SIST EN 12697-1:2020
(Main)Bituminous mixtures - Test methods - Part 1: Soluble binder content
Bituminous mixtures - Test methods - Part 1: Soluble binder content
This document describes test methods for the determination of the soluble binder content of samples of bituminous mixtures.
The test methods described are suitable for quality control purposes during the production of plant mix and for checking compliance with a product specification.
For the analysis of mixtures containing modified binders, the guidance of Annex D should be followed.
Asphalt - Prüfverfahren - Teil 1: Löslicher Bindemittelgehalt
Dieses Dokument beschreibt Prüfverfahren zur Bestimmung des löslichen Bindemittelgehaltes in Proben aus Asphalt.
Die beschriebenen Prüfverfahren sind zur Qualitätskontrolle während der Herstellung des Mischgutes sowie zur Überprüfung der Übereinstimmung mit einer Produktspezifikation geeignet.
Zur Untersuchung von Gemischen, welche modifizierte Bindemittel enthalten, sollten die Hinweise in Anhang D beachtet werden.
Mélanges bitumineux - Méthodes d'essai - Partie 1 : Teneur en liant soluble
Le présent document décrit des méthodes d’essai pour déterminer la teneur en liant soluble d’échantillons de matériaux enrobés.
Les méthodes d’essai décrites sont applicables pour la maîtrise de la qualité de production en usine et pour les vérifications de conformité aux spécifications des produits.
Pour l'analyse des mélanges contenant des liants modifiés, il convient de suivre les recommandations données en Annexe D.
Bitumenske zmesi - Preskusne metode - 1. del: Topni delež veziva
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 12697-1:2020
01-maj-2020
Nadomešča:
SIST EN 12697-1:2012
Bitumenske zmesi - Preskusne metode - 1. del: Topni delež veziva
Bituminous mixtures - Test methods - Part 1: Soluble binder content
Asphalt - Prüfverfahren - Teil 1: Löslicher Bindemittelgehalt
Mélanges bitumineux - Méthodes d'essai - Partie 1 : Teneur en liant soluble
Ta slovenski standard je istoveten z: EN 12697-1:2020
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
SIST EN 12697-1:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 12697-1:2020
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SIST EN 12697-1:2020
EN 12697-1
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2020
EUROPÄISCHE NORM
ICS 93.080.20 Supersedes EN 12697-1:2012
English Version
Bituminous mixtures - Test methods - Part 1: Soluble
binder content
Mélanges bitumineux - Méthodes d'essai - Partie 1 : Asphalt - Prüfverfahren - Teil 1: Löslicher
Teneur en liant soluble Bindemittelgehalt
This European Standard was approved by CEN on 18 November 2019.
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, Turkey 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
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12697-1:2020 E
worldwide for CEN national Members.
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SIST EN 12697-1:2020
EN 12697-1:2020 (E)
Contents Page
European foreword . 5
Introduction . 7
1 Scope . 8
2 Normative references . 8
3 Terms and definitions . 8
4 Preparation of laboratory samples . 10
5 Determination of binder content . 10
5.1 General principles of test . 10
5.2 Binder extraction . 10
5.2.1 Solvent . 10
5.2.2 Apparatus . 11
5.2.3 Procedure. 11
5.3 Separation of mineral matter . 11
5.3.1 Apparatus . 11
5.3.2 Procedure. 11
5.4 Binder quantity . 12
5.4.1 Apparatus . 12
5.4.2 Procedure. 12
5.5 Calculation and expression of results . 12
5.5.1 General . 12
5.5.2 Binder content determined by difference . 12
5.5.3 Binder content by total recovery . 12
5.5.4 Binder content by recovery from portion (volume calculation) . 13
5.5.5 Binder content by recovery from portion (mass calculation) . 13
6 Drying to constant mass . 14
6.1 General . 14
6.2 Apparatus . 14
6.3 Procedure. 14
7 Reporting of results . 14
7.1 Results . 14
7.2 Test report . 15
8 Precision data . 15
8.1 General . 15
8.2 Precision — Experiment 1 . 15
8.3 Precision — Experiment 2 . 16
8.4 Precision — Experiment 3 . 17
8.5 Precision — Experiment 4 . 17
8.6 Precision — Experiment 5 . 17
