EN 12697-4:2023
(Main)Bituminous mixtures - Test methods - Part 4: Bitumen recovery: Fractionating column
Bituminous mixtures - Test methods - Part 4: Bitumen recovery: Fractionating column
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.
Asphalt - Prüfverfahren - Teil 4: Rückgewinnung des Bindemittels: Fraktionierkolonne
Dieses Dokument legt ein Verfahren fest, mit dem lösliches Bitumen aus Asphalt für Straßen, Flugplätze oder ähnliche Verkehrsflächen in einer Form zurückgewonnen wird, die für weitere Prüfungen geeignet ist.
Das Verfahren ist anwendbar zur Rückgewinnung von Straßenbaubitumen und ist das Referenzverfahren zur Rückgewinnung von löslichem Bitumen aus/von Asphalten, die flüchtige Bestandteile enthalten, wie z. B. Verschnittbitumen.
Das Verfahren ist nicht anwendbar zur Rückgewinnung von polymermodifiziertem Bitumen.
ANMERKUNG EN 12697 3 ist das Referenzverfahren zur Rückgewinnung von Straßenbaubitumen und polymermodifiziertem Bitumen.
Mélanges Bitumineux - Méthodes d’essai - Partie 4 : Extraction des bitumes à la colonne à distiller
Le présent document décrit une méthode permettant de récupérer du bitume soluble à partir de mélanges bitumineux utilisés pour les routes, les aéroports ou des chaussées similaires sous une forme se prêtant à des essais complémentaires.
Cette méthode s’applique à la récupération de bitume routier usuel et constitue la méthode de référence pour la récupération de mélanges bitumineux contenant des matières volatiles comme le bitume fluidifié.
Cette méthode ne s’applique pas à la récupération de bitume modifié par des polymères.
NOTE L’EN 12697-3 constitue la méthode de référence pour la récupération de bitume routier usuel et de bitume modifié par des polymères.
Bitumenske zmesi - Preskusne metode - 4. del: Ponovna pridobitev bitumna: kolonska frakcionirana destilacija
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 12697-4:2023
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
SIST EN 12697-4:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST EN 12697-4:2023
---------------------- Page: 2 ----------------------
SIST EN 12697-4:2023
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.
---------------------- Page: 3 ----------------------
SIST EN 12697-4:2023
EN 12697-4:2023 (E)
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
2
---------------------- Page: 4 ----------------------
SIST EN 12697-4:2023
EN 12697-4:2023 (E)
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.
3
---------------------- Page: 5 ----------------------
SIST EN 12697-4:2023
EN 12697-4:2023 (E)
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.
4
---------------------- Page: 6 ----------------------
SIST EN 12697-4:2023
EN 12697-4:2023 (E)
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
---------------------- Page: 7 ----------------------
SIST EN 12697-4:2023
EN 12697-4:2023 (E)
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 ar
...
SLOVENSKI STANDARD
oSIST prEN 12697-4:2022
01-april-2022
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 : Récupération des bitumes à la
colonne à distiller
Ta slovenski standard je istoveten z: prEN 12697-4
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
oSIST prEN 12697-4:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN 12697-4:2022
---------------------- Page: 2 ----------------------
oSIST prEN 12697-4:2022
DRAFT
EUROPEAN STANDARD
prEN 12697-4
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2022
ICS 93.080.20 Will supersede 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
Récupération des bitumes à la colonne à distiller Bindemittels: Fraktionierkolonne
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 227.
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 12697-4:2022 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 12697-4:2022
prEN 12697-4:2022 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 6
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
Bibliography . 14
2
---------------------- Page: 4 ----------------------
oSIST prEN 12697-4:2022
prEN 12697-7:2022 (E)
European foreword
This document (prEN 12697-4:2022) has been prepared by Technical Committee CEN/TC 227 “Road
materials”, the secretariat of which is held by BSI.
This document is currently submitted to the CEN Enquiry.
This document will supersede 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;
— clarification of the scope. Clause 1;
— correction of dated reference to EN 12697-1. Clause 2;
— deletion of references to EN 12697-3 and EN 12697-38. Clause 2;
— deletion of paragraph describing calibration and maintenance for the centrifuge (5.2.1);
— clarification of the temperature capacity for oil bath (5.3.2);
— the term “accuracy” for thermometer replaced by “maximum permissible error (5.3.5);
— correction of dated reference to EN 12697-1:2020 and paragraph revised for clarity (7.1.2);
— completion of tolerances for temperatures (7.3.5);
— revision of data to be reported. Clause 9.
A list of all parts in the EN 12697 series can be found on the CEN website.
3
---------------------- Page: 5 ----------------------
oSIST prEN 12697-4:2022
prEN 12697-4:2022 (E)
Introduction
WARNING — The method described in this European Standard 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.
4
---------------------- Page: 6 ----------------------
oSIST prEN 12697-4:2022
prEN 12697-7:2022 (E)
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 for bituminous mixtures
containing volatile matter such as cut-back bitumen.
The method is not applicable for recovery of polymer-modified bitumen.
NOTE 1 This document is the reference method for recovery of bituminous mixtures containing volatile matter
such as cut-back bitumen.
NOTE 2 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 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
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 may be followed by binder recovery.
3.2
insoluble binder content
percentage by mass of binder that adheres to the aggregate after extraction
5
---------------------- Page: 7 ----------------------
oSIST prEN 12697-4:2022
prEN 12697-4:2022 (E)
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 cutback 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 might 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.
2
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.