Bituminous mixtures - Test methods for hot mix asphalt - 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.
Test methods for the analysis of mixtures containing modified binders are outside the scope of this document.

Asphalt - Prüfverfahren für Heißasphalt - Teil 1: Löslicher Bindemittelgehalt

Mélanges bitumineux - Méthode d'essai pour mélange hydrocarboné à chaud - 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.
Les méthodes d’essai pour l’analyse des matériaux contenant des liants modifiés n’appartiennent pas au domaine d’application du présent document, sauf si les conseils donnés en annexe D sont suivis. Même dans ce cas, la précision des analyses est susceptible d’être défaillante.

Bitumenske zmesi – Preskusne metode za vroče asfaltne zmesi – 1. del: Topni delež veziva

General Information

Status
Withdrawn
Publication Date
22-Nov-2005
Withdrawal Date
05-Jun-2012
Current Stage
9960 - Withdrawal effective - Withdrawal
Start Date
06-Jun-2012
Completion Date
06-Jun-2012

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SLOVENSKI STANDARD
SIST EN 12697-1:2006
01-februar-2006
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SIST EN 12697-1:2002
SIST EN 12697-1:2002/AC:2002
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GHOHåYH]LYD

Bituminous mixtures - Test methods for hot mix asphalt - Part 1: Soluble binder content

Asphalt - Prüfverfahren für Heißasphalt - Teil 1: Löslicher Bindemittelgehalt

Mélanges bitumineux - Méthode d'essai pour mélange hydrocarboné a chaud - Partie 1:

Teneur en liant soluble
Ta slovenski standard je istoveten z: EN 12697-1:2005
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
SIST EN 12697-1:2006 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 12697-1:2006
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SIST EN 12697-1:2006
EUROPEAN STANDARD
EN 12697-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2005
ICS 93.080.20 Supersedes EN 12697-1:2000
English Version
Bituminous mixtures - Test methods for hot mix asphalt - Part 1:
Soluble binder content

Mélanges bitumineux - Méthode d'essai pour mélange Asphalt - Prüfverfahren für Heißasphalt - Teil 1: Löslicher

hydrocarboné à chaud - Partie 1: Teneur en liant soluble Bindemittelgehalt
This European Standard was approved by CEN on 30 September 2005.

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 Central Secretariat 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 Central Secretariat has the same status as the official

versions.

CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,

Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,

Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12697-1:2005: E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 12697-1:2006
EN 12697-1:2005 (E)
Content Page

Foreword ..........................................................................................................................................................4

Introduction......................................................................................................................................................7

1 Scope...................................................................................................................................................8

2 Normative references.........................................................................................................................8

3 Terms and definitions.........................................................................................................................8

4 Preparatory treatment of laboratory samples of bituminous mixtures...........................................9

5 Determination of binder content........................................................................................................9

5.1 General principles of test ...................................................................................................................9

5.2 Binder extraction...............................................................................................................................10

5.2.1 Solvent...............................................................................................................................................10

5.2.2 Apparatus..........................................................................................................................................10

5.2.3 Procedure..........................................................................................................................................10

5.3 Separation of mineral matter............................................................................................................11

5.3.1 Apparatus..........................................................................................................................................11

5.3.2 Procedure..........................................................................................................................................11

5.4 Binder quantity..................................................................................................................................11

5.4.1 Apparatus..........................................................................................................................................11

5.4.2 Procedure..........................................................................................................................................11

5.5 Calculation and expression of results.............................................................................................12

5.5.1 General..............................................................................................................................................12

5.5.2 Binder determined by difference .....................................................................................................12

5.5.3 Binder by total recovery ...................................................................................................................12

5.5.4 Binder by recovery from portion (volume calculation) ..................................................................12

5.5.5 Binder by recovery from portion (mass calculation)......................................................................13

6 Drying to constant mass ..................................................................................................................13

6.1 General..............................................................................................................................................13

6.2 Apparatus..........................................................................................................................................13