Annex A (informative) Guidance on the determination of binder content . 18
A.1 Evaluation of the results . 18
A.2 Effect of water content . 19
A.3 Choice of test equipment and the sequence of operations . 19
2
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A.4 Determination of total binder content . 19
Annex B (normative) Use of equipment for the determination of binder content . 21
B.1 Binder extraction . 21
B.1.1 Hot extractor (paper filter) method . 21
B.1.2 Hot extractor (wire mesh filter) method . 26
B.1.3 Soxhlet extractor method . 27
B.1.4 Bottle rotation machine method . 29
B.1.5 Centrifuge extractor method . 32
B.1.6 Cold mix dissolution of bitumen by agitation . 34
B.1.7 Automatic extractor method . 35
B.2 Separation of mineral matter . 36
B.2.1 Continuous flow centrifuge . 36
B.2.2 Pressure filter . 38
B.2.3 Bucket type centrifuge — Type 1 . 39
B.2.4 Bucket type centrifuge — Type 2 . 41
B.3 Soluble binder content . 41
B.3.1 Method by recovery from a portion using a volume calculation . 41
B.3.2 Method by recovery from a portion using a mass calculation. 44
Annex C (normative) Determination of residual mineral matter in the binder extract by
incineration . 45
C.1 General . 45
C.2 Method 1 . 45
C.2.1 Apparatus . 45
C.2.2 Reagent . 45
C.2.3 Procedure . 45
C.3 Method 2 . 46
C.3.1 Apparatus . 46
C.3.2 Procedure . 46
Annex D (informative) Guidance on determination of soluble binder content of mixtures
with polymer-modified binders . 48
D.1 General . 48
D.2 Preparatory treatment of laboratory samples of bituminous mixtures . 48
D.3 Determination of binder content . 48
D.3.1 General principles of test . 48
D.3.2 Binder extraction . 48
D.3.3 Separation of mineral matter . 50
D.3.4 Binder quantity . 51
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EN 12697-1:2020 (E)
D.3.5 Calculation and expression of results . 51
D.4 Drying to constant mass . 51
D.5 Reporting of results . 51
D.6 Precision data . 51
Bibliography . 52
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EN 12697-1:2020 (E)
European foreword
This document (EN 12697-1:2020) 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 September 2020, and conflicting national standards
shall be withdrawn at the latest by September 2020.
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 12697-1:2012.
The following is a list of significant technical changes since the previous edition:
— the title no longer makes the method exclusively for hot mix asphalt;
— [ge] editorial update according to current standard template;
— [ge] NOTES modified or adjusted to normal text where appropriate according to ISO/IEC Directives
– Part 2:2016, 24.5;
— [ge] the wording “accuracy of” has been altered to “to the nearest” in relevant procedures;
3 3 3 3
— [ge] The unit mm x 10 mm corrected to cm ;
— [Clause 2 and 5.3.2.4] EN 933-1 replaced by EN 12697-2;
— [Clause 4] Title amended to read: Preparation of laboratory samples. Completed with description
for mixtures with high mineral matter content;
— [5.2.2.1], [6.2.2] and [B.1.7.1.6] accuracy for balance of 0,05 % amended to ± 0,1 g;
— [5.2.3.1] clause deleted (superfluous). Following clauses renumbered accordingly;
— [5.5.2 to 5.5.5] Titles amended for clarification;
— [6.1] completed with observation about influence of water for the result of binder content;
— [8.2.2 and 8.2.3] dated reference deleted for EN 12697-28:2000;
— [8.6] new clause about precision of automatic devices:
— [Figure A.1] new figure introduced. Completed with Automatic extractor method. Minor editorial
corrections;
— [B.1.5.1.5] table with dimensions related to Figure B.7 has been corrected in accordance with
figure;
— [B.1.7] procedure for automatic extractor method included;
2
— [B.2.1.1.1] acceleration amended to 25 000 m/s for consistency with EN 12697-3;
5
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EN 12697-1:2020 (E)
— [C.2.1.1.1] accuracy of balance amended to read ± 1 mg;
3
— [C.2.1.5] capacity of ignitions dishes clarified: Ignition dish, of at least 125 cm capacity;
— [C.3.1.1] accuracy of balance, amended to read ± 10 mg;
— [Bibliography] updated.
