižni reometer (DSR)
Bitumen and bituminous binders - Determination of complex shear modulus and phase
angle - Dynamic Shear Rheometer (DSR)
Bitumen und bitumenhaltige Bindemittel - Bestimmung des komplexen Schermoduls und
des Phasenwinkels - Dynamisches Scherrheometer (DSR)
Bitumes et liants bitumineux - Détermination du module complexe en cisaillement et de
l'angle de phase - Rhéometre a cisaillement dynamique (DSR)
Ta slovenski standard je istoveten z: EN 14770:2005
ICS:
75.140 Voski, bitumni in drugi naftni Waxes, bituminous materials
proizvodi and other petroleum products
91.100.50 Veziva. Tesnilni materiali Binders. Sealing materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD
EN 14770
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2005
ICS 75.140; 91.100.50
English Version
Bitumen and bituminous binders - Determination of complex
shear modulus and phase angle - Dynamic Shear Rheometer
(DSR)
Bitumes et liants bitumineux - Détermination du module Bitumen und bitumenhaltige Bindemittel - Bestimmung des
complexe en cisaillement et de l'angle de phase - komplexen Schermoduls und des Phasenwinkels -
Rhéomètre à cisaillement dynamique (DSR) Dynamisches Scherrheometer (DSR)
This European Standard was approved by CEN on 26 August 2005.
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-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14770:2005: E
worldwide for CEN national Members.
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions.4
4 Principle.5
5 Apparatus .5
6 Preparation of rheometers .6
7 Sample preparation.7
8 Procedure .7
9 Expression of results.9
10 Precision.9
11 Test report .10
Annex A (informative) Temperature verification procedure.11
Annex B (informative) Determining equilibration time .12
Bibliography.13
Foreword
This European Standard (EN 14770:2005) has been prepared by Technical Committee CEN/TC 336
“Bituminous binders”, the secretariat of which is held by AFNOR.
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 2006, and conflicting national standards shall be withdrawn at the
latest by April 2006.
This European standard is based on IP PM CM-02 [1] and XPT 66-065 [2].
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland
and United Kingdom.
1 Scope
This European Standard specifies a number of methods using a dynamic shear rheometer (DSR) capable of
measuring the rheological properties of bituminous binders. The procedure involves determining the complex
shear modulus and phase angle of binders over a range of test frequencies and test temperatures when
tested in oscillatory shear.
From the test, the norm of the complex shear modulus, IG*I, and its phase angle, δ, at a given temperature
and frequency can be calculated, as well as the components G', G'', J' and J'' of the complex shear modulus
and of the complex compliance.
This method is applicable to unaged, aged and recovered bituminous binders, cut-back or fluxed bituminous
binders stabilised from emulsions.
WARNING — The use of this standard can involve hazardous materials, operations and equipment.
This standard does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this standard to establish appropriate health and safety 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 1427, Bitumen and bituminous binders – Determination of softening point – Ring and Ball method.
EN 12594, Bitumen and bituminous binders – Preparation of test samples.
3 Terms and definitions
For the purposes of this European Standard, the following terms and definitions apply.
3.1
norm of the complex shear modulus
IG*I
ratio of peak stress to the peak strain in harmonic sinusoidal oscillation
3.2
phase angle
δ
phase difference between stress and strain in harmonic sinusoidal oscillation
3.3
norm of the complex shear compliance
IJ*I
ratio of the peak strain to the peak stress in harmonic sinusoidal oscillation
NOTE The real parts of the complex shear modulus IG*I and the complex shear compliance IJ*I are respectively G’
and J’ and are associated with the elastic part of the material behaviour. The imaginary parts of the complex shear
modulus and the complex shear compliance are respectively G’’ and J’’ and are associated with the viscous part of the
material behaviour. The tangent of the phase angle δ represents the ratio of its viscous component over its elastic
component (e.g. tan δ equals G”/G’ or J”/J’).
3.4
isotherm
equation or curve on a graph representing the behaviour of a material at a constant temperature
3.5
isochron
equation or curve on a graph representing the behaviour of a material at a constant frequency
3.6
region of linear viscoelastic behaviour
region in which complex dynamic (shear) modulus is independent of (shear) stress or strain
4 Principle
A known oscillatory shear stress is applied to the temperature controlled test geometry, in which is held the
bituminous test specimen. The binder's strain response to the stress is measured. Alternatively, a known
oscillatory shear strain is applied to the test specimen and the resulting shear stress is measured.
