FprEN 12596

Bitumen and bituminous binders - Determination of dynamic viscosity by vacuum capillary

This document specifies a method for the determination of the dynamic viscosity of bituminous binders by means of a vacuum capillary viscometer at 60 °C in a range between 0,003 6 Pa⋅s and 580 000 Pa⋅s. Other temperatures are possible if calibration constants are known. Bituminous emulsions and non-newtonian binders (e.g. some polymer modified bitumen) are not within the scope of this method.
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 identify the hazards and assess the risks involved in performing this test method and to implement sufficient control measures to protect individual operators (and the environment). This includes appropriate safety and health practices and determination of the applicability of regulatory limitations prior to use.

Bitumen und bitumenhaltige Bindemittel - Bestimmung der dynamischen Viskosität mit Vakuum-Kapillaren

Dieses Dokument legt ein Verfahren zur Bestimmung der dynamischen Viskosität von bitumenhaltigen Bindemitteln mit Hilfe eines Vakuum-Kapillar-Viskosimeters bei 60 °C im Bereich von 0,003 6 Pa·s bis 580 000 Pa·s fest. Andere Temperaturen sind möglich, wenn die Kalibrierkonstanten bekannt sind. Dieses Verfahren gilt nicht für Bitumenemulsionen und für nichtnewtonsche Bindemittel (z. B. einige polymermodifizierte Bitumen).
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, die Gefahren zu identifizieren und die mit der Durchführung der Prüfung verbundenen Risiken zu beurteilen sowie geeignete Kontrollmaßnahmen zu implementieren, um den Ausführenden (und die Umwelt) zu schützen. Dies beinhaltet einen angemessenen Arbeits- und Gesundheitsschutz sowie die Klärung vor der Anwendung, ob einschränkende Vorschriften zu berücksichtigen sind.

Bitumes et liants bitumineux - Détermination de la viscosité dynamique par viscosimètre capillaire sous vide

Le présent document prescrit une méthode pour la détermination de la viscosité dynamique de liants bitumineux au moyen d’un viscosimètre capillaire sous vide à 60 °C dans un intervalle de 0,003 6 Pa·s à 580 000 Pa·s. D’autres températures sont possibles si les constantes d’étalonnage sont connues. Le domaine d'application de la présente méthode ne couvre pas les liants non-newtoniens (par exemple certains bitumes modifiés par des polymères) ni les émulsions bitumineuses.

Bitumen in bitumenska veziva - Določanje dinamične viskoznosti z metodo kapilare z vakuumom

General Information

• Status: Not Published
• Publication Date: 21-Sep-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: 5060 - Closure of Vote - Formal Approval
• Start Date: 27-Apr-2023
• Due Date: 20-Jun-2023
• Completion Date: 27-Apr-2023
• Ref Project: kSIST FprEN 12596:2023 - Bitumen and bituminous binders - Determination of dynamic viscosity by vacuum capillary

Relations

• Revises: EN 12596:2014 - Bitumen and bituminous binders - Determination of dynamic viscosity by vacuum capillary
• Effective Date: 15-Jan-2020

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN 12596:2022
01-februar-2022
Bitumen in bitumenska veziva - Določanje dinamične viskoznosti z metodo
kapilare z vakuumom
Bitumen and bituminous binders - Determination of dynamic viscosity by vacuum
capillary

Bitumen und bitumenhaltige Bindemittel - Bestimmung der dynamischen Viskosität mit

Vakuum-Kapillaren

Bitumes et liants bitumineux - Détermination de la viscosité dynamique par viscosimètre

capillaire sous vide
Ta slovenski standard je istoveten z: prEN 12596
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 12596:2022 en,fr,de

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

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oSIST prEN 12596:2022
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oSIST prEN 12596:2022
DRAFT
EUROPEAN STANDARD
prEN 12596
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2021
ICS 75.140; 91.100.50 Will supersede EN 12596:2014
English Version
Bitumen and bituminous binders - Determination of
dynamic viscosity by vacuum capillary

Bitumes et liants bitumineux - Détermination de la Bitumen und bitumenhaltige Bindemittel -

viscosité dynamique par viscosimètre capillaire sous Bestimmung der dynamischen Viskosität mit Vakuum-

vide Kapillaren

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

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 12596:2021 E

worldwide for CEN national Members.
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oSIST prEN 12596:2022
prEN 12596:2021 (E)
Contents Page