A list of all parts in the EN 12697 series can be found on the CEN website
WARNING — The method described in this document may require the use of dichloromethane
(methylene chloride), 1,1,1-trichloroethane, benzene, trichloroethylene, xylene, toluene,
perchloroethylene (tetracloroethylene) or other solvents 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.
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, Turkey and the
United Kingdom.
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EN 12697-1:2020 (E)
Introduction
This document describes a unified approach to the examination of bituminous mixtures that allows
some divergence in the detail of procedures followed by individual laboratories. In Clause 5 of this
document, a description is given of the basic operations that together form the test method for the
proper determination of the binder content of bituminous mixtures. Guidance on the test method is
given in Annex A and Figure A.1, while the use of alternative items of equipment that are equally
suitable for carrying out particular parts of the test method are described in Annex B. Although the
apparatus specified for the separation of mineral filler from the binder solution obtained after
extraction is of a suitably efficient level not to affect the precision of the test described in Clause 8, a
method for determining the amount of residual mineral matter in the extract is given in Annex C for use
in those particular cases where some doubt may exist.
Methods and equipment other than those described in Annex B and Annex C, including automated
equipment, are permissible provided that they have been demonstrated to provide the same results as
one of the methods in Annex B or Annex C within the limits of the precision given in this document.
Guidance on determination of soluble binder content of mixtures with polymer-modified binders is
given in Annex D.
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EN 12697-1:2020 (E)
1 Scope
This document describes test methods for the determination of the soluble binder content of samples of
bituminous mixtures.
The test methods described are suitable for quality control purposes during the production of plant mix
and for checking compliance with a product specification.
For the analysis of mixtures containing modified binders, the guidance of Annex D should be followed.
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 12697-2, Bituminous mixtures — Test methods — Part 2: Determination of particle size distribution
EN 12697-3, Bituminous mixtures — Test methods — Part 3: Bitumen recovery: Rotary evaporator
EN 12697-4, Bituminous mixtures — Test methods — Part 4: Bitumen recovery: Fractionating column
EN 12697-14, Bituminous mixtures — Test methods — Part 14: Water content
EN 12697-28, Bituminous mixtures — Test methods — Part 28: Preparation of samples for determining
binder content, water content and grading
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
ISO 3310-2, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated metal
plate
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 http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/ui
3.1
soluble binder content
percentage by mass of extractable binder in an anhydrous sample, determined by extracting the binder
from the sample
3.2
insoluble binder content
percentage by mass of binder that adheres to the aggregate particles after extraction
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3.3
precision
closeness of agreement between independent test results obtained under stipulated conditions
Note 1 to entry: Precision depends only on the distribution of random errors and does not relate to the true
value or the specified value.
Note 2 to entry: The measure of precision is usually expressed in terms of imprecision and computed as a
standard deviation of the test results. Less precision is indicated by a larger standard deviation.
Note 3 to entry: “Independent test results” means results obtained in a manner not influenced by any previous
result on the same or similar test sample. Quantitative measures of precision depend critically on the stipulated
conditions. Repeatability and reproducibility conditions are particular sets of extreme conditions.
3.4
repeatability
precision under repeatability conditions
3.5
repeatability conditions
conditions in which independent test results are obtained with the same method on identical test items
in the same laboratory by the same operator using the same equipment within short intervals of time
3.6
repeatability limit
maximum absolute difference between two test results obtained under repeatability conditions that
may be expected with a probability of 95 %
Note 1 to entry: The symbol used for repeatability limit is r.