5 Apparatus
Usual laboratory apparatus and glassware, together with the following:
5.1 Dynamic Shear Rheometer (DSR), with either an integral temperature control system or
temperature control attachments, capable of controlling the temperature over a minimum range of 5 °C to
85 °C with an accuracy of ± 0,1 °C throughout the test period. The rheometer shall be fitted with parallel plates,
with a constant gap across the area of the plates. The temperature control system shall encompass both
plates, to avoid temperature gradients across the plates. Where the test specimen is immersed in liquid other
than water, ensure that the liquid does not affect the properties of the material being analysed. The rheometer
shall be able to determine G*, in the range of 1 kPa to 10 MPa (± 2 %) and the phase angle (δ), in the range 0
to 90° (± 0,1°).
NOTE 1 For rheometers using an air bearing, and to avoid damage, the air supply to the bearing should be switched
on before the instrument is switched on. When not in use, the spindle should be secured.
NOTE 2 When liquid is used to immerse the test specimen, a water/glycol mixture has been found to be suitable. The
proportions used depend on how low a temperature it is intended to test. Rheometers using radio frequency (RF) heating
and/or liquid gas cooling should be used in accordance with the manufacturers instructions.
NOTE 3 Where the bottom plate is nominally the same diameter as the top plate, then a visual check should be made
to ensure the two plates are vertically aligned. If there is any doubt as to the alignment of the top and bottom plates, then
the manufacturer, or a qualified technician, should re-align the plate geometry.
NOTE 4 For information, diameters from 8 mm to 25 mm and gap settings from 0,5 mm to 2,0 mm have been found to
be suitable for bituminous binders. In terms of operational ranges, 25 mm plates are generally suitable for stiffnesses in
the range 1 kPa to 100 kPa and 8 mm plates suitable for stiffnesses (|G*|) in the range 100 kPa to 10 MPa. Plates of other
diameters can also be used, providing compliance effects of the instrument are not affecting the results (see 6.1, Note 1)
and the testing is done in the linear region, see 8.
NOTE 5 The fact that the temperature control range is 5 °C to 85 °C should not be taken to imply that accurate results
will necessarily be obtained for all binders over this range (see 5.1, Note 4 and 6.1, Note 1). Also temperatures outside
this range can be used provided results are not affected by machine compliance.
5.2 Moulds, sheet materials or vials, for the preparation of the test specimens. The moulds or sheet
material, where used, shall be of silicone or similar material, which does not adhere to the test specimen. Vials
or containers, where used, shall be of an appropriate material and size for the purpose.
5.3 Oven, ventilated laboratory model, capable of being controlled at temperatures between 50 °C and
200 °C with an accuracy of ± 5 °C.
6 Preparation of rheometers
6.1 Set up
Set up the rheometer in the sequence given in the manufacturer's instructions, including the procedure for the
selecting and setting the correct geometry and gap. Select the appropriate oscillation package, if applicable,
from the software menu. It is essential that the operational limits of stiffness for the selected geometry are
determined.
NOTE 1 The selection of system geometry may affect the accuracy of results. The manufacturer may have determined
the operational limits and this information may be available but, if not, it can be determined by running a test specimen
over a range of test temperatures using all the test geometries likely to be used in practice, and plotting |G*| against either
frequency or phase angle (δ). Where the divergence between the plots for each geometry exceeds 15 %, this is an
indication that compliance effects are affecting one or more of the geometries. The chosen geometry(ies) which shows the
more rapid fall in |G*|, or the lower phase angle, indicates that its accuracy limit has been reached. Also, for most
rheometers generally used for this standard, irrespective of geometry chosen, values of |G*| in excess of 10 Pa are likely
to be suspect. Software corrections to the stiffness may be acceptable provided appropriate validation is supplied to the
operator.
NOTE 2 The rheometer and temperature control system should be calibrated at regular intervals in accordance with
the quality assurance procedure of the laboratory. A suitable method is that the rheometer and temperature control system
should be calibrated by a means traceable to a national standard. Also, it is adviseable to verify the accuracy of the
temperature control system by means of a certified temperature measuring device at regular intervals. Also note that
external devices read the accurate temperature value only if they are calibrated correctly. A temperature verification
procedure is described in Annex A.
NOTE 3 The temperature in the test sample may differ from the temperature read by the
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