prEN 14770

Bitumen and bituminous binders - Determination of complex shear modulus and phase angle - Dynamic Shear Rheometer (DSR)

This document specifies a general method of using a dynamic shear rheometer (DSR) for 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 complex shear modulus, |G*|, and its phase angle, δ, at a given temperature and frequency are calculated, as well as the components G' and G'' of the complex shear modulus.
This method is applicable to un-aged, aged and recovered bituminous binders.
WARNING -The use of this document can involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this document to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.

Bitumen und bitumenhaltige Bindemittel - Bestimmung des komplexen Schermoduls und des Phasenwinkels - Dynamisches Scherrheometer (DSR)

Dieses Dokument legt ein allgemeines Verfahren fest, bei dem ein dynamisches Scherrheometer (DSR) zur Anwendung kommt, mit dem die rheologischen Eigenschaften von bitumenhaltigen Bindemitteln gemessen werden können. Die Durchführung schließt die Bestimmung des komplexen Schermoduls und des Phasenwinkels von Bindemitteln über einen Bereich von Prüffrequenzen und Prüftemperaturen bei der Prüfung im Oszillations-Modus ein.
Aus der Prüfung werden sowohl der komplexe Schermodul, |G*|, und der zugehörige Phasenwinkel,δ,, für eine gegebene Temperatur und Frequenz als auch die Komponenten G' und G'' des komplexen Schermoduls berechnet.
Dieses Verfahren ist anwendbar für nicht gealterte, gealterte und rückgewonnene bitumenhaltige Bindemittel.
WARNUNG - Die Anwendung dieses Dokuments kann den Umgang mit gefährlichen Substanzen und Ausrüstungsteilen und die Ausführung gefährlicher Arbeitsgänge einschließen. Dieses Dokument erhebt nicht den Anspruch, alle mit seiner Anwendung verbundenen Sicherheitsprobleme anzusprechen. Es liegt in der Verantwortung des Anwenders dieses Dokuments, geeignete Verhaltensregeln für den Arbeits- und Gesundheitsschutz festzulegen und vor der Anwendung zu klären, ob einschränkende Vorschriften zu berücksichtigen sind.

Bitumes et liants bitumineux - Détermination du module complexe en cisaillement et de l'angle de phase à l'aide d'un rhéomètre à cisaillement dynamique (DSR)

Ce document spécifie une méthode générale faisant appel à l’utilisation d’un rhéomètre à cisaillement dynamique (DSR) pour mesurer les caractéristiques rhéologiques de liants bitumineux. La procédure repose sur la détermination du module complexe en cisaillement et de l’angle de phase des liants sur une plage de fréquences et de températures d’essai, lorsqu’ils sont testés en cisaillement oscillatoire.
À partir de cet essai, il est possible de déterminer le module complexe en cisaillement |G*| et son angle de phase , à une température et à une fréquence données, ainsi que les composantes G’ et G“ du module complexe en cisaillement.
Cette méthode est applicable aux liants bitumineux neufs, vieillis et récupérés.
AVERTISSEMENT — L'utilisation de ce document peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. Le présent document n'est pas censé aborder tous les problèmes de sécurité concernés par son usage. Il incombe à son utilisateur 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 - Dinamični strižni reometer (DSR)

General Information

• Status: Not Published
• Publication Date: 21-Dec-2023
• ICS: 75.140 - Waxes, bituminous materials and other petroleum products
• ICS: 91.100.50 - Binders. Sealing materials
• Technical Committee: CEN/TC 336 - Bituminous binders
• Drafting Committee: CEN/TC 336/WG 1 - Bituminous binders for paving
• Current Stage: 4599 - Dispatch of FV draft to CMC - Finalization for Vote
• Start Date: 16-Dec-2022
• Due Date: 31-Dec-2022
• Completion Date: 16-Dec-2022
• Ref Project: oSIST prEN 14770:2022 - Bitumen and bituminous binders - Determination of complex shear modulus and phase angle - Dynamic Shear Rheometer (DSR)

Relations

• Revises: EN 14770:2012 - Bitumen and bituminous binders - Determination of complex shear modulus and phase angle - Dynamic Shear Rheometer (DSR)
• Effective Date: 18-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN 14770:2022
01-maj-2022
Bitumen in bitumenska veziva - Ugotavljanje kompleksnega strižnega modula in
faznega kota - Dinamični 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 à l'aide d'un rhéomètre à cisaillement dynamique (DSR)
Ta slovenski standard je istoveten z: prEN 14770
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
oSIST prEN 14770:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN 14770:2022
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oSIST prEN 14770:2022
DRAFT
EUROPEAN STANDARD
prEN 14770
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2022
ICS 75.140; 91.100.50 Will supersede EN 14770:2012
English Version
Bitumen and bituminous binders - Determination of
complex shear modulus and phase angle - Dynamic Shear
Rheometer (DSR)

Bitumes et liants bitumineux - Détermination du Bitumen und bitumenhaltige Bindemittel -

module complexe en cisaillement et de l'angle de phase Bestimmung des komplexen Schermoduls und des

à l'aide d'un rhéomètre à cisaillement dynamique Phasenwinkels - Dynamisches Scherrheometer (DSR)

(DSR)

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 336.