3.7
reproducibility
precision under reproducibility conditions
3.8
reproducibility conditions
conditions in which test results are obtained with the same method on identical test items in different
laboratories with different operators using different equipment
3.9
reproducibility limit
maximum absolute difference between two test results obtained under reproducibility conditions that
may be expected with a probability of 95 %
Note 1 to entry: The symbol used for reproducibility limit is R.
3.10
single test result
value obtained by applying the standard test method once, fully, on a single specimen
Note 1 to entry: The single test result can also be the mean of two or more observations or the result of a
calculation from a set of observations as specified by the standard test method.
9
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EN 12697-1:2020 (E)
4 Preparation of laboratory samples
Prepare laboratory samples in accordance with EN 12697-28 to obtain suitable test portions.
In the case of bituminous mixtures with high mineral matter content, take into account the capacity of
the apparatus described in B.2 to determine the mass of the material.
5 Determination of binder content
5.1 General principles of test
The test method for determining the binder content of a test portion of bituminous mixture, prepared in
accordance with Clause 4, normally comprises the following basic operations:
a) binder extraction by dissolving in a hot or cold solvent;
b) separation of mineral matter from the binder solution;
c) determination of binder quantity by difference or binder recovery;
d) calculation of soluble binder content.
NOTE 1 The sequence of operations and choice of test procedures to be followed are illustrated in Figure A.1.
If it is suspected that water is present in the laboratory sample, the sample should either be dried to
constant mass (see Clause 6), or the water content determined by the method described in EN 12697-
14, or the sample treated as in EN 12697-28.
NOTE 2 All test procedures and associated equipment relating to each basic operation shown in Figure A.1 are
equally acceptable. Other equipment and procedures, including non-extraction methods, can also be used. There
are documented data to show that the method and equipment will provide results with an accuracy and a
precision no worse than that of one of the procedures explicitly shown in Figure A.1.
5.2 Binder extraction
5.2.1 Solvent
The tests in this document require the use of solvents capable of dissolving bitumen and in some cases
involve distilling the solution to recover all or some of the bitumen.
NOTE Currently all hydrocarbon solvents are regarded as “hazardous” and “environmentally unfriendly” to
varying degrees.
Until such time as there is an agreed CEN policy with regard to the usage of hydrocarbon solvents, each
member state should specify its preferred solvent, taking into account the Montreal Protocol and the
views of its own Regulatory Bodies (see also “Warning” in the Foreword).
Trichloroethylene should be stored in sealed bottles or canisters, which are protected against UV
radiation.
When trichloroethylene is recovered by distillation for further use, care should be taken to ensure that
the solvent still complies with the appropriate requirements. In particular, acidity may develop; a useful
precaution is to store the solvent over calcium oxide in coloured glass or suitable metal containers.
10
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EN 12697-1:2020 (E)
5.2.2 Apparatus
The apparatus should be calibrated and traceable.
5.2.2.1 Balance, capable of weighing a test portion to an accuracy of ± 0,1 g.
5.2.2.2 Binder extraction apparatus, conforming to the requirements of the method selected from
B.1, as appropriate.
5.2.3 Procedure
5.2.3.1 Weigh the test portion to the nearest 0,1 g, and place it in the binder extraction apparatus in
accordance with the requirements of the method selected from B.1, as appropriate.
5.2.3.2 The binder extraction procedure shall ensure that no soluble binder is left adhering to the
aggregate particles after extraction.
NOTE In limited cases, it can be difficult to dissolve every trace of binder adhering to the aggregate (see A.4).
5.3 Separation of mineral matter
5.3.1 Apparatus
5.3.1.1 Trays, that can be heated without damage or change in mass and which are used to dry
recovered aggregate.
5.3.1.2 Apparatus for the separation of mineral filler from the binder solution, conforming to
the requirements of the method selected from B.2, as appropriate.
5.3.2 Procedure
5.3.2.1 Collect the binder solution obtained in accordance with 5.2 and proceed in accordance with
the method selected from B.2, as appropriate.