6.3 Procedure..........................................................................................................................................14

7 Reporting of results..........................................................................................................................14

7.1 Results...............................................................................................................................................14

7.2 Test report.........................................................................................................................................14

8 Precision data...................................................................................................................................14

8.1 Precision – Experiment 1 .................................................................................................................15

8.2 Precision – Experiment 2 .................................................................................................................15

8.3 Precision – Experiment 3 .................................................................................................................16

Annex A (informative) Guidance on the determination of binder content .................................................17

A.1 Evaluation of the results ..................................................................................................................17

A.2 Effect of water content.....................................................................................................................17

A.3 Choice of test equipment and the sequence of operations...........................................................18

A.4 Determination of total binder content .............................................................................................18

Annex B (normative) Use of equipment for the determination of binder content .....................................20

B.1 Binder extraction...............................................................................................................................20

B.1.1 Hot extractor (paper filter) method ..................................................................................................20

B.1.2 Hot extractor (wire mesh filter) method ..........................................................................................23

B.1.3 Soxhlet extractor method.................................................................................................................25

B.1.4 Bottle rotation machine method ......................................................................................................27

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SIST EN 12697-1:2006
EN 12697-1:2005 (E)

B.1.5 Centrifuge extractor method............................................................................................................29

B.1.6 Cold mix dissolution of bitumen by agitation.................................................................................31

B.2 Separation of mineral matter............................................................................................................31

B.2.1 Continuous flow centrifuge..............................................................................................................31

B.2.2 Pressure filter....................................................................................................................................33

B.2.3 Bucket type centrifuge – Type 1 ......................................................................................................34

B.2.4 Bucket type centrifuge – Type 2 ......................................................................................................35

B.3 Soluble binder content .....................................................................................................................36

B.3.1 Method by recovery from a portion using a volume calculation...................................................36

B.3.2 Method by recovery from a portion using a mass calculation ......................................................38

Annex C (normative) Determination of residual mineral matter in the binder extract by

incineration........................................................................................................................................39

C.1 General..............................................................................................................................................39

C.2 Method 1............................................................................................................................................39

C.2.1 Apparatus..........................................................................................................................................39

C.2.2 Reagent..............................................................................................................................................39

C.2.3 Procedure..........................................................................................................................................39

C.3 Method 2............................................................................................................................................40

C.3.1 Apparatus..........................................................................................................................................40

C.3.2 Procedure..........................................................................................................................................40

Annex D (informative) Guidance on determination of soluble binder content of mixtures with

polymer-modified binders ................................................................................................................42

D.1 General..............................................................................................................................................42

D.2 Preparatory treatment of laboratory samples of bituminous mixtures.........................................42

D.3 Determination of binder content......................................................................................................42

D.3.1 General principles of test .................................................................................................................42

D.3.2 Binder extraction..............................................................................................................................42

D.3.3 Separation of mineral matter............................................................................................................44

D.3.4 Binder quantity..................................................................................................................................45

D.3.5 Calculation and expression of results.............................................................................................45

D.4 Drying to constant mass ..................................................................................................................45

D.5 Reporting of results..........................................................................................................................45

D.6 Precision data...................................................................................................................................45

Bibliography...................................................................................................................................................46

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SIST EN 12697-1:2006
EN 12697-1:2005 (E)
Foreword

This document (EN 12697-1:2005) has been prepared by Technical Committee CEN/TC 227 “Road materials”,

the secretariat of which is held by DIN.

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 May 2006, and conflicting national standards shall be withdrawn at the

latest by January 2008.
This document is one of a series of standards as listed below.

EN 12697-1, Bituminous mixtures — Test methods for hot mix asphalt — Part 1: Soluble binder content.

EN 12697-2, Bituminous mixtures — Test methods for hot mix asphalt — Part 2: Determination of particle size

distribution.

EN 12697-3, Bituminous mixtures —Test methods for hot mix asphalt — Part 3: Bitumen recovery: Rotary

evaporator.

