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

Status
Published
Public Enquiry End Date
19-Feb-2019
Publication Date
07-Apr-2020
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
31-Mar-2020
Due Date
05-Jun-2020
Completion Date
08-Apr-2020

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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

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SIST EN 12697-1:2020
EN 12697-1:2020 (E)

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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SIST EN 12697-1:2020
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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SIST EN 12697-1:2020
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;

— [B.2.1.1.1] acceleration amended to 25 000 m/s for consistency with EN 12697-3;

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SIST EN 12697-1:2020
EN 12697-1:2020 (E)
— [C.2.1.1.1] accuracy of balance amended to read ± 1 mg;

— [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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SIST EN 12697-1:2020
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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SIST EN 12697-1:2020
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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SIST EN 12697-1:2020
EN 12697-1:2020 (E)
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.
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SIST EN 12697-1:2020
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.

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SIST EN 12697-1:2020
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
...

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