5.3.2.2 The procedure used to separate the mineral filler from the binder solution shall ensure that
the residue on ignition of the recovered binder does not exceed 0,5 %, i
...
SLOVENSKI STANDARD
oSIST prEN 12697-1:2019
01-februar-2019
Bitumenske zmesi - Preskusne metode - 1. del: Topni delež veziva
Bituminous mixtures - Test methods - Part 1: Soluble binder content
Asphalt - Prüfverfahren - Teil 1: Löslicher Bindemittelgehalt
Mélanges bitumineux - Méthodes d'essai - Partie 1 : Teneur en bitume
Ta slovenski standard je istoveten z: prEN 12697-1
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
oSIST prEN 12697-1:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 12697-1:2019
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oSIST prEN 12697-1:2019
DRAFT
EUROPEAN STANDARD
prEN 12697-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2018
ICS 93.080.20 Will supersede EN 12697-1:2012
English Version
Bituminous mixtures - Test methods - Part 1: Soluble
binder content
Mélanges bitumineux - Méthodes d'essai - Partie 1 : Asphalt - Prüfverfahren - Teil 1: Löslicher
Teneur en bitume Bindemittelgehalt
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, 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
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 12697-1:2018 E
worldwide for CEN national Members.
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oSIST prEN 12697-1:2019
prEN 12697-1:2018 (E)
Contents
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Preparatory treatment of laboratory samples of bituminous mixtures . 8
5 Determination of binder content . 8
5.1 General principles of test . 8
5.2 Binder extraction . 8
5.3 Separation of mineral matter . 9
5.4 Binder quantity . 10
5.5 Calculation and expression of results . 10
6 Drying to constant mass . 12
6.1 General . 12
6.2 Apparatus . 12
6.3 Procedure. 12
7 Reporting of results . 12
7.1 Results . 12
7.2 Test report . 12
8 Precision data . 13
8.1 General . 13
8.2 Precision — Experiment 1 . 13
8.3 Precision — Experiment 2 . 14
8.4 Precision — Experiment 3 . 14
8.5 Precision — Experiment 4 . 15
Annex A (informative) Guidance on the determination of binder content . 16
A.1 Evaluation of the results . 16
A.2 Effect of water content . 17
A.3 Choice of test equipment and the sequence of operations . 17
A.4 Determination of total binder content . 17
Annex B (normative) Use of equipment for the determination of binder content . 19
B.1 Binder extraction . 19
B.1.1 Hot extractor (paper filter) method . 19
B.1.2 Hot extractor (wire mesh filter) method . 24
B.1.3 Soxhlet extractor method . 25
B.1.4 Bottle rotation machine method . 27
B.1.5 Centrifuge extractor method . 29
B.1.6 Cold mix dissolution of bitumen by agitation . 32
B.2 Separation of mineral matter . 32
B.2.1 Continuous flow centrifuge . 32
2
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B.2.2 Pressure filter . 34
B.2.3 Bucket type centrifuge — Type 1 . 35
B.2.4 Bucket type centrifuge — Type 2 . 37
B.3 Soluble binder content . 37
B.3.1 Method by recovery from a portion using a volume calculation . 37
B.3.2 Method by recovery from a portion using a mass calculation. 40
Annex C (normative) Determination of residual mineral matter in the binder extract by
incineration . 41
C.1 General . 41
C.2 Method 1 . 41
C.2.1 Apparatus . 41
C.2.2 Reagent . 41
C.2.3 Procedure . 41
C.3 Method 2 . 42
C.3.1 Apparatus . 42
C.3.2 Procedure . 42
Annex D (informative) Guidance on determination of soluble binder content of mixtures
with polymer-modified binders . 44
D.1 General . 44
D.2 Preparatory treatment of laboratory samples of bituminous mixtures . 44
D.3 Determination of binder content . 44
D.3.1 General principles of test . 44
D.3.2 Binder extraction . 44
D.3.3 Separation of mineral matter . 46
D.3.4 Binder quantity . 47
D.3.5 Calculation and expression of results . 47
D.4 Drying to constant mass . 47
D.5 Reporting of results . 47
D.6 Precision data . 47
Bibliography . 48
3
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oSIST prEN 12697-1:2019
prEN 12697-1:2018 (E)
European foreword
This document (prEN 12697-1:2018) 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 enquiry.
