Bituminous mixtures - Test methods - Part 4: Bitumen recovery: Fractionating column

This European Standard specifies a test method for the recovery of soluble bitumen from bituminous mixtures from pavements in a form suitable for further testing. The procedure is suitable for the recovery of paving grade bitumen and is also suitable for mixtures containing volatile matter such as cut-back bitumen but the results may be less precise. This European Standard is the reference method for mixtures containing volatile matter, but the rotary evaporator procedure (see EN 12697-3) for mixtures with paving grade bitumen.
NOTE   There is limited experience of recovery when polymer-modified bitumen is used.

Asphalt - Prüfverfahren - Teil 4: Rückgewinnung des Bindemittels: Fraktionierkolonne

Dieses Dokument legt ein Verfahren zur Rückgewinnung von löslichem Bitumen aus Asphalt für Straßen, Flug
plätze oder ähnliche Beläge in einer zur weiteren Prüfung geeigneten Form fest.
Das Verfahren ist anwendbar zur Rückgewinnung von Straßenbaubitumen und für Asphalte, die flüchtige Bestandteile enthalten, wie z.B. verschnittenes Bitumen.
Das Verfahren ist nicht anwendbar zur Rückgewinnung von polymermodifiziertem Bitumen.
ANMERKUNG1 Dieses Dokument ist das Referenzverfahren zur Rückgewinnung von Asphalten, die flüchtige Bestand
teile enthalten, wie z.B. verschnittenes Bitumen.
ANMERKUNG2 EN12697-3 ist das Referenzverfahren zur Rückgewinnung von Straßenbaubitumen und polymermo
difiziertem 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 terrains d’aviation 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 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 1   Le présent document constitue la méthode de référence pour la récupération de mélanges bitumineux contenant des matières volatiles telles que le bitume fluidifié.
NOTE 2   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

Status
Not Published
Publication Date
11-Jul-2023
Current Stage
5060 - Closure of Vote - Formal Approval
Start Date
02-Feb-2023
Due Date
14-Nov-2023
Completion Date
02-Feb-2023

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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.

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oSIST prEN 12697-4:2022
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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.
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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

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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.
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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.

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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
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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.
...

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