If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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 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, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 14770:2022 E

worldwide for CEN national Members.
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Contents Page

European foreword ............................................................................................................................................ 3

1 Scope .......................................................................................................................................................... 5

2 Normative references .......................................................................................................................... 5

3 Terms and definitions ......................................................................................................................... 5

4 Principle ................................................................................................................................................... 6

5 Apparatus ................................................................................................................................................ 6

6 Preparation of rheometers ................................................................................................................ 7

6.1 General...................................................................................................................................................... 7

6.2 Selection of Geometry ......................................................................................................................... 7

6.3 Set up ......................................................................................................................................................... 8

6.4 Zero Gap Setting .................................................................................................................................... 8

7 Specimen preparation ......................................................................................................................... 8

7.1 General...................................................................................................................................................... 8

7.2 Heating procedure for binders prepared above 100 °C .......................................................... 8

7.3 Heating procedure for binders prepared at temperatures less than 100 °C .................. 9

7.4 Specimen manufacturing and storage conditions .................................................................... 9

8 Procedure ................................................................................................................................................ 9

8.1 General...................................................................................................................................................... 9

8.2 Specimen placing onto the rheometer ........................................................................................ 10

8.3 Gap setting ............................................................................................................................................. 10

8.4 Temperature and frequency conditions selecting .................................................................. 10

8.5 Testing measurement procedure ................................................................................................. 11

9 Expression of results ......................................................................................................................... 12

10 Precision ................................................................................................................................................ 12

11 Test report ............................................................................................................................................. 14

Annex A (informative) Temperature verification procedure .......................................................... 15

Annex B (informative) Determining equilibration time .................................................................... 16

Annex C (normative) Determination of the linear viscoelastic (LVE) range .............................. 17

Annex D (normative) Determining rheological parameters TX and δ ...................................... 18

Annex E (informative) Flow chart .............................................................................................................. 20

Bibliography ....................................................................................................................................................... 22

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European foreword

This document (prEN 14770:2022) has been prepared by Technical Committee CEN/TC 336 “Bituminous

binders”, the secretariat of which is held by AFNOR.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 14770:2012.

In comparison with the previous edition, the following technical modifications have been made:

a) reference to outdated standards IP PM CM-02 and XPT 66-065 removed;
b) integration of “complex compliance” removed;
c) use of the terms “shear strain” and “shear stress” unified;
d) use of the term “bituminous binder” unified;

e) reference to EN 1427 moved from Clause 2 to Bibliography; references to EN 12607-1, EN 14023 and

EN 14769 added to Bibliography;

f) definitions “shear strain controlled mode“ and “shear stress controlled mode” added;

g) use of the term “range of linear viscoelastic behaviour” unified;

h) use of the term “complex shear modulus” together with the corresponding symbol |G*| unified;

description of the complex shear modulus slightly revised;
i) 6.1, 7.1 and 8.1 added with reference to Annex E;

j) information about different plate diameters relocated from 5.1 to new 6.2; information about

different plate diameters in 6.2 updated and plate diameter of 4 mm added;
k) deviation for rheometer specification removed in 5.1;
l) suitable dimensions for silicone moulds added in 5.2;
m) vials for preparation of test specimen removed in 5.2. 7.3, 7.4 and 8.2;
n) use of the term “specimen” unified;
o) 6.4 “Zero gap setting” revised and clarified;
p) sub-samples smaller 50 g introduced in 7.2;
q) paring of specimen at room temperature removed in 7.4;
r) storage conditions and storage duration of specimens revised in 7.4;
s) 8.2 “Specimen placing onto the rheometer” and 8.3 “Gap setting” revised;
t) gap compensation added in 8.4;
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u) calculation of TX and δ added in Clause 9 and new Annex D;

v) Clause 10 revised and complemented with new precision data, instead of coefficient of variation

repeatability r and reproducibility R are now used;
w) terms c) and d) added in Clause 11;
x) revision of Annex C “Determination of the linear viscoelastic (LVE) range”;
y) Annex E “Flow Chart” added.
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1 Scope

This document specifies a general method of using a dynamic shear rheometer (DSR) for 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 complex shear modulus, |G*|, and its phase angle, δ, at a given temperature and

frequency are calculated, as well as the components G' and G'' of the complex shear modulus.