This document will supersede EN 12697-1:2012.
The following is a list of significant technical changes since the previous edition:
— the title no longer makes the method exclusively for hot mix asphalt;
— [ge] editorial update according to current standard template;
2
— [B.2.1.1.1] Acceleration amended to 25000 m/s for consistency with EN 12697-3;
3 3 3
— [C.2.1.5] Capacity of ignitions dishes clarified: Ignition dish, of at least 125 mm × 10 mm
capacity ;
A list of all parts in the EN 12697 series can be found on the CEN website
WARNING — The method described in this European Standard may require the use of dichloromethane
(methylene chloride), 1,1,1-trichloroethane, benzene, trichloroethylene, xylene, toluene,
perchloroethylene (tetracloroethylene) or other solvents 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
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oSIST prEN 12697-1:2019
prEN 12697-1:2018 (E)
Introduction
This European Standard describes a unified approach to the examination of bituminous mixtures that
allows some divergence in the detail of procedures followed by individual laboratories. In Clause 5 of
this European Standard, a description is given of the basic operations that together form the test
method for the proper determination of the binder content of bituminous mixtures. Guidance on the
test method is given in Annex A and Figure A.1, while the use of alternative items of equipment that are
equally suitable for carrying out particular parts of the test method are described in Annex B. Although
the apparatus specified for the separation of mineral filler from the binder solution obtained after
extraction is of a suitably efficient level not to affect the precision of the test described in Clause 8, a
method for determining the amount of residual mineral matter in the extract is given in Annex C for use
in those particular cases where some doubt may exist.
Methods and equipment other than those described in Annex B and Annex C, including automated
equipment, are permissible provided that they have been demonstrated to provide the same results as
one of the methods in Annex B or Annex C within the limits of the precision given in this document.
Guidance on determination of soluble binder content of mixtures with polymer-modified binders is
given in Annex D.
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1 Scope
This document describes test methods for the determination of the soluble binder content of samples of
bituminous mixtures.
The test methods described are suitable for quality control purposes during the production of plant mix
and for checking compliance with a product specification.
For the analysis of mixtures containing modified binders, the guidance of Annex D should be followed.
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 12697-3, Bituminous mixtures - Test methods for hot mix asphalt - Part 3: Bitumen recovery: Rotary
evaporator
EN 12697-4, Bituminous mixtures - Test methods - Part 4: Bitumen recovery: Fractionating column
EN 12697-14, Bituminous mixtures - Test methods for hot mix asphalt - Part 14: Water content
EN 12697-28, Bituminous mixtures - Test methods for hot mix asphalt - Part 28: Preparation of samples
for determining binder content, water content and grading
EN 933-1, Tests for geometrical properties of aggregates - Part 1: Determination of particle size
distribution - Sieving method
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
ISO 3310-2, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated metal
plate
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 http://www.electropedia.org/
• ISO Online browsing platform: available at http://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 particles after extraction
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3.3
precision
closeness of agreement between independent test results obtained under stipulated conditions
Note 1 to entry: Precision depends only on the distribution of random errors and does not relate to the true
value or the specified value.
Note 2 to entry: The measure of precision is usually expressed in terms of imprecision and computed as a
standard deviation of the test results. Less precision is indicated by a larger standard deviation.
Note 3 to entry: “Independent test results” means results obtained in a manner not influenced by any previous
result on the same or similar test sample. Quantitative measures of precision depend critically on the stipulated
conditions. Repeatability and reproducibility conditions are particular sets of extreme conditions.
3.4
repeatability
precision under repeatability conditions
3.5
repeatability conditions
conditions in which independent test results are obtained with the same method on identical test items
in the same laboratory by the same operator using the same equipment within short intervals of time
3.6
repeatability limit
maximum absolute difference between two test results obtained under repeatability conditions that
may be expected with a probability of 95 %
Note 1 to entry: The symbol used for repeatability limit is r.
