Bituminous mixtures - Test methods - Part 39: Binder content by ignition

This document describes a test method for the determination of the binder content of samples of bituminous mixtures by ignition. As such, it is an alternative to the more traditional method of extracting the binder using solvents. The method can be used for evaluation of mixture composition because the remaining aggregate can be used for determining aggregate gradation and density, provided excessive breakdown of the aggregate particles does not occur at the temperature reached. The results can be used for process control or checks on the compliance of mixtures. However, the need for calibration of a mixture, either on the complete mixture or on each of its component materials separately, before an analysis can be carried out makes this method easier to use with regularly used mixtures rather than with an extensive range of different mixtures from different aggregate sources. The test method is equally suitable for the analysis of mixtures containing unmodified or modified binders because the method has to be calibrated for each mixture being checked when calibration on mixtures is used. In case of doubt/dispute, the determination of the calibration value based on laboratory-prepared bituminous mixtures (see A.1 and A.2) is the reference method.

Asphalt - Prüfverfahren - Teil 39: Bindemittelgehalt durch Thermoanalyse

Dieses Dokument beschreibt ein Prüfverfahren zur Bestimmung des Bindemittelgehaltes von Asphalt-Proben durch Thermoanalyse. Als solches stellt es eine Alternative zum eher traditionellen Verfahren der Bindemittelextraktion mit Lösemitteln dar. Das Verfahren kann zur Bewertung der Mischgut-zusammensetzung verwendet werden, weil die verbleibenden Gesteinskörnungen zur Bestimmung der Korngrößenverteilung der Gesteinskörnungen und der Dichte verwendet werden können, vorausgesetzt, dass bei der erreichten Temperatur kein übermäßiger Zerfall der Gesteinskörnungen auftritt. Die Ergebnisse können zur Prozesssteuerung oder zur Überprüfung der Übereinstimmung von Gemischen mit Anforderungen verwendet werden. Durch die Notwendigkeit, das Gemische als Ganzes oder seine Bestandteile einzeln zu kalibrieren, bevor eine Analyse durchgeführt werden kann, eignet sich dieses Verfahren eher für die Anwendung auf regelmäßig verwendete Gemische als auf eine ganze Reihe verschiedener Gemische mit Gesteinskörnungen unterschiedlicher Herkunft. Das Prüfverfahren ist ebenso geeignet für die Analyse von Mischgütern mit nicht modifizierten oder modifizierten Bindemitteln, weil es für jedes zu überprüfende Gemisch zu kalibrieren ist, sofern eine Kalibrierung an Gemischen durchgeführt wird. In Zweifels- oder Streitfällen gilt die Bestimmung des Kalibrierwertes auf der Grundlage von im Labor hergestellten Asphalt (siehe A.1 und A.2) als Referenzverfahren.

Mélanges bitumineux - Méthodes d'essai - Partie 39 : Détermination de la teneur en liant par calcination

Ce document décrit une méthode d’essai pour la détermination de la teneur en liant d’échantillons de mélanges bitumineux par calcination. Comme telle, il représente une alternative à la méthode plus traditionnelle d’extraction de liant au moyen de solvants. La méthode peut être utilisée pour l’évaluation de la composition d’un mélange, les granulats restants pouvant servir à déterminer la granularité et la masse volumique du granulat à condition que les grains n’aient pas subi d’éclatements excessifs à cause de la température atteinte. Les résultats peuvent être utilisés pour la maîtrise de la fabrication ou pour des vérifications de conformité des mélanges. Toutefois, la nécessité de calibrer un mélange, soit sur le mélange complet, soit séparément sur chacun de ses matériaux constitutifs, avant de réaliser une analyse rend cette méthode préférable pour des mélanges utilisés régulièrement, plutôt que pour des familles de mélanges comportant des composants d’origines variées. La méthode d’essai est applicable également pour des mélanges comportant des liants modifiés ou non, le calibrage étant effectué pour chaque mélange à analyser. En cas de doute ou de litige, la détermination du facteur de calibrage fondé sur des mélanges bitumineux préparés en laboratoire (voir A.1 et A.2) est la procédure de référence.

