EN 1744-4:2021

Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility of fillers for bituminous mixtures

This document specifies the procedure for the determination of the water susceptibility of fillers for bituminous mixtures, by separation of filler from a bitumen filler mixture.
A method for the determination of water susceptibility by volume increase and loss of stability of a Marshall specimen is described in Annex A.

Prüfverfahren für chemische Eigenschaften von Gesteinskörnungen - Teil 4: Bestimmung der Wasserempfindlichkeit von Füllern in bitumenhaltigen Mischungen

Dieses Dokument legt ein Verfahren für die Bestimmung der Wasserempfindlichkeit von Füllern für bitumenhaltige Mischungen durch Abtrennung von Füllern aus einer bitumenhaltigen Mischung fest.
Ein Verfahren zur Bestimmung der Wasserempfindlichkeit durch Volumenzunahme und Stabilitätsverlust eines Marshall-Probekörpers wird in Anhang A beschrieben.

Essais pour déterminer les caractéristiques chimiques des granulats - Partie 4 : Détermination de la sensibilité à l’eau des fillers pour mélanges bitumineux

Le présent document spécifie le mode opératoire pour la détermination de la sensibilité à l’eau des fillers pour mélanges bitumineux, par séparation du filler d’un mélange bitume-filler.
Une méthode de détermination de la sensibilité à l’eau par augmentation de volume et perte de stabilité d’une éprouvette Marshall est décrite à l’Annexe A.

Preskusi kemičnih lastnosti agregatov - 4. del: Ugotavljanje občutljivosti polnil za bitumenske mešanice na vodo

Ta dokument določa postopek za ugotavljanje občutljivosti polnil za bitumenske mešanice na vodo z ločevanjem polnila iz bitumenske mešanice s polnilom.
Metoda za ugotavljanje občutljivosti na vodo s povečanjem volumna in izgubo stabilnosti vzorca po Marshallu je opisana v dodatku A.

General Information

• Status: Published
• Publication Date: 21-Dec-2021
• Withdrawal Date: 29-Jun-2022
• ICS: 91.100.15 - Mineral materials and products
• Technical Committee: CEN/TC 154 - Aggregates
• Drafting Committee: CEN/TC 154/SC 6 - Test methods
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 22-Dec-2021
• Completion Date: 22-Dec-2021
• Directive: 305/2011 - Regulation (eu) No 305/2011 of the European Parliament and of the Council of 9 march 2011 laying down harmonised conditions for the marketing of construction products and repealing council directive 89/106/eec
• Mandate: M/125 - Mandate to CEN/CENELEC concerning the execution of standardization work for harmonized standards on aggregates
• Ref Project: SIST EN 1744-4:2022 - Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility of fillers for bituminous mixtures

Relations

• Replaces: EN 1744-4:2005 - Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility of fillers for bituminous mixtures
• Effective Date: 19-Jul-2017

Standards Content (Sample)

SLOVENSKI STANDARD
01-april-2022
Nadomešča:
SIST EN 1744-4:2005
Preskusi kemičnih lastnosti agregatov - 4. del: Ugotavljanje občutljivosti polnil za
bitumenske mešanice na vodo
Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility
of fillers for bituminous mixtures
Prüfverfahren für chemische Eigenschaften von Gesteinskörnungen - Teil 4:
Bestimmung der Wasserempfindlichkeit von Füllern in bitumenhaltigen Mischungen
Essais pour déterminer les caractéristiques chimiques des granulats - Partie 4 :
Détermination de la sensibilité à l’eau des fillers pour mélanges bitumineux
Ta slovenski standard je istoveten z: EN 1744-4:2021
ICS:
91.100.15 Mineralni materiali in izdelki Mineral materials and
products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 1744-4
EUROPEAN STANDARD
NORME EUROPÉENNE
December 2021
EUROPÄISCHE NORM
ICS 91.100.15 Supersedes EN 1744-4:2005
English Version
Tests for chemical properties of aggregates - Part 4:
Determination of water susceptibility of fillers for
bituminous mixtures
Essais pour déterminer les caractéristiques chimiques Prüfverfahren für chemische Eigenschaften von
des granulats - Partie 4 : Détermination de la Gesteinskörnungen - Teil 4: Bestimmung der
sensibilité à l'eau des fillers pour mélanges bitumineux Wasserempfindlichkeit von Füllern in bitumenhaltigen
Mischungen
This European Standard was approved by CEN on 22 November 2021.

