SIST EN 1744-4:2022

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
• Public Enquiry End Date: 19-May-2020
• Publication Date: 13-Mar-2022
• ICS: 91.100.15 - Mineral materials and products
• Technical Committee: AGR - Aggregates
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 22-Feb-2022
• Due Date: 29-Apr-2022
• Completion Date: 14-Mar-2022
• 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: EN 1744-4:2021 - Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility of fillers for bituminous mixtures

Relations

• Replaces: SIST EN 1744-4:2005 - Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility of fillers for bituminous mixtures
• Effective Date: 01-Apr-2022
• Replaces: SIST EN 1744-4:2005 - Tests for chemical properties of aggregates - Part 4: Determination of water susceptibility of fillers for bituminous mixtures
• Effective Date: 08-Jun-2022

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN 1744-4:2022
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
SIST EN 1744-4:2022 en,fr,de

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

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SIST EN 1744-4:2022
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SIST EN 1744-4:2022
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.
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
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

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SIST EN 1744-4:2022
EN 1744-4:2021 (E)

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

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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
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.
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
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)
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
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.

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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
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.
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
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.
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EN 1744-4:2021 (E)

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

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SIST EN 1744-4:2022
EN 1744-4:2021 (E)

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

following equation:
mm−
2 1
W × 100 (1)
where:
m is the mass of the test portion in grams;
m is the mass of the filter paper in grams;
m is the mass of the filter paper and filler in grams.
W should be rounded to the nearest 1 % by mass.
5.7 Test report

The test result shall be accompanied by an affirmation that the water susceptibility was determined in

accordance with this document.
The test report shall include the following information:
a) reference to this document;

b) identification of the test sample, including identification of the source and date of sampling;

c) sample reception date if different from sampling date;
d) identification of the laboratory;
e) the test results for water susceptibility;
f) deviations from the reference method – if any.
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
Annex A
(normative)
Determination of the volume increase and loss of stability of a Marshall
specimen
A.1 General

This annex specifies a method for the determination of the volume increase and loss of stability of a

Marshall specimen (VIM) which gives a measure of the influence of fillers on the durability of an asphalt

in the presence of water.
A.2 Principle

Hot mix asphalt 0/8, consisting of aggregates suitable for use and incorporating the filler under test, shall

be tested to determine volume increase and loss of stability after storage in water (40 ± 1) °C for 48 h.

The increase in volume shall be indicated in %.
A.3 Materials
A.3.1 Bitumen: 160/220.
A.3.2 Aggregates:
A.3.2.1 Aggregate stability:

Coarse aggregate shall be volumetrically stable under the conditions of this test.

A.3.2.2 Aggregate size/shape:

a) 5/8 mm (Flakiness Index FI or Shape Index SI , determined in accordance with EN 933-3 or

20 20
EN 933-4 respectively);
b) 2/5 mm;
c) 0,125/2 mm.
A.3.3 Test filler, < 0,125 mm.
A.4 Apparatus

A.4.1 All apparatus, unless otherwise stated, shall conform to the general requirements of EN 932-5.

A.4.2 Apparatus for preparation of a Marshall specimen, as specified in EN 12697-30.

A.4.3 Water bath to enable the samples to be held at (40 ± 1) °C and (25 ± 1) °C. The water bath shall have

a grid which enables the samples to be surrounded by water on all sides. It shall be large enough to ensure

that the amount of water available is equal to at least three times the volume of the samples.

A.4.4 Balance capable of weighing up to 5 000 g, accurate to 0,5 g, with a device for weighing under water

(e.g. wire basket).
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
A.4.5 Desiccator.
A.4.6 Vacuum or water-jet pump.

A.4.7 Mixer capable of producing mix sufficient for 8 Marshall-specimens in accordance with

EN 12697-35.
A.5 Sampling

Samples shall be taken in accordance with EN 932-1 and reduced in accordance with EN 932-2. The

masses of the test portions for Marshall specimens are specified in Table A.1.
Table A.1 — Mass of test portions
Aggregate sizes (d/D) Mass of test portion
mm kg
5/8 3
2/5 3
0,125/2 4,5
0/0,125 (test filler) 1,5

Dry the reduced mass of filler for 4 h in an oven at a temperature of (110 ± 5) °C and cool to room

temperature in a desiccator for at least 90 min. Sieve it on 125 µm.
A.6 Preparation of Marshall specimens

Screen the coarse aggregate to remove oversize and undersize and wash to remove fines. Screen the fine

aggregate into size fractions of 0,125/0,25 mm, 0,25/0,71 mm and 0,71/2,0 mm by wet sieving.

Eight Marshall specimens shall be prepared in accordance with EN 12697-30 from a mixture of hot mix

asphalt using the proportion of aggregates shown in Table A.2.

The bitumen is to be used in a quantity which, together with the aggregate mix specified, gives a void

content of (5,5 ± 0,5) % by volume of a Marshall specimen.