Bitumenske zmesi - Preskusne metode - 39. del: Ugotavljanje deleža veziva s sežigom

General Information

Status
Published
Publication Date
25-Feb-2020
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
26-Feb-2020
Completion Date
26-Feb-2020

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SLOVENSKI STANDARD
SIST EN 12697-39:2020
01-maj-2020
Nadomešča:
SIST EN 12697-39:2012
Bitumenske zmesi - Preskusne metode - 39. del: Ugotavljanje deleža veziva s
sežigom
Bituminous mixtures - Test methods - Part 39: Binder content by ignition
Asphalt - Prüfverfahren - Teil 39: Bindemittelgehalt durch Thermoanalyse
Mélanges bitumineux - Méthodes d'essai - Partie 39 : Teneur en bitume
Ta slovenski standard je istoveten z: EN 12697-39:2020
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
SIST EN 12697-39:2020 en,fr,de

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

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SIST EN 12697-39:2020
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SIST EN 12697-39:2020
EN 12697-39
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2020
EUROPÄISCHE NORM
ICS 93.080.20 Supersedes EN 12697-39:2012
English Version
Bituminous mixtures - Test methods - Part 39: Binder
content by ignition

Mélanges bitumineux - Méthodes d'essai - Partie 39 : Asphalt - Prüfverfahren - Teil 39: Bindemittelgehalt

Teneur en bitume par calcination durch Thermoanalyse
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 12697-39:2020 E

worldwide for CEN national Members.
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SIST EN 12697-39:2020
EN 12697-39:2020 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 5

5 Apparatus ........................................................................................................................................................... 6

6 Preparatory treatment of laboratory samples of bituminous mixtures ..................................... 7

7 Procedure........................................................................................................................................................... 8

7.1 General ................................................................................................................................................................ 8

7.2 Test procedure for furnace with internal balance (Method A) ...................................................... 8

7.3 Procedure for furnace without internal balance (Method B) ......................................................... 9

8 Calculation ...................................................................................................................................................... 10

8.1 Method A.......................................................................................................................................................... 10

8.2 Method B.......................................................................................................................................................... 11

9 Test report ...................................................................................................................................................... 11

10 Precision data ................................................................................................................................................ 12

Annex A (normative) Calculation of calibration value .................................................................................. 13

A.1 General ............................................................................................................................................................. 13

A.2 Calibration based on laboratory-prepared bituminous mixtures ............................................. 13

A.3 Calibration based on parallel analysis with extraction methods ............................................... 14

A.4 Calibration based on dry analysis of constituent aggregate ......................................................... 15

Annex B (informative) Aggregate grading .......................................................................................................... 18

Bibliography ................................................................................................................................................................. 19

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SIST EN 12697-39:2020
EN 12697-39:2020 (E)
European foreword

This document (EN 12697-39:2020) 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 August 2020, and conflicting national standards shall

be withdrawn at the latest by August 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 12697-39:2012.

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] references added to each formula in related text;

— [ge] NOTEs modified or adjusted to normal text where appropriate according to ISO/IEC Directives

– Part 2:2016, 24.5;
— [Clause 2] titles for test methods EN 12697-series corrected.
A list of all parts in the EN 12697 series can be found on the CEN website.

WARNING — The temperature of the oven and the different accessories is extremely high during the

ignition method. Special care should be taken when handling the equipment and the samples baskets

etc. should be placed, shielded and marked in a way that helps ensure any unpremeditated contact is

avoided.

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 12697-39:2020
EN 12697-39:2020 (E)
1 Scope

This document describes a test method for the determination of the binder content of samples of

bituminous mixtures by ignition. As such, it is an alternative to the more traditional method of

extracting the binder using solvents. The method can be used for evaluation of mixture composition

because the remaining aggregate can be used for determining aggregate gradation and density,

provided excessive breakdown of the aggregate particles does not occur at the temperature reached.

The results can be used for process control or checks on the compliance of mixtures. However, the need

for calibration of a mixture, either on the complete mixture or on each of its component materials

separately, before an analysis can be carried out makes this method easier to use with regularly used

mixtures rather than with an extensive range of different mixtures from different aggregate sources.

The test method is equally suitable for the analysis of mixtures containing unmodified or modified

binders because the method has to be calibrated for each mixture being checked when calibration on

mixtures is used. In case of doubt/dispute, the determination of the calibration value based on

laboratory-prepared bituminous mixtures (see A.1 and A.2) is the reference method.

