EN 12697-4:2023

SLOVENSKI STANDARD
01-september-2023
Nadomešča:
SIST EN 12697-4:2015
Bitumenske zmesi - Preskusne metode - 4. del: Ponovna pridobitev bitumna:
kolonska frakcionirana destilacija
Bituminous mixtures - Test methods - Part 4: Bitumen recovery: Fractionating column
Asphalt - Prüfverfahren - Teil 4: Rückgewinnung des Bindemittels: Fraktionierkolonne
Mélanges Bitumineux - Méthodes d’essai - Partie 4 : Extraction des bitumes à la colonne
à distiller
Ta slovenski standard je istoveten z: EN 12697-4:2023
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 12697-4
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2023
EUROPÄISCHE NORM
ICS 93.080.20 Supersedes EN 12697-4:2015
English Version
Bituminous mixtures - Test methods - Part 4: Bitumen
recovery: Fractionating column
Mélanges Bitumineux - Méthodes d'essai - Partie 4 : Asphalt - Prüfverfahren - Teil 4: Rückgewinnung des
Extraction des bitumes à la colonne à distiller Bindemittels: Fraktionierkolonne
This European Standard was approved by CEN on 3 March 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 12697-4:2023 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Apparatus . 6
5.1 Apparatus for the extraction of the soluble bitumen . 6
5.2 Apparatus for the clarification of the bitumen solution . 6
5.3 Distillation apparatus . 7
6 Solvent and other materials . 7
7 Procedure. 7
7.1 Extraction of the bitumen and removal of insoluble matter . 7
7.2 Assembling and checking the apparatus for air leaks . 8
7.3 Distillation procedure . 8
8 Preparation of the bitumen for testing . 9
9 Test report . 9
10 Precision . 9
Bibliography . 14

European foreword
This document (EN 12697-4:2023) has been prepared by Technical Committee CEN/TC 227 “Road
materials”, the secretariat of which is held by BSI.
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 October 2023, and conflicting national standards shall
be withdrawn at the latest by October 2023.
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 12697-4:2015.
The main changes compared to the previous edition are listed below:
— general update of standard texts according to CEN/CENELEC Internal Regulations Part 3:2019;
— [Clause 1] clarification of the scope;
— [Clause 2] deletion of “for hot mix asphalt” for EN 12697-1 and correction of dated reference;
— [Clause 2] deletion of reference to EN 12697-3. Added to Bibliography;
— [Clause 2] deletion of reference to EN 12697-38;
— [Clause 5.2.1] deletion of paragraph describing calibration and maintenance for the centrifuge with
reference to EN 12697-38;
— [Clause 5.3.2] clarification of the temperature capacity for oil bath;
— [Clause 5.3.5] the term “accuracy” for thermometer replaced by “maximum permissible error;
— [Clause 7.1.2] correction of dated reference to EN 12697-1:2020;
— [Clause 7.3.5] completion of tolerances for temperatures;
— [Clause 9] revision of data to be reported;
— [Clause 10.1] completion with reference to Table 1 in paragraph;
— [Figure 2] completion with keys for X and Y.
A list of all parts in the EN 12697 series can be found on the CEN website.
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.
Introduction
WARNING — The method described in this document may require the use of dichloromethane
(methylene chloride), 1,1,1 trichlorethane, benzene, trichlorethylene, xylene, toluene or other
solvent capable of dissolving bitumen. These solvents are hazardous to health and are subject to
occupational exposure limits as detailed in relevant legislation and regulations.
Exposure levels are related to both handling procedures and ventilation provision and it is emphasized
that adequate training should be given to staff employed in the usage of these substances.
1 Scope
This document specifies a method for the recovery of soluble bitumen from bituminous mixtures used in
road, airfield or similar pavements in a form suitable for further testing.
The method is applicable for the recovery of paving grade bitumen and is the reference method for
recovery of soluble bitumen from bituminous mixtures containing volatile matter such as cut-back
bitumen.