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

1 Scope .................................................................................................................................................................. 4

2 Normative references .................................................................................................................................. 4

3 Terms and definitions ................................................................................................................................. 4

4 Principle ........................................................................................................................................................... 5

5 Apparatus ........................................................................................................................................................ 5

6 Preparation of test samples ...................................................................................................................... 7

7 Procedure ........................................................................................................................................................ 7

8 Calculation ....................................................................................................................................................... 8

9 Expression of results ................................................................................................................................... 8

10 Precision .......................................................................................................................................................... 9

10.1 Repeatability .................................................................................................................................................. 9

10.2 Reproducibility .............................................................................................................................................. 9

11 Test report ....................................................................................................................................................... 9

Annex A (normative) Specifications of viscometers ................................................................................... 10

Annex B (informative) Calibration of viscometers ..................................................................................... 16

Annex C (informative) Example for calculation of results ....................................................................... 18

Bibliography .............................................................................................................................................................. 19

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oSIST prEN 12596:2022
prEN 12596:2021 (E)
European foreword

This document (prEN 12596:2021) 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 12596:2014.

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

— amended scope (clarification of applicability of test methods); deletion of notes from scope;

— removal of dated references;
— reference to mercury thermometer has been deleted (5.2);
— reference to total immersion thermometer has been deleted (5.2);
— time to reach thermal equilibrium has been prolonged to 1 hour;

— “bulb” changed into “tube section” in 5.1.2, 5.1.3, Figures A.2 and A.3, and added “tube section” to

Clause 9 (consistency of wording);

— information on validity of individual test data to calculate mean value added in Clause 8;

— appropriate range of flow time readings added in Clause 9;
— Annex C has been deleted;
— new Annex C introduced with examples on calculation;
— ASTM E77-98 deleted from the Bibliography.
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oSIST prEN 12596:2022
prEN 12596:2021 (E)
1 Scope

This document specifies a method for the determination of the dynamic viscosity of bituminous binders

by means of a vacuum capillary viscometer at 60 °C in a range between 0,003 6 Pa⋅s and 580 000 Pa⋅s.

Other temperatures are possible if calibration constants are known. Bituminous emulsions and non-

newtonian binders (e.g. some polymer modified bitumen) are not within the scope of this method.

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 identify the hazards and assess the risks involved in

performing this test method and to implement sufficient control measures to protect individual operators

(and the environment). This includes appropriate safety and health practices and determination of 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 58, Bitumen and bituminous binders - Sampling bituminous binders
EN 12594, Bitumen and bituminous binders - Preparation of test samples

EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987)

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
dynamic viscosity
ratio between the applied shear stress and the velocity gradient

Note 1 to entry: Dynamic viscosity is a measure of the resistance to the flow of a liquid and is commonly called the

viscosity of the liquid. For the purposes of this document, the word viscosity means the dynamic viscosity of a liquid.

Note 2 to entry: The SI unit of dynamic viscosity is Pa⋅s.
3.2
newtonian liquid
liquid with a viscosity that is independent of the rate of shear

Note 1 to entry: The constant ratio of the shear stress to the velocity gradient is the dynamic viscosity of the liquid.

If this ratio is not constant, the liquid is non-newtonian.
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3.3
density
mass of a liquid divided by its volume

Note 1 to entry: When reporting density, the unit of density used, together with the temperature, is stated

explicitly, for example kilogram per cubic metre.
Note 2 to entry: The SI unit of density is kg/m .
3.4
kinematic viscosity

ratio between the dynamic viscosity and the density of a liquid at the temperature of viscosity measured

Note 1 to entry: Kinematic viscosity is a measure of the resistance to flow of a liquid under gravity.

2 2

Note 2 to entry: The Sl unit of kinematic viscosity is m /s; for practical use, a sub-multiple (mm /s) is more

convenient.
4 Principle

To determine the time for a fixed volume of the liquid to be drawn up through a capillary tube by means

of a vacuum, under closely controlled conditions of vacuum and temperature. The viscosity is calculated

by multiplying the flow time in s by the viscometer calibration factor.
5 Apparatus

5.1 Viscometer, capillary-type and made of borosilicate glass as described in 5.1.1 to 5.1.3.

Calibrated viscometers are available from commercial suppliers. Details regarding the calibration of

viscometers are given in Annex B.
5.1.1 Cannon-Manning vacuum capillary viscometer (CMVV).