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 12597, Bitumen and bituminous binders — Terminology
EN 12697-1, Bituminous mixtures — Test methods — Part 1: Soluble binder content
EN 12697-14, Bituminous mixtures — Test methods — Part 14: Water content
EN 12697-27, Bituminous mixtures — Test methods — Part 27: Sampling

EN 12697-28, Bituminous mixtures — Test methods — Part 28: Preparation of samples for determining

binder content, water content and grading
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
binder
covers bituminous binder as described in EN 12597
3.2
corrected binder content

calculated binder content after correction by the calibration value in order to compensate for

components in the asphalt material itself that, due to the high temperatures during ignition, could give

rise to misinterpretations
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SIST EN 12697-39:2020
EN 12697-39:2020 (E)
3.3
calibration value

mean difference between the actual and measured binder contents for a particular bituminous mixture,

in per cent, as measured from three samples

Note 1 to entry: The calibration value is a specific, material-dependent value that normally results from a loss of

mass during the ignition from constituents in the mixture other than the binder. The principle of the binder

content by ignition is based upon a pre-determination of the corrections for the constituents used in the mixture,

primarily the aggregate.

Note 2 to entry: Mineral aggregates will show varying losses of mass during the test depending on their origin

(petrographic composition). Examples of components that give rise to high corrections are limestone, hydrated

lime and cellulose fibres.

Note 3 to entry: Methods for determining the calibration values are given in Annex A (normative).

3.4
target temperature

temperature to which the furnace would raise the sample in the test without the rise in temperature

due to the exothermic reaction of burning the binder

Note 1 to entry: The target temperature (usually 540 °C) is determined during the calibration.

3.5
test completion time

time from when the temperature in the furnace returns to the target temperature, after the initial rise

above that temperature, to when the test is completed with the sample having nominally reached

constant mass

Note 1 to entry: If a furnace with an internal balance is used, the completion time is when the loss of mass

between individual readings taken at 1 min intervals for three consecutive minutes is less than a constant mass

limit. If a furnace without an internal balance is used, the completion time is when the change in the mass of the

sample after further ignition for 15 min is less than a constant mass limit.
4 Principle

The test method determines the binder content of bituminous mixtures by ignition of the mixture in a

furnace.

The corrected binder content is obtained by a calculation that includes a calibration term. Calibration

terms are determined for particular asphalt mixtures or aggregates. Two test methods are described:

Method A utilizes a furnace with an internal balance; Method B permits the use of a furnace and

external balance. Re-determination (re-calibration or re-calculation depending on the calibration

method chosen from Annex A) shall be undertaken for each significant change in the mixture, including

changes in the constituent materials or their proportions.

The ignition process should have a controlled rise in temperature in order to avoid excessive heating of

the mineral aggregate which can break down the aggregate particles depending on the petrographic

composition.

NOTE The calculation of the calibration value based on parallel analysis with extraction methods (A.1 and

A.3) is appropriate for mixtures for which the intended proportions of the constituent materials are not known.

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SIST EN 12697-39:2020
EN 12697-39:2020 (E)
5 Apparatus
5.1 Furnace.

5.1.1 Furnace, capable of burning all the binder with the features detailed in 5.1.2 to 5.1.6 for

Method A and 5.1.2 to 5.1.4 for Method B.

NOTE The temperature required to burn all the binder will depend on the technology used and is determined

as part of the calibration procedure (see Annex A).

The furnace should not operate at its maximum capacity in order to allow flexibility and to ensure long

service.

5.1.2 Sample chamber, having an internal capacity capable of taking the sample without touching

the sides and with the maximum dimensions not greater than twice the minimum dimensions.

NOTE Larger chamber sizes can expedite testing by allowing larger sample basket(s) (and thus the material

to be tested can be placed in thinner layers).

5.1.3 Automatic lock, that shall not allow the door to be opened until the completion of the test

procedure, and a warning system to indicate the end of the pre-programmed temperature cycle.

5.1.4 System for reducing furnace emissions, by which the furnace shall be vented into a hood or to

the outside and which, when properly set up, shall permit no noticeable odours escaping into the

laboratory.

The furnace shall have a fan with the capability to pull sufficient air through the furnace to expedite the

test and to reduce the escape of smoke into the laboratory.

NOTE The method for reducing furnace emissions can comprise a filter and a post combustion chamber that

is designed to eliminate the toxic residues produced by burning the binder.

If mechanical ventilation is used, the air flow should be adjusted so as not to affect the operation of the

equipment (e.g. a forced air extraction system may result in a loss of fines and the generation of fumes

from the furnace).

5.1.5 Internal balance, capable of detecting mass variations of ± 0,1 g in the sample within the

baskets.
The balance shall be thermally isolated from the furnace chamber.

5.1.6 Data collection system and a warning system, which shall be capable of being set to a value

such that the loss in mass between individual readings taken at 1 min intervals for three consecutive

minutes at end of the pre-programmed temperature cycle is not higher than the values stated in

Table 1.

