EN 12596:2023

SLOVENSKI STANDARD
01-november-2023
Nadomešča:
SIST EN 12596:2014
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: EN 12596:2023
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.

EN 12596
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2023
EUROPÄISCHE NORM
ICS 75.140; 91.100.50 Supersedes 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 European Standard was approved by CEN on 28 May 2023.

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 CEN-CENELEC 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 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, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12596:2023 E
worldwide for CEN national Members.

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 test samples . 8
7 Procedure . 8
8 Calculation . 9
9 Expression of results . 10
10 Precision . 10
10.1 Repeatability . 10
10.2 Reproducibility . 10
11 Test report . 10
Annex A (normative) Specifications of viscometers . 11
Annex B (informative) Calibration of viscometers . 17
Annex C (informative) Example for calculation of results . 19
Bibliography . 20
European foreword
This document (EN 12596:2023) 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 January 2024, and conflicting national standards shall
be withdrawn at the latest by January 2024.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 12596:2014.
In comparison with the previous edition, the main technical changes are:
— amended scope (clarification of applicability of test methods); deletion of notes from scope;
— “accuracy” is changed to “maximum permissible error” in several clauses (5.2, 5.4, 5.5 and 5.6);
— reference to mercury thermometer deleted (5.2);
— reference to total immersion thermometer deleted (5.2);
— maximum permissible error for temperature of bath changed from 0,5 °C to 0,3 °C (5.3);
— the required precision of the oven reduced to (135 ± 5) °C in (5.7, 7.2, 7.4 and 7.5);
— time to reach thermal equilibrium 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);
— new subclause 5.8 added on Calibration/Verification;
— information on validity of individual test data to calculate mean value added in Clause 8; including a
new NOTE 2 and renumbering existing notes respectively;
— appropriate range of flow time readings added in Clause 9;
— Table B.1 updated with informative values for viscosity standards;
— all time measurements with a maximum permissible error of 0,1 s in B.3.1;
— Annex C deleted;
— new Annex C introduced with examples on calculation;
— ASTM E77-98 deleted from the Bibliography;
— reference to ASTM D2171-01 in Bibliography updated and reference (footnote) to Institute of
Petroleum deleted.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the United
Kingdom.
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 terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
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.
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 kg/m .
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 SI 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 seconds 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.
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 a maximum permissible error 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 0,3 °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 maximum permissible error 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
...