3.7
reproducibility
precision under reproducibility conditions
3.8
reproducibility conditions
conditions in which test results are obtained with the same method on identical test items in different
laboratories with different operators using different equipment
3.9
reproducibility limit
maximum absolute difference between two test results obtained under re…bility conditions that may be
expected with a probability of 95 %
Note 1 to entry: The symbol used for reproducibility limit is R.
3.10
single test result
value obtained by applying the standard test method once, fully, on a single specimen
Note 1 to entry: The single test result may also be the mean of two or more observations or the result of a
calculation from a set of observations as specified by the standard test method.
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4 Preparatory treatment of laboratory samples of bituminous mixtures
Prepare laboratory samples in accordance with EN 12697-28 to obtain suitable test portions.
5 Determination of binder content
5.1 General principles of test
The test method for determining the binder content of a test portion of bituminous mixture, prepared in
accordance with Clause 4, normally comprises the following basic operations:
a) binder extraction by dissolving in a hot or cold solvent;
b) separation of mineral matter from the binder solution;
c) determination of binder quantity by difference or binder recovery;
d) calculation of soluble binder content.
NOTE 1 The sequence of operations and choice of test procedures to be followed are illustrated in Figure A.1.
If it is suspected that water is present in the laboratory sample, the sample should either be dried to
constant mass (see Clause 6), or the water content determined by the method described in
EN 12697-14, or the sample treated as in EN 12697-28.
NOTE 2 All test procedures and associated equipment relating to each basic operation shown in Figure A.1 are
equally acceptable. Other equipment and procedures, including non-extraction methods, may also be used. There
are documented data to show that the method and equipment will provide results with an accuracy and a
precision no worse than that of one of the procedures explicitly shown in Figure A.1.
5.2 Binder extraction
5.2.1 Solvent
The tests in this European Standard require the use of solvents capable of dissolving bitumen and in
some cases involve distilling the solution to recover all or some of the bitumen.
NOTE Currently all hydrocarbon solvents are regarded as “hazardous” and “environmentally unfriendly” to
varying degrees.
Until such time as there is an agreed CEN policy with regard to the usage of hydrocarbon solvents, each
member state should specify its preferred solvent, taking into account the Montreal Protocol and the
views of its own Regulatory Bodies (see also “Warning” in the Foreword).
Trichloroethylene should be stored in sealed bottles or canisters, which are protected against UV
radiation.
When trichloroethylene is recovered by distillation for further use, care should be taken to ensure that
the solvent still complies with the appropriate requirements. In particular, acidity may develop; a useful
precaution is to store the solvent over calcium oxide in coloured glass or suitable metal containers.
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5.2.2 Apparatus
The apparatus should be calibrated and traceable.
5.2.2.1 Balance, capable of weighing a test portion to an accuracy of 0,05 % of its mass.
5.2.2.2 Binder extraction apparatus, conforming to the requirements of the method selected from
B.1, as appropriate.
5.2.3 Procedure
5.2.3.1 Prepare laboratory samples in accordance with EN 12697-28 to obtain suitable test
portions.
NOTE If determining binder content by difference, see Annex A.
5.2.3.2 Weigh the test portion to the nearest 0,05 % of the mass taken, and place it in the binder
extraction apparatus in accordance with the requirements of the method selected from B.1, as
appropriate.
5.2.3.3 The binder extraction procedure shall ensure that no soluble binder is left adhering to the
aggregate particles after extraction.
NOTE In limited cases, it may be difficult to dissolve every trace of binder adhering to the aggregate (see A.4).
5.3 Separation of mineral matter
5.3.1 Apparatus
5.3.1.1 Trays, that can be heated without damage or change in mass and which are used to dry
recovered aggregate.
5.3.1.2 Apparatus for the separation of mineral filler from the binder solution, conforming to
the requirements of the method selected from B.2, as appropriate.