EN 12697-4, Bituminous mixtures — Test methods for hot mix asphalt — Part 4: Bitumen recovery:

Fractionating column.

EN 12697-5, Bituminous mixtures — Test methods for hot mix asphalt — Part 5: Determination of the

maximum density.

EN 12697-6, Bituminous mixtures — Test methods for hot mix asphalt — Part 6: Determination of bulk density

of bituminous specimens.

EN 12697-7, Bituminous mixtures — Test methods for hot mix asphalt — Part 7: Determination of bulk density

of bituminous specimens by gamma rays.

EN 12697-8, Bituminous mixtures — Test methods for hot mix asphalt — Part 8: Determination of void

characteristics of bituminous specimens.

EN 12697-9, Bituminous mixtures — Test methods for hot mix asphalt — Part 9: Determination of the

reference density.

EN 12697-10, Bituminous mixtures — Test methods for hot mix asphalt — Part 10: Compactability.

EN 12697-11, Bituminous mixtures — Test methods for hot mix asphalt — Part 11: Determination of the

affinity between aggregate and bitumen.

EN 12697-12, Bituminous mixtures — Test methods for hot mix asphalt — Part 12: Determination of the water

sensitivity of bituminous specimens.

EN 12697-13, Bituminous mixtures — Test methods for hot mix asphalt — Part 13: Temperature measure-

ment.

EN 12697-14, Bituminous mixtures — Test methods for hot mix asphalt — Part 14: Water content.

EN 12697-15, Bituminous mixtures — Test methods for hot mix asphalt — Part 15: Determination of the

segregation sensitivity.

EN 12697-16, Bituminous mixtures — Test methods for hot mix asphalt — Part 16: Abrasion by studded tyres.

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SIST EN 12697-1:2006
EN 12697-1:2005 (E)

EN 12697-17, Bituminous mixtures — Test methods for hot mix asphalt — Part 17: Particle loss of porous

asphalt specimen.

EN 12697-18, Bituminous mixtures — Test methods for hot mix asphalt — Part 18: Binder drainage.

EN 12697-19, Bituminous mixtures — Test methods for hot mix asphalt — Part 19: Permeability of specimen.

EN 12697-20, Bituminous mixtures — Test methods for hot mix asphalt — Part 20: Indentation using cube or

Marshall specimens.

EN 12697-21, Bituminous mixtures — Test methods for hot mix asphalt — Part 21: Indentation using plate

specimens.

EN 12697-22, Bituminous mixtures — Test methods for hot mix asphalt — Part 22: Wheel tracking.

EN 12697-23, Bituminous mixtures — Test methods for hot mix asphalt — Part 23: Determination of the

indirect tensile strength of bituminous specimens.

EN 12697-24, Bituminous mixtures — Test methods for hot mix asphalt — Part 24: Resistance to fatigue.

EN 12697-25, Bituminous mixtures — Test methods for hot mix asphalt — Part 25: Cyclic compression test.

EN 12697-26, Bituminous mixtures — Test methods for hot mix asphalt — Part 26: Stiffness.

EN 12697-27, Bituminous mixtures — Test methods for hot mix asphalt — Part 27: Sampling.

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 12697-29, Bituminous mixtures — Test methods for hot mix asphalt — Part 29: Determination of the

dimensions of a bituminous specimen.

EN 12697-30, Bituminous mixtures — Test methods for hot mix asphalt — Part 30: Specimen preparation,

impact compactor.

EN 12697-31, Bituminous mixtures — Test methods for hot mix asphalt — Part 31: Specimen preparation,

gyratory compactor.

EN 12697-32, Bituminous mixtures — Test methods for hot mix asphalt — Part 32: Laboratory compaction of

bituminous mixtures by a vibratory compactor.

EN 12697-33, Bituminous mixtures — Test methods for hot mix asphalt — Part 33: Specimen prepared, by

roller compactor.

EN 12697-34, Bituminous mixtures — Test methods for hot mix asphalt — Part 34: Marshall test.