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
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 1744-4:2021 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 6
4 Principle . 6
5 Separation of filler from a bitumen filler mixture . 7
5.1 Reagents . 7
5.2 Apparatus . 7
Figure 1 — T-shaped stirrer . 8
5.3 Sampling . 9
5.4 Preparation of test portions . 9
5.5 Procedure . 9
5.6 Calculation and expression of results . 10
5.7 Test report . 10
Annex A (normative) Determination of the volume increase and loss of stability of a Marshall
specimen . 11
A.1 General. 11
A.2 Principle . 11
A.3 Materials . 11
A.4 Apparatus . 11
A.5 Sampling . 12
Table A.1 — Mass of test portions . 12
A.6 Preparation of Marshall specimens . 12
Table A.2 — Proportion of the aggregates . 13
A.7 Procedure . 13
A.8 Calculation and expression of results . 13
A.9 Test report . 14
A.10 Precision . 14
Table A.3 — Repeatability (same observer, same apparatus) . 14
Table A.4 — Reproducibility (different observers, different apparatus) . 15
Annex B (informative) Water susceptibility of fillers – Shaking abrasion method . 16
B.1 General. 16
B.2 Principle . 16
B.3 Apparatus . 16
Figure B.1 — Shaking device . 17
B.4 Materials . 17
B.5 Preparation of the specimens . 17
B.5.1 Composition of the specimen mixture . 17
Table B.1 — Proportion of particle size classifications applied in the specimen mixture when
determining water susceptibility using the shaking abrasion method . 18
Table B.2 — Specimen mixture composition for determining water susceptibility using the
shaking abrasion method . 18
B.5.2 Preparation of the specimen mixture . 18
B.5.3 Manufacturing the specimens . 19
B.6 Procedure . 19
B.6.1 Determining water absorption and swelling. 19
B.6.2 Determining the shaking abrasion . 20
B.6.3 Calculation and expression of results . 20
B.6.3.1 Bulk density of the composite aggregate 0/0,4 mm . 20
B.6.3.2 Water absorption . 21
B.6.3.3 Swelling . 21
B.6.3.4 Shaking abrasion . 22
B.7 Test report . 22
Table B.3 — Example of tabular representation . 22
Bibliography . 23