This method is applicable to un-aged, aged and recovered bituminous binders.

WARNING — The use of this document can involve hazardous materials, operations and equipment. This

document does not purport to address all of the safety problems associated with its use. It is the

responsibility of the user of this document to establish appropriate safety and health practices and to

determine the applicability of regulatory limitations prior to use.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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 12594, Bitumen and bituminous binders - Preparation of test samples
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
3.1
shear strain controlled mode

rheometer control mode where a demand angular displacement is applied to the specimen and the

corresponding torque is measured

Note 1 to entry: Using the shear strain factor of the measuring geometry, a specimen shear strain can be calculated

from the applied angular displacement. Using the shear stress factor of the measuring geometry, a specimen shear

stress can be calculated from the measured torque. Additional corrections can be applied to calculate true specimen

shear strain and true specimen shear stress.
3.2
shear stress controlled mode

rheometer control mode where a demand torque is applied to the specimen and the corresponding

angular displacement is measured

Note 1 to entry: Using the shear stress factor of the measuring geometry, a specimen shear stress can be calculated

from the applied torque. Using the shear strain factor of the measuring geometry, a specimen shear strain can be

calculated from the measured angular displacement. Additional corrections can be applied to calculate true

specimen shear stress and true specimen shear strain.
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3.3
complex shear modulus
|G*|

ratio of the amplitude of the shear stress to the amplitude of the shear strain in harmonic sinusoidal

oscillation

Note 1 to entry: The (mathematical) real part of the complex shear modulus |G*| is G´. It is associated with the

elastic part of material behaviour which represents energy stored during a shear cycle. The real part is the complex

shear modulus multiplied with cosine of phase angle expressed in degrees.

Note 2 to entry: The (mathematical) imaginary part of the complex shear modulus is G´´. It is associated with the

viscous part of material behaviour which represents energy dissipated during a shear cycle. The imaginary part is

the complex shear modulus multiplied with sine of phase angle expressed in degrees.

3.4
phase angle
phase difference between shear stress and shear strain in harmonic oscillation
3.5
isotherm

equation or curve on a graph representing the behaviour of a material at a constant temperature

3.6
isochrone

equation or curve on a graph representing the behaviour of a material at a constant frequency

3.7
range of linear viscoelastic behaviour

range in which complex shear modulus is independent of shear stress or shear strain

4 Principle

A known oscillatory shear stress is applied to the temperature controlled test geometry, in which the

bituminous test specimen is held. The binder's shear strain response to the shear stress is measured.

Alternatively, a known oscillatory shear strain is applied to the test specimen and the resulting shear

stress is measured.

Except for specific purposes, the test is performed in the region of linear viscoelastic behaviour.

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. Depending on the expected complex

shear modulus range different plate diameters (for example 25 mm, 8 mm or 4 mm) are used (see 6.2).

The temperature control system shall encompass both plates to avoid temperature gradients across the

plates. When 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 capable to determine |G*|, at

least in the range of 1 kPa to 10 MPa and the phase angle (δ), in the range 0° to 90°.

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NOTE 1 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 the temperature intended for testing is. Rheometers using radio

frequency (RF) heating and/or liquid gas cooling or other heating/cooling systems can be used in accordance with

the manufacturer's instructions.

Where the bottom plate is nominally the same diameter as the top plate, 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, the manufacturer, or a qualified technician, should re-align the plate geometry.

NOTE 2 The fact that the temperature control range is 5 °C to 85 °C does not imply that accurate results will

necessarily be obtained for all binders over this range (see 6.2 and 6.3, Note 1). Furthermore, temperatures outside

this range can also be used, provided the results are not affected by material or instrument limitations (see 6.2).

5.2 Moulds or sheet materials, 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.

For a testing geometry with a diameter of 25 mm and a gap setting of 1 mm, a mould with a cavity of

approximately 18 mm in diameter and 2 mm deep may be used. For a testing geometry with a diameter

of 8 mm and a gap setting of 2 mm, a mould with a cavity of approximately 8 mm in diameter and 2,5 mm

deep may be used. For a testing geometry with a diameter of 4 mm with different gap settings, a mould

with a cavity of approximately 4 mm in diameter and 3 mm deep may be used. In any case, the operator

shall assure adequate filling of the gap according to 8.3.