5.3.2 Procedure
5.3.2.1 Collect the binder solution obtained in accordance with 5.2 and proceed in accordance with
the method selected from B.2, as appropriate.
5.3.2.2 The procedure used to separate the mineral filler from the binder solution shall ensure that
the residue on ignition of the recovered binder does not exceed 0,5 %, if the nominal filler content is
less than 6 % of the mass of aggregate, or 1 % if the nominal filler content is 6 % or greater, when
determined in accordance with Annex C.
NOTE 1 This check is not necessary for all samples but rather serves to prove the effectiveness of the method.
NOTE 2 The residue depends on the solvent and the equipment used.
5.3.2.3 Transfer, where necessary, the clean recovered aggregate to a tray. Evaporate the solvent
from the aggregate and the binder extraction apparatus. Transfer any remaining fine mineral matter
from the binder extraction apparatus to the tray with the rest of the recovered aggregate, ensuring that
all mineral matter has been removed from the binder extraction apparatus. Weigh and record the mass
of the aggregate in the tray.
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5.3.2.4 If required, determine the particle size distribution of the recovered aggregate in
accordance with EN 933-1, making due allowance for any mineral filler collected by the filter paper,
where appropriate.
5.4 Binder quantity
5.4.1 Apparatus
5.4.1.1 Recovery apparatus, conforming to the requirements of the method selected from B.3.
The apparatus should be calibrated and traceable.
5.4.2 Procedure
5.4.2.1 Difference method
Where the binder quantity is determined by difference, add the mass of recovered aggregate to the
mass of any mineral filler collected by filter paper.
5.4.2.2 Recovery method
Where the binder quantity is determined by recovering the binder of the binder solution, follow the
procedures described in B.3.
5.5 Calculation and expression of results
5.5.1 General
The soluble binder content, S, as a percentage of the mass of the original dry test portion, shall be
calculated in accordance with 5.5.2, 5.5.3, 5.5.4 or 5.5.5, as appropriate.
NOTE 1 Formulae are given for un-dried test portions. Where test portions have been dried to constant mass,
M, becomes the mass of the dried test portion and M , is deleted.
W
NOTE 2 For mixtures with a binder having a significant proportion of insolubles, the total binder content can
be calculated by taking account of the insoluble binder content in accordance with A.4.
5.5.2 Binder determined by difference
Calculate the soluble binder content, S, in percentage by mass, by means of the following formula:
100×[M−(M +M )]
1 W
S= (1)
M−M
W
where
S is the soluble binder content, expressed in percent (%);
M is the mass of un-dried test portion, expressed in grams (g);
M is the mass of recovered mineral matter, expressed in grams (g);
1
M is the mass of water in the un-dried test portion, expressed in grams (g).
W
5.5.3 Binder by total recovery
Calculate the soluble binder content, S, in percentage by mass, by means of the following formula:
100×M
b
S= (2)
M−M
W
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where
S is the soluble binder content, expressed in percent (%);
M is the mass of un-dried test portion, expressed in grams (g);
M is the mass of recovered binder, expressed in grams (g);
b
M is the mass of water in the un-dried test portion, expressed in grams (g).
W
5.5.4 Binder by recovery from portion (volume calculation)
Calculate the soluble binder content, S, in percentage by mass, by means of the following formula:
100×z×V×d (3)
S=
(M− M )×(d×v− z)
w
where
S is the soluble binder content, expressed in percent (%);
M is the mass of un-dried test portion, expressed in grams (g);
z is the average mass of binder recovered from each aliquot portion of binder solution,
expressed in grams (g);
V
3
is the total volume of solvent, expressed in cubic millimetres (mm );
v
3
is the volume of each aliquot solution portion, expressed in cubic millimetres (mm );
d
3
is the density of the binder at 25 °C, expressed in grams per cubic millimetres (g/mm );
M is the mass of water in the un-dried test portion, expressed in grams (g).
W
5.5.5 Binder by recovery from portion (mass calculation)
Calculate the soluble binder conten
...
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