European foreword
This document (EN 1744-4:2021) has been prepared by Technical Committee CEN/TC 154 “Aggregates”,
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 June 2022, and conflicting national standards shall be
withdrawn at the latest by June 2022.
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 1744-4:2005.
This document forms part of a series of tests for chemical properties of aggregates. Test methods for
other properties of aggregates are covered by Parts of the following European Standards:
— EN 932, Tests for general properties of aggregates
— EN 933, Tests for geometrical properties of aggregates
— EN 1097, Tests for mechanical and physical properties of aggregates
— EN 1367, Tests for thermal and weathering properties of aggregates
— EN 13179, Tests for filler aggregate used in bituminous mixtures
The other parts of EN 1744 are, or will be:
— Part 1: Chemical analysis
— Part 2: Determination of resistance to alkali/aggregate reaction
— Part 3: Preparation of eluates by leaching of aggregates
— Part 5: Determination of acid soluble chloride salts
— Part 6: Determination of the influence of aggregate extract on the initial setting time of cement
— Part 7: Determination of loss on ignition of Municipal Incinerator Bottom Ash Aggregate (MIBA
Aggregate)
— Part 8: Sorting test to determine metal content of Municipal Incinerator Bottom Ash (MIBA) Aggregates
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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.
1 Scope
This document specifies the procedure for the determination of the water susceptibility of fillers for
bituminous mixtures, by separation of filler from a bitumen filler mixture.
A method for the determination of water susceptibility by volume increase and loss of stability of a
Marshall specimen is described in Annex A.
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 932-1, Tests for general properties of aggregates - Part 1: Methods for sampling
EN 932-2, Tests for general properties of aggregates - Part 2: Methods for reducing laboratory samples
EN 932-5, Tests for general properties of aggregates - Part 5: Common equipment and calibration
EN 933-1:2012, Tests for geometrical properties of aggregates - Part 1: Determination of particle size
distribution - Sieving method
EN 933-2, Tests for geometrical properties of aggregates - Part 2: Determination of particle size distribution
- Test sieves, nominal size of apertures
EN 933-3, Tests for geometrical properties of aggregates - Part 3: Determination of particle shape -
Flakiness index
EN 933-4, Tests for geometrical properties of aggregates - Part 4: Determination of particle shape - Shape
index
EN 12274-7:2005, Slurry surfacing - Test Methods - Part 7: Shaking abrasion test
EN 12591, Bitumen and bituminous binders – Specifications for paving grade bitumen
EN 12697-6:2020, Bituminous mixtures - Test methods - Part 6: Determination of bulk density of bituminous
specimens
EN 12697-12:2018, Bituminous mixtures - Test methods - Part 12: Determination of the water sensitivity of
bituminous specimens
EN 12697-30, Bituminous mixtures - Test methods - Part 30: Specimen preparation by impact compactor
EN 12697-34, Bituminous mixtures - Test methods - Part 34: Marshall test
EN 12697-35, Bituminous mixtures - Test methods - Part 35: Laboratory mixing
EN 12846-2, Bitumen and bituminous binders - Determination of efflux time by the efflux viscometer - Part
2: Cut-back and fluxed bituminous binders
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth (ISO
3310-1)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
3.1
filler aggregate
aggregate, most of which passes a 0,063 mm sieve, which can be added to construction materials to
provide certain properties
3.2
water susceptibility of filler
measure of the degree of separation which occurs in the presence of water from a filler bitumen mixture,
e.g. as a result of intra-crystalline water inclusion between aggregate particles and binder coating
3.3
subsample
sample obtained from sampling increments or a bulk sample by means of a sample reduction procedure
3.4
test portion
sample used as a whole in a single test
3.5
aggregate size
designation of aggregate in terms of lower (d) and upper (D) sieve sizes expressed as d/D
Note 1 to entry: This designation accepts the presence of some particles which will be retained on the upper sieve
(oversize) and some which will pass the lower sieve (undersize).
3.6
particle size fraction
fraction of an aggregate passing the larger of two sieves and retained on the smaller
Note 1 to entry: The smaller sieve size can be zero.
3.7
constant mass
successive weighings after drying at least 1 h apart not differing by more than 0,1 %, by mass
Note 1 to entry: In many cases constant mass can be achieved after a test portion has been dried for a pre-
determined period in a specified oven at (110 ± 5) °C. Test laboratories can determine the time required to achieve
constant mass for specific types and sizes of sample dependent upon the drying capacity of the oven used.