The use of grease or other anti-stick products should be avoided because they can affect the adherence

of the specimen to the rheometer plates.

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 General

An informative flow chart for preparation of rheometers is given in Annex E, Figure E.1.

6.2 Selection of Geometry

For different ranges of complex shear modulus plates of different diameters and gap settings shall be

used to respect the instruments limitations.

For determining complex shear modulus of bituminous binders in the range 1 kPa to 100 kPa, the

geometry with a diameter of 25 mm and a gap setting of 1,0 mm is suitable for most instruments. For

determining complex shear modulus of bituminous binders in the range 100 kPa to 10 MPa, the geometry

with a diameter of 8 mm a gap setting from 2,0 mm is suitable for most instruments. Overlapping of test

results from both geometries is recommended (see 8.5).

For determining complex shear modulus of bituminous binders below 1 kPa, a geometry with a diameter

bigger than 25 mm is recommended. Alternatively, the geometry with a diameter of 25 mm may be used

provided that test results in the expected range of the complex shear modulus are verified with a

calibrated fluid.

Plates of other diameters and other gap settings with different ranges of complex shear modulus may

also be used, ensuring compliance effects of the instrument do not affect the results (see 6.3, Note 1), the

minimum torque specification of the rheometer is respected and the testing is done in the linear

viscoelastic range (see Clause 8).
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NOTE Recent research results demonstrate the suitability of a plate diameter of 4 mm for testing complex

shear modulus in a range 10 MPa to 1 GPa. Depending on the specimen installation procedure, a gap setting between

1,0 mm and 3,0 mm is generally suitable.
6.3 Set up

Set up the rheometer in the sequence given in the manufacturer's instructions, including the procedure

for selecting and setting the correct geometry and gap.

NOTE 1 The selection of system geometry can affect the accuracy of results. The manufacturer can have

determined the operational limits and this information can 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 in this document, irrespective of the geometry chosen,

values of |G*| in excess of 10 Pa are likely to be suspect. Software corrections to the stiffness can be acceptable

provided appropriate validation is supplied by the manufacturer.

The rheometer and temperature control system should be calibrated at regular intervals in accordance

with the quality assurance procedure of the laboratory. The rheometer and temperature control system

should be calibrated by a means traceable to a national standard. Also, it is advisable to verify the

accuracy of the temperature control system by means of a certified temperature-measuring device at

regular intervals. Take 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 2 The temperature in the test specimen can differ from the temperature read by the device if insufficient

equilibration time is used. A procedure for determining equilibration time is described in Annex B.

6.4 Zero Gap Setting

For initialization, the gap between the plates shall be set to zero to give a reference for the gap change for

the thermal expansion of the geometry. Prior to loading the first test specimen, the zero gap is set with

both clean plates at ambient temperature.

NOTE For temperature control systems with minimized thermal gradients within the gap, the zero gap can be

set at any temperature assuring thermal equilibrium of the geometry.

If the DSR has no gap compensation feature, the zero gap can be set at the mid-point of the temperature

range to be tested.
7 Specimen preparation

CAUTION — This document involves handling of apparatus and binders at very high temperatures.

Always wear protective gloves and eyeglasses when handling hot binder, and avoid contact with any

exposed skin.
7.1 General

An informative flow chart for specimen preparation is given in Annex E, Figure E.1.

7.2 Heating procedure for binders prepared above 100 °C

This procedure is applicable for all binders except cut-backs and stabilised binders from emulsions.

Prepare the bituminous binder in accordance with EN 12594.

If the specification grade of the binder is known, the upper softening point limit may be used.

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Avoid prolonged heating of the bulk binder sample, and use the heating periods in EN 12594 as the

maximum time prior to withdrawal of (a) sub-sample(s). For very large bulk samples, it is convenient to

redistribute the binder in smaller bulk samples after heating and careful homogenisation. Place the

sample in the oven maintained at a temperature of (85 ± 5) °C above the expected softening point of the

binder, or at 180 °C, whichever is the lower. For polymer-modified binders, the temperature shall be in

accordance with EN 12594.
Binder samples shall not be reheated more than two times.
Reheating times for sub-samples shall conform to following requirements:
• < 50 g: max 15 min;
• 50 g to 100 g: max 30 min;
• 100 g to 500 g: max 1 h;
• 500 g to 1 kg: max 2 h.
7.3 Heating procedure for binders prepared at temperatures less than 100 °C

This procedure is intended for cut-back binders and stabilised binders from emulsions. Warm the binder

sufficiently and for the minimum time required until it becomes sufficiently fluid either to prepare

smaller bulk samples or to directly prepare moulded test specimens. The binder shall not be heated above

100 °C.