EN 12697-35, Bituminous mixtures — Test methods for hot mix asphalt — Part 35: Laboratory mixing.

EN 12697-36, Bituminous mixtures — Test methods for hot mix asphalt — Part 36: Determination of the

thickness of a bituminous pavement.

EN 12697-37, Bituminous mixtures — Test methods for hot mix asphalt — Part 37: Hot sand test for the

adhesivity of binder on precoated chippings for HRA.

EN 12697-38, Bituminous mixtures — Test methods for hot mix asphalt — Part 38: Common equipment and

calibration.

EN 12697-39, Bituminous mixtures — Test methods for hot mix asphalt — Part 39: Binder content by ignition.

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SIST EN 12697-1:2006
EN 12697-1:2005 (E)

EN 12697-40, Bituminous mixtures - Test methods for hot mix asphalt - Part 40: In-situ drainablility

EN 12697-41, Bituminous mixtures — Test methods for hot mix asphalt — Part 41: Resistance to de-icing

fluids.

EN 12697-42, Bituminous mixtures — Test methods for hot mix asphalt — Part 42: Amount of foreign matters

in reclaimed asphalt.

EN 12697-43, Bituminous mixtures — Test methods for hot mix asphalt — Part 43: Resistance to fuel.

The applicability of this European Standard is described in the product standards for bituminous mixtures.

This European Standard supersedes EN 12697-1:2000.
WARNING — The method described in this European Standard may require the use of

dichloromethane (methylene chloride), 1.1.1 trichlorethane, benzene, trichlorethylene, xylene, toluene,

perchloroethylene (tetracloroethylene) 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 emphasised 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 organizations of the following

countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,

Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland

and United Kingdom.
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SIST EN 12697-1:2006
EN 12697-1:2005 (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 whilst 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 it has been demonstrated that they 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 12697-1:2006
EN 12697-1:2005 (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.

The analysis of mixtures containing modified binders is outside the scope of this document unless the advice

given in Annex D is followed. Even when that advice is followed, the precision of the analysis may be

compromised.
2 Normative references

The following referenced documents are indispensable for the application 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 12697-3:2005, Bituminous mixtures — Test methods for hot mix asphalt — Part 3: Bitumen recovery:

Rotary evaporator.

EN 12697-4:2005, Bituminous mixtures — Test methods for hot mix asphalt — 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, wafer 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.
3.1
soluble binder content

percentage by mass of extractable binder in an anhydrous sample determined by extracting the binder from

the sample
NOTE 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

3.3
precision

closeness of agreement between independent test results obtained under stipulated conditions

NOTE 1 Precision depends only on the distribution of random errors and does not relate to the true value or the

specified value.
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SIST EN 12697-1:2006
EN 12697-1:2005 (E)

NOTE 2 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 "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

value less than or equal to which the absolute difference between two test results obtained under repeatability

conditions may be expected to be with a probability of 95 %
NOTE 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

value less than or equal to which the absolute difference between two test results obtained under

reproducibility conditions may be expected to be with a probability of 95 %
NOTE The symbol used for reproducibility limit is R.
3.10
single test result

value obtained by applying the standard test method fully, once to a single specimen may 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
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:
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SIST EN 12697-1:2006
EN 12697-1:2005 (E)
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.

NOTE 2 If it is suspected that water is present in the laboratory sample, it should be dried to constant mass (see

clause 6) or the water content may be determined by the method described in EN 12697-14 or the sample treated as in

EN 12697-28.

NOTE 3 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 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 1 Currently all hydrocarbon solvents are regarded as "hazardous" and "environmentally unfriendly" to varying

degrees.

NOTE 2 Until such time as there is an agreed CEN policy with regard to their usage, 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).

NOTE 3 Trichloroethylene should be stored in sealed bottles or canisters, which are protected against UV radiation.

NOTE 4 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 and a useful precaution is to

store the solvent over calcium oxide in coloured glass or suitable metal containers.

5.2.2 Appa
...

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