4 Principle
A mixture of filler and bitumen is stirred in hot water. If filler becomes separated from the mixture
(indicated by the turbidity of the water), the filler is recovered on a filter paper and weighed.
5 Separation of filler from a bitumen filler mixture
5.1 Reagents
5.1.1 Bitumen: 50/70.
5.1.2 Redistilled Kerosene (paraffin oil), petroleum distillate with a boiling range between 190 °C and
260 °C.
The displacement liquid used in the method of testing density of cement, as specified in EN 196-6, is
suitable.
5.1.3 Low viscosity bitumen solution, obtained by dissolution of 50/70 bitumen (5.1.1) in kerosene (5.1.2),
with viscosity at 25 °C of ((60 ± 5) s, S.T.V. (Standard Tar Viscometer) 10 mm) as specified in EN 12846-2.
5.1.4 Demineralized water.
5.2 Apparatus
5.2.1 All apparatus, unless otherwise stated, shall conform to the general requirements of EN 932-5.
5.2.2 Sampling apparatus.
5.2.3 A balance capable of weighing up to 2000 g, accurate to 0,1 g. Other analytical balance capable of
weighing with an accuracy of 1 mg.
5.2.4 Glass conical flask, wide-mouthed, or disposable tinplate can. Glass or tinplate can, shall be of 250 ml
capacity.
5.2.5 Water bath, capable of maintaining a temperature of (60 ± 1) °C.
5.2.6 Motor-driven T-shaped stirrer, capable of maintaining (25 ± 1) revs/s (see Figure 1).
5.2.7 Lead cap with a hole in its centre to cover the tinplate can as the can is light-weighted with risk to
float and to allow stirring.
Dimensions in millimetres
Key
1 Air vent
Figure 1 — T-shaped stirrer
5.2.8 Glass beaker, 600 ml capacity.
5.2.9 Spatula.
5.2.10 Desiccator.
5.2.11 Sieve, 0,125 mm, complying with EN 933-2.
5.2.12 Well-ventilated oven, capable of maintaining a temperature of (110 ± 5) °C.
5.2.13 Graduated measuring cylinder, 100 ml capacity.
5.2.14 Two thermometers, 0 °C to 100 °C with 1 °C sub-divisions.
5.2.15 Stop-watch, or timer, readable to 1 s.
5.2.16 Büchner funnel, 90 mm diameter.
5.2.17 Vacuum flask, with suitable Büchner funnel adapter.
5.2.18 Medium grade filter paper, ashless, for quantitative analysis, of a diameter appropriate to the size
of the funnel (5.2.16).
5.3 Sampling
The laboratory sub-sample shall be taken in accordance with EN 932-1 and reduced in accordance with
EN 932-2, to produce a mass of about 50 g.
5.4 Preparation of test portions
Dry the reduced mass of filler in an oven at a temperature of (110 ± 5) °C to constant mass and cool to
room temperature in a desiccator for at least 90 min. If agglomerates are present in the material, reduce
these agglomerates to powder by means of a spatula. Mix the pulverised agglomerates with the rest of
the sub-sample and sieve the sub-sample through the 0,125 mm sieve. Remix the material passing the
sieve and take (10 ± 0,1) g as the test portion (m0).
5.5 Procedure
Place (50,0 ± 0,5) g of low viscosity bitumen solution (5.1.3) into the conical flask or the tinplate can and
add the test portion of filler to the conical flask or tinplate can. Measure (100 ± 5) ml of demineralized
water into the measuring cylinder.
Place the conical flask or the tinplate with the lead cap and the measuring cylinder in the water bath until
a temperature of (60 ± 1) °C has been reached by the contents of both vessels (checking by means of
thermometers) and maintain this temperature during the test. Stir the contents of the conical flask or the
tinplate can with its lead cap mechanically for (300 ± 5) s and then allow the mixture to stand for
(300 ± 5) s.
Pour the water from the measuring cylinder into the conical flask or the tinplate can with the lead cap
and stir again for (300 ± 5) s.
In the case of use of tinplate can, the supernatant water is to be transferred into a beaker, to see if
uncoated filler has separated.
In the case of a use of a glass conical flask, examine the mixture to see if uncoated filler has separated. If
not, the filler shall be considered as non-susceptible to water.
If the filler separates, or in the case of turbidity of the water, determine the water susceptibility as follows.
Allow the conical flask or the tinplate can and its contents to cool so that the mixture becomes kneadable.
Pour the water and the filler separated from the mixture by kneading in the flask with a spatula and
washing with water. Pour the water and the separated filler into the beaker and repeat the process until
the washing with water becomes clear.
Weigh a dried filter paper and records its mass (m ). Filter the contents of the beaker through the
weighed filter paper in a Büchner funnel to the vacuum flask. Remove the last traces of bitumen by
washing with kerosene (5.1.2). Dry the filter and recovered filler in an oven at (110 ± 5) °C to constant
mass.
Weigh the filter paper with the filler to the nearest 1 mg (m ).
5.6 Calculation and expression of results
Calculate the water susceptibility (W ), as a percentage by mass of the filler, in accordance with the
s
following equation:
mm−
2 1
W × 100 (1)
s
m
...