The method is not applicable for recovery of polymer-modified bitumen.
NOTE EN 12697-3 is the reference method for the recovery of paving grade bitumen and polymer-modified
bitumen.
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
EN 12697-1:2020, Bituminous mixtures - Test methods - Part 1: Soluble binder content
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
soluble binder content
percentage by mass of extractable binder in an anhydrous sample determined by extracting the binder
from the sample
Note 1 to entry: Extraction can be followed by binder recovery.
3.2
insoluble binder content
percentage by mass of binder that adheres to the aggregate after extraction
4 Principle
The bitumen is separated from the sample by dissolving in dichloromethane (or other suitable solvent).
After removal of undissolved solids, the bitumen solution is concentrated by atmospheric distillation in
a fractionating column. The last traces of solvent are removed from the concentrate by distillation at a
temperature of 100 °C above the expected softening point or 175 °C, whichever is the higher, with the
pressure reduced from atmospheric pressure 100 kPa to 20 kPa and with the aid of a stream of carbon
dioxide gas. When cut-back bitumens containing very volatile fluxes, e.g. white spirit, are being recovered
the carbon dioxide gas is omitted.
5 Apparatus
5.1 Apparatus for the extraction of the soluble bitumen
Suitable container with stopper, in which the sample and solvent can be agitated together, or other
apparatus for the extraction of soluble bitumen defined in EN 12697-1.
NOTE The use of the hot extraction methods in EN 12697-1 can harden the binder and hence affect the results
from subsequent tests. However, this hardening is usually regarded as approximately balancing the softening
resulting from any remaining solvent.
5.2 Apparatus for the clarification of the bitumen solution
For separation of solids from the bitumen solution, a sample-tube centrifuge, a continuous centrifuge or
a filtration system may be used.
Centrifuges are suitable for separation of solids from any bitumen solutions and are the recommended
apparatus for use with this method. The filtration apparatus may not be suitable for the separation of
solids from all types of bituminous solutions but it has been included in this method because of the
general availability of this equipment in asphalt testing laboratories. If difficulties are experienced using
a pressure filter the centrifuge technique should be used.
5.2.1 Sample tube centrifuge, capable of developing an acceleration of at least 15 000 m/s in
accordance with the following formula:
2 −6
a = 1,097× n × r × 10 (1)
where
a is the acceleration, expressed in metres per second squared (m/s );
n is the number of revolutions, expressed in revolutions per minute (r/min);
r is the radius to the bottom of the tubes (internal) when rotating, expressed in millimetres
(mm).
The centrifuge tubes shall be fitted with effective closures.
NOTE A typical centrifuge of this type, suitable for this method, carries four or six tubes of 200 ml or 500 ml
capacity rotating at 3 000 r/min at a radius (as defined above) of 250 mm.
5.2.2 Continuous laboratory centrifuge, that takes a continuous feed of material, giving a continuous
discharge of solution and capable of achieving an acceleration of 25 000 m/s .
5.2.3 A pressure filter, of an appropriate size.
5.2.4 An air pump, for supplying oil-free air at about 200 kPa.
5.2.5 A supply of filter papers with a minimum retention size of 11 µm, to fit the pressure filter.
NOTE A pressure filter taking a paper of 270 mm diameter is suitable.
5.3 Distillation apparatus
See Figure 1.
5.3.1 500 ml round-bottomed flask of heat resisting glass fitted with a three-necked glass
adaptor.
The central neck is used either to accommodate a stirrer (see Figures 2 or 3) or a glass tube from 4 mm
to 6 mm internal diameter for sweeping carbon dioxide through the flask when required. A 250 ml
stoppered separating funnel is fitted to one side neck of the multiple adapter. The other side neck is
connected to the fractionating column followed by an efficient water-cooled glass condenser and receiver
system. The fractionating column is of the Dufton type or Vigreux type having an effective length from
300 mm to 400 mm and may be vacuum jacketed. The receiver system includes a tap by which the main
receiver can be isolated from
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