The CMVV is available in eleven sizes (see Table A.1), covering a range between 0,003 6 Pa⋅s to 8 000 Pa⋅s.

Details of the design and construction of CMVV are shown in Figure A.1. The size numbers, approximate

calibration factors K, and viscosity ranges for the series of CMVV are given in Table A.1.

For all viscometer sizes, the volume of measuring bulb C is approximately three times that of bulb B.

Bulb B, bulb C and bulb D are defined by timing marks F, G and H.
5.1.2 Asphalt Institute vacuum capillary viscometer (AIVV).

The AIVV is available in seven sizes (see Table A.2) from a range between 4,2 Pa⋅s to 580 000 Pa⋅s.

Sizes 50 to 200 are best suited to viscosity measurements of bituminous binders at 60 °C.

Details of design and construction of the AIVV are shown in Figure A.2. The size numbers, approximate

capillary radii, approximate calibration factors K, and viscosity range for the series of AIVV are given in

Table A.2.

This viscometer has measuring tube section B, tube section C and tube section D, located on the

viscometer arm M, which is a precision bore glass capillary. The measuring bulbs/test sections are 20 mm

long capillary segments defined by timing marks F, G, H and I.
5.1.3 Modified Koppers vacuum capillary viscometer (MKVV).

The MKVV is available in five sizes (see Table A.3) covering a range between 4,2 Pa⋅s to 20 000 Pa⋅s.

Sizes 50 to 200 are best suited to viscosity measurements of bituminous binders at 60 °C.

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oSIST prEN 12596:2022
prEN 12596:2021 (E)

Details of design and construction of the MKVV are shown in Figure A.3. The size numbers, approximate

capillary radii, approximate calibration factors K, and viscosity ranges for the series of MKVV are given in

Table A.3.

This viscometer consists of a separate filling tube A, and precision-bore glass capillary vacuum tube M.

These two parts are joined by a borosilicate ground glass joint N, with a 24/40 standard taper. Measuring

tube section B, tube section C and tube section D, on the glass capillary are 20 mm long capillary

segments, defined by timing marks F, G, H and I.

5.1.4 Holder, made by drilling two holes, 22 mm and 8 mm internal diameter, through a No. 11 rubber

stopper. The centre-to-centre distance between holes shall be 25 mm. Slit the rubber stopper between

the holes and between the 8 mm hole and edge of the stopper. When placed in a 51 mm diameter hole in

the bath cover, the stopper shall hold the viscometer in place. For the MKVV the viscometer holder can

be made by drilling a 28 mm hole through the centre of a No. 11 rubber stopper and slitting the stopper

between the hole and the edge.
Such holders are commercially available.
5.2 Temperature measuring device.
A temperature measuring device (combining sensor and reading unit) shall
— have a range from at least 55 °C to 65 °C;
— be readable to 0,05 °C or less;
— have an accuracy of 0,2 °C.

Sensors based on platinum resistance thermometers have been found suitable but other principles are

also allowed. The temperature measuring device shall be calibrated regularly.

When measuring and controlling nominally constant temperatures, as in this test method, the thermal

response time can be rather high (e.g. slow response to a change in temperature). Care shall be taken to

consider this aspect since low thermal response time of the sensor can indicate greater cyclic variations

than the bituminous material in practise experiences.

5.3 Bath, suitable for immersion of the viscometer so that the liquid reservoir or the top of the capillary

whichever is uppermost, is at least 20 mm below the top of the bath level, and with provisions for

visibility of the viscometer and the thermometer. Firm supports for the viscometer shall be provided, or

the viscometer shall be an integral part of the bath. The efficiency of the stirring and the balance between

heat losses and heat input shall be such that the temperature of the bath medium does not vary by more

than 0,5 °C over the length of the viscometer, or from viscometer to viscometer in the various bath

positions.

5.4 Vacuum system, capable of maintaining a vacuum with a reading accuracy of ± 100 Pa of the

desired level up to and including 40 000 Pa. A vacuum or aspirator pump is suitable for the vacuum

source.

5.5 Timer, or stop watch (spring or battery driven) graduated in divisions of 0,1 s or less and accurate

to 0,5 s over 1 000 s when tested over intervals of not le
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