NOTE Normally, warming the binder to its softening point is sufficient. For heavily modified stabilised binders

from emulsions, a temperature closer to 100 °C can be more appropriate. For too viscous samples, a spatula can be

used to remove small quantities at a time from the bulk to place onto the rheometer plate.

Binder samples shall not be reheated more than two times.
7.4 Specimen manufacturing and storage conditions
Moulds or sheet materials may be used for all types of binders.

When the binder reaches temperature after the heating period, stir and mix with a spatula to ensure

homogeneity (especially for polymer modified binders); or after the heating period, remove a sub-sample

of convenient size for handling safely and of sufficient volume, to prepare the required number of test

specimens plus approximately 50 %.

Pour into moulds or directly on to sheets. Care shall be taken to avoid air bubbles in the specimen. Choose

one or more test shapes that will give reliable measurements with the selected test apparatus. The

moulds shall be stored at ambient temperature. If the ambient temperature is higher than 30 °C or the

binder is very soft, specimens may be cooled down for storage, but not below 5 °C. All specimens shall be

covered.

A minimum storage duration before the de-moulding and testing procedure of 30 min shall be maintained

for all bituminous binders. For modified binders that do exhibit phenomena such as crystallization (e.g.

EVA modified binders) the minimum storage duration shall be increased to 12 h. A maximum delay of

two weeks shall not be exceeded for all bituminous binders. The storage time shall be stated in the test

report.
8 Procedure
8.1 General

An informative flow chart for the test procedure is given in Annex E, Figure E.2.

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8.2 Specimen placing onto the rheometer

Carefully prepare the rheometer plates for receipt of the test specimen by cleaning them with a suitable

solvent and soft cleaning cloth or paper. Do not use metal or any other materials, which may damage the

surfaces of the plates, and take care not to bend the shaft of the upper plate.

When using moulds or sheet material, the specimens may be placed in the refrigerator but not below 5 °C

for a maximum time of 30 min prior to de-moulding. De-moulding and loading onto the rheometer should

take place just after removal from the refrigerator.

Specimen installation shall be performed in conditions ensuring satisfactory adhesion of the test

specimen to the rheometer plate, resetting rheologic history of the specimen by allowing sufficient

molecular mobility and ensuring adequate filling of the gap (see 8.3). If the sample flows out of the gap

before reaching gap setting and there is no adequate filling, the installation temperature shall be reduced.

Set the temperature of both plates to the expected softening point of the binder plus 5 °C to 20 °C. The

temperature shall be within a tolerance of ± 1,0 °C for a period of at least 5 min. If the upper plate has no

heating, it can be warmed by contact with lower plate and/or using a water bath. Load the specimen and

set the trimming gap according 8.3.

Alternative temperatures may be used for the temperature for both plates provided that adhesion takes

place between the binder and the plate, and that the binder is sufficiently fluid to allow the gap to be

achieved.
8.3 Gap setting

Values of 1,0 mm for 25 mm plate diameters and 2,0 mm for 8 mm plate diameters are recommended gap

settings.

Bring the test specimen to the selected gap setting plus 0,05 mm for 25 mm plate diameter and plus

0,10 mm for 8 mm plate diameter. The normal force should be monitored during gap setting and reach

the key value of 1,0 N or below to continue the procedure. If the normal force can not be monitored by

the instrument a waiting time of at least 5 min need to be maintained after gap setting. Then trim any

excess binder with a knife, a spatula or a special trimming tool. It has been found helpful to heat the

trimming tool before trimming. After trimming, raise or lower the opposing plate to the set testing gap

(± 0,01 mm). Do not trim at this stage. The entire process of placing and trimming the specimen shall not

take more than 10 min.

For the testing gap to be adequately filled, the test specimen shall cover the whole measuring plate

(indicated by a slight bulging at the periphery of the test specimen). If the testing gap is not adequately

filled, remove, re-prepare the rheometer plates, and prepare a fresh test specimen.

8.4 Temperature and frequency conditions selecting

Set up the rheometer to test in the oscillatory mode to ensure a dynamic response from the specimen

under test.

Select the test temperatures appropriate to the binder being tested. Temperatures should be selected so

that the binder can be adequately characterised with no temperature increment being greater than

(10,0 ± 0,1) °C. Allow the test specimen to equilibrate within the test geometry at each test temperature

before testing (see Annex B). The equilibration time between test temperatures shall be stated in

...