Heat the aggregate mixture and bitumen for eight Marshall specimens in an air circulating oven without

fresh air supply for about 3 h at 140 °C. Place the hot aggregates into the mixer preheated to 140 °C and

add the prescribed quantity of binder. Mix the components in accordance with EN 12697-35 to prepare

a mixture to produce eight Marshall specimens.

Directly after the mixing process, the aggregate mixture is divided in 8 subsamples.

Heat the asphalt mixtures to 140 °C, again in the ventilated oven, within 1 h of mixing process.

Subsequently compact the specimens in accordance with EN 12697-34 within 30 min.
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
Table A.2 — Proportion of the aggregates
Aggregate Fractions % by mass
Coarse 5/8 25
2/5 25
Fine 0,71/2 25
0,25/0,71
0,125/0,25 4
Test filler 0/0,125 10
A.7 Procedure

Determine the volume before storage (V ) of four specimens in accordance with EN 12697-12. Directly

after water storage determine the volume (V ), in accordance with EN 12697-6. Determine the Marshall

stability values in accordance with EN 12697-34.

Determine the Marshall stability values of the four remaining specimens in accordance with

EN 12697-34.
A.8 Calculation and expression of results

Calculate the water susceptibility as the percentage increase in volume of Marshall specimens with the

test filler after water storage in accordance with the following equation:
VV−
Q A
Q ×100 (A.1)
where:
Q is the volume increase in %;
V is the volume of specimens before water shortage, in cubic centimetres;
V is the volume of specimen after water storage, in cubic centimetres.

The volume increase shall be reported to the nearest 0,1 % by volume as the mean of a minimum of three

individual values.

The highest individual value minus the lowest individual value should not exceed 25 % of the mean of the

individual values (or 25 % by volume if this is greater).

To determine the mean value, only those values which fall within the permitted range may be used.

Furthermore the mass loss between the dry mass before test and the dry mass after test shall not exceed

2 g.
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SIST EN 1744-4:2022
EN 1744-4:2021 (E)
...

SLOVENSKI STANDARD
oSIST prEN 1744-4:2020
01-maj-2020

Preskusi kemičnih lastnosti agregatov - 4. del: Ugotavljanje sprejemljivosti vode

polnil za bitumenske mešanice

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
Ta slovenski standard je istoveten z: prEN 1744-4
ICS:
91.100.15 Mineralni materiali in izdelki Mineral materials and
products
oSIST prEN 1744-4:2020 en,fr,de

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

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oSIST prEN 1744-4:2020
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oSIST prEN 1744-4:2020
DRAFT
EUROPEAN STANDARD
prEN 1744-4
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2020
ICS 91.100.15 Will supersede EN 1744-4:2005
English Version
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

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 154.

If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations

which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.

This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other

language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC

Management Centre has the same status as the official versions.

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

Finland, 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.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 1744-4:2020 E

worldwide for CEN national Members.
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Contents Page

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

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

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

3 Terms and definitions ....................................................................................................... 5

4 Principle ................................................................................................................................. 6

5 Separation of filler from a bitumen filler mixture .................................................. 6

5.1 Reagents ................................................................................................................................. 6

5.2 Apparatus .............................................................................................................................. 6

5.3 Sampling ................................................................................................................................ 8

5.4 Preparation of test portions ........................................................................................... 8

5.5 Procedure .............................................................................................................................. 8

5.6 Calculation and expression of results ......................................................................... 9

5.7 Test report ............................................................................................................................ 9

Annex A (normative) Determination of the volume increase and loss of stability of a

Marshall specimen .......................................................................................................... 10

A.1 General ................................................................................................................................ 10

A.2 Principle .............................................................................................................................. 10

A.3 Materials ............................................................................................................................. 10

A.3.2 Aggregates: ......................................................................................................................... 10

A.4 Apparatus ........................................................................................................................... 10

A.5 Sampling ............................................................................................................................. 11

A.6 Preparation of Marshall specimens .......................................................................... 11

A.7 Procedure ........................................................................................................................... 12

A.8 Calculation and expression of results ...................................................................... 12

A.9 Test report ......................................................................................................................... 13

A.10 Precision ............................................................................................................................. 13

Bibliography .................................................................................................................................... 15

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European foreword

This document (prEN 1744-4:2020) has been prepared by Technical Committee CEN/TC 154

“Aggregates”, the secretariat of which is held by BSI.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 1744-4:2005.
The main changes compared to EN 1744-4:2005 are:
— updated normative references;
— clarification of the apparatus described in 5.2;
— clarification of the procedure described in 5.5.

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
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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 933-2, 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 12697-6, Bituminous mixtures — Test methods for hot mix asphalt — Part 6: Determination

of bulk density of bituminous specimens

EN 12697-12, 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
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3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following

addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
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.
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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 Bit
...