5.2 Metal baskets, manufactured from perforated sheet of tempered stainless steel or other suitable

material that permits adequate air flow through the sample and retains the majority of the sample

throughout the test.

The dimensions shall be specified by the furnace manufacturer to provide the maximum surface area

for the sample while still providing sufficient room to safely load and unload the sample. The baskets

shall be capable of being nested.

5.3 Catch pan, made of stainless steel with dimensions sized to accommodate the metal baskets

specified in 5.2.
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SIST EN 12697-39:2020
EN 12697-39:2020 (E)

5.4 Oven, with convection or forced draft, capable of maintaining a temperature of (110 ± 5) °C in the

vicinity of the samples.

5.5 External balance, capable of weighing the mass of trays plus the catch pan and the test sample

according to Table 1 to ± 0,1 g.

5.6 Safety equipment, including safety glasses or face shield, high temperature gloves, and long

sleeved jacket.

5.7 Heat-resistant surface, capable of withstanding 650 °C and able to act as a heat sink that can

speed the cooling of the sample baskets, and protective cage, capable of completely surrounding the

sample baskets and preventing accidental physical contact with them.

An appropriate sign warning of the danger of ‘Very Hot Surfaces’ should be attached to the protective

cage.

5.8 Pan, larger than the sample basket(s), for transferring samples after ignition.

5.9 Spatulas.
5.10 Bowls.
5.11 Wire brushes.
6 Preparatory treatment of laboratory samples of bituminous mixtures

6.1 Sampling shall be performed in accordance with EN 12697-28 to achieve a sample size as given in

Table 1. The mass of the sample in the baskets during the test shall be the same as the mass used for the

calibration to ± 100 g.
Table 1 — Size of sample
Nominal maximum aggregate Mass of sample Maximum constant mass
size limit
mm g g
4 1 000 to 1 400 0,15
5,6 or 6,3 or 8 or 10 1 000 to 1 600 0,15
11,2 or 12,5 or 14 or 16 1 000 to 1 700 0,20
20 or 22,4 1 000 to 2 400 0,25
31,5 1 000 to 3 000 0,30
40 or 45 1 000 to 4 000 0,40

When the mass of the test specimen exceeds the capacity of the equipment used, the test specimen may

be divided into suitable increments, tested, and the results combined by weighted average for

calculation of the corrected binder content.

NOTE Large samples of fine mixtures tend to result in incomplete ignition of the binder.

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SIST EN 12697-39:2020
EN 12697-39:2020 (E)

6.2 The sample shall be dried to constant mass in an oven at (110 ± 5) °C unless it is known that the

sample does not contain water. Alternatively, the water content shall be determined in accordance with

EN 12697-14 for later correction.

NOTE If a damp sample is tested, the water content will be driven off and could be counted as binder if no

correction is made.
7 Procedure
7.1 General

7.1.1 Obtain the calibration value in accordance with Annex A for the specific mixture to be analysed

either directly or from records. The calibration procedure (or re-calculation for calibration based on dry

analysis of constituent aggregate) shall be carried out with a mixture before undertaking any

acceptance testing, and repeated at regular intervals. It shall also be carried out each time there is a

significant change in the mixture design. A significant change is classified as being:

— a change of source for any component material (particularly recycled asphalt pavement); and/or

— a change in the proportion of the component materials (other than the binder or recycled asphalt

pavement) by 10 % or more of their original proportion; and/or

— a change in the proportion of any recycled asphalt pavement by 5 % or more of the original

proportion; and/or
— a change of target binder content by 0,5 % or more.

NOTE 1 The calculation of the calibration value based on parallel analysis with extraction methods (A.1 and

A.3) is appropriate for mixtures for which the intended proportions of the constituent materials are not known.

NOTE 2 The analysis method by ignition can be affected by the type of aggregate in the mixture.

NOTE 3 Mineral aggregate (and organic fibres) will show varying losses of mass during the test depending on

their origin (petrographic composition). Examples of components that give rise to high corrections are limestone,

hydrated lime and cellulose fibres. The calibration value for these components can be measured by determination

on a bitumen/filler mortar (A.4).

7.1.2 The test shall be carried out using the same equipment used in the calibration, including furnace

and sample baskets.

7.1.3 Pre-heat the ignition furnace. Record the furnace temperature at the start of the test.

7.1.4 Continue the procedure in accordance with either 7.2 